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WO2019034006A1 - 一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺 - Google Patents

一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺 Download PDF

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WO2019034006A1
WO2019034006A1 PCT/CN2018/100115 CN2018100115W WO2019034006A1 WO 2019034006 A1 WO2019034006 A1 WO 2019034006A1 CN 2018100115 W CN2018100115 W CN 2018100115W WO 2019034006 A1 WO2019034006 A1 WO 2019034006A1
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continuous flow
process according
production process
still
full continuous
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French (fr)
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马兵
潘帅
舒鑫琳
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Shanghai Hybrid-Chem Technologies
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Shanghai Hybrid-Chem Technologies
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Priority claimed from CN201810900615.8A external-priority patent/CN109553560A/zh
Application filed by Shanghai Hybrid-Chem Technologies filed Critical Shanghai Hybrid-Chem Technologies
Priority to JP2020516679A priority Critical patent/JP6925079B2/ja
Priority to EP18846139.6A priority patent/EP3666754B1/en
Publication of WO2019034006A1 publication Critical patent/WO2019034006A1/zh
Priority to US16/787,029 priority patent/US10919849B2/en
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C407/00—Preparation of peroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C409/00—Peroxy compounds
    • C07C409/38—Peroxy compounds the —O—O— group being bound between a >C=O group and a carbon atom, not further substituted by oxygen atoms, i.e. esters of peroxy acids

Definitions

  • the invention relates to the field of chemistry, in particular to an in-line full continuous flow production process for directly preparing an organic peroxide from an alcohol or an alkane, wherein the organic peroxide is a flammable and explosive compound.
  • the organic peroxide refers to an organic compound containing a -O-O-peroxy functional group formed by replacing a hydrogen atom in hydrogen peroxide with an organic group such as an alkyl group, an acyl group or an aromatic group.
  • the characteristic is that when the heat exceeds a certain temperature, it will decompose to generate oxygenated free radicals, which is unstable and easy to decompose.
  • the organic peroxide produced by the chemical industry is mainly used as a polymerization initiator and catalyst for synthetic resins. In the field of polymer materials, organic peroxides are used as initiators for radical polymerization, initiators for grafting reactions, crosslinkers for rubber and plastics, curing agents for unsaturated polyesters, and in the preparation of spun grade polypropylene.
  • Organic peroxides are sources of free radicals for use in the following: 1 free radical polymerization and copolymerization initiators of vinyl and diene monomers; 2 vulcanizing agents for thermosetting resins; 3 crosslinkers of elastomers and polyethylene .
  • organic peroxides are used as photoinitiators and sensitizers in the film industry for photosensitive polymer materials, photosensitive resins, etc., and are also commonly used in the production of epoxy resins;
  • organic peroxides are also used in bleaching agents, decolorizing agents, bactericides, cleaning agents, etc. for the sterilization of medical devices and foods, textiles, paper, and the like.
  • Peroxycarboxylic acid esters and peroxycarbonates are important organic peroxides, such as tert-butyl peroxy-2-octanyl carbonate, cumene peroxy neodecanoate and neodecanoic acid-1. 1,3,3-tetramethylbutyl ester.
  • Peroxycarboxylic acid esters and peroxycarbonates are low temperature initiators for free radical polymerization and are widely used in polyethylene (LDPE), polyvinyl chloride (PVC), polystyrene (PS), and styrene copolymers (eg, Production areas such as ABS), polymethacrylate (PMMA) and polyvinyl acetate (PVAc).
  • Peroxy ketals are mainly used as crosslinking agents for unsaturated polyesters, as initiators for rubber and plastics.
  • the demand for peroxycarboxylic acid esters, peroxycarbonates and peroxyketals is increasing in domestic and foreign markets, so the continuous production process of developing organic peroxides has practical significance and great prospects.
  • Organic peroxides are very reactive compounds that are easily decomposed into highly reactive free radicals and oxygen, which can release a large amount of heat or even cause an explosion.
  • SADT self-accelerating decomposition temperature
  • the exothermic rate of the organic peroxide decomposition reaction is unbalanced with the environmental heat dissipation rate, that is, the heat of the system is Accumulating, at this time, organic peroxides can cause dangerous self-accelerating decomposition reactions and explosions or fires in adverse environments by thermal decomposition. Contact with incompatible materials and increased mechanical stress can result in decomposition at or below SADT.
  • the organic peroxide decomposes under the action of temperature due to the presence of an oxygen-oxygen bond which can be opened in the energy range ⁇ H of about 84 to 184 kJ/mol, depending on the organic peroxide. nature. That is to say, the energy required for the decomposition of different organic peroxides to open the oxygen-oxygen bond is different depending on the respective properties. Therefore, different organic peroxides have large differences in self-decomposition acceleration temperature and thermal stability.
  • peroxy carboxylic acid ester peroxide peroxyphenyl phthalate has a self-decomposition acceleration temperature (SADT) of 10 ° C, a 10-hour half-life corresponding to a temperature of 38 ° C; peroxypivalic acid
  • SADT self-decomposition acceleration temperature
  • TBPV tert-butyl ester
  • SADT self-decomposition acceleration temperature
  • SADT self-decomposition acceleration temperature
  • SADT self-decomposition acceleration temperature
  • tert-butyl peroxy neodecanoate is 15 ° C, 10
  • the half-life of the hour corresponds to a temperature of 46 ° C
  • the peroxycarbonate peroxide peroxide 2-ethylhexyl carbonate tert-butyl ester (TBEC) self-decomposition acceleration temperature (SADT) is 60 ° C
  • the 10-hour half-life corresponds to the temperature 100 ° C
  • the first step is an oxidation reaction.
  • the alcohol or alkane reacts with an oxidant to synthesize an alkyl peroxide R(OOH) n and a dialkyl peroxide ROOR.
  • impurities such as dialkyl peroxide ROOR and water are removed.
  • the oxidation reaction product alkyl peroxide R(OOH) n is obtained , and the reaction formula is as follows:
  • the second step is a condensation reaction in which an alkyl peroxide R(OOH) n is reacted with a base and an acyl compound to synthesize a peroxycarboxylate or a peroxycarbonate.
  • the reaction formula is as follows:
  • the alkyl peroxide R(OOH) n is reacted with an acid and an alcohol or a ketone to synthesize a peroxy ketal.
  • the reaction formula is as follows:
  • R is selected from saturated or unsaturated C 1 -C 12 alkyl, unsubstituted or substituted aryl, unsubstituted or substituted heterocyclic aryl, unsubstituted or substituted saturated heterocycloalkyl, unsubstituted Or a partially saturated heterocycloalkyl group, an unsubstituted or substituted cycloalkyl group.
  • R 1 is selected from a saturated or unsaturated C 1 -C 20 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group.
  • R 2 is selected from a saturated or unsaturated C 1 -C 20 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocycloalkyl group, an unsubstituted or Substituting partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl.
  • R 3 is selected from saturated or unsaturated C 1 -C 12 alkyl, unsubstituted or substituted aryl, unsubstituted or substituted heterocyclic aryl, unsubstituted or substituted saturated heterocycloalkyl, unsubstituted or Substituting partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl.
  • R 4 or R 4 ' is selected from a saturated or unsaturated C 1 -C 12 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocycloalkyl group. Unsubstituted or substituted partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl.
  • the improvement of the industrial production process of chemical products mainly refers to the improvement of the process.
  • the process refers to a method and a process for processing or reacting raw materials by using various equipments to obtain a final product, and is a process of obtaining a product by adjusting chemical, physical, or physical processes by adjusting technical parameters such as temperature, pressure, and material ratio. That is, the production process refers to the process of realizing a chemical reaction or a physical process on an industrial scale.
  • a process can contain one reaction or multiple reactions.
  • the reaction involved in the preparation of the chemical product and the corresponding reaction route are determined by the reaction mechanism, but for the same reaction route, it can be achieved by different production processes.
  • Production process optimization and improvement may achieve the following effects: first, improve production efficiency, increase production capacity, reduce production costs; second, improve process safety; third, improve product quality; fourth, reduce “three wastes” emissions.
  • the oxidation reaction and the condensation reaction correspond to an oxidation process and a condensation process, respectively.
  • the oxidation reaction and the condensation reaction are both oil-water two-phase reaction, the reaction efficiency is low, and a large amount of water exists in the reaction system.
  • the oxidant used in the first oxidation reaction is a liquid oxidant (for example: hydrogen peroxide) or a gaseous oxidant (for example, oxygen).
  • the two problems caused by the oxidation reaction are: 1) due to the oxidation process, the oxidant cannot be completely converted, and Inevitably, dialkyl peroxides are formed, and dialkyl peroxides and oxidants which are not completely reacted become impurities in the oxidation process, and these impurities must be removed to carry out the next condensation reaction.
  • peroxide impurities dialkyl peroxide and hydrogen peroxide directly affect the quality of the final product (peroxycarboxylic acid ester, peroxycarbonate, peroxyketal).
  • the target product is tert-butyl peroxy neodecanoate
  • the tert-butyl peroxy neodecanoate has a SADT of 15 ° C
  • the half-life of 10 h corresponds to a temperature of 46 ° C
  • the second process of preparing peroxy neodecanoate is prepared.
  • the SADT of tert-butyl hydroperoxide is 80 ° C, and the half-life of 10 h corresponds to a temperature of 121 ° C.
  • the SADT and half-life of different concentrations of hydrogen peroxide are different.
  • the half-life of hydrogen peroxide in fresh water at normal temperature is 8 hours. In 20 days, it can be seen that the SADT and the half-life of the three are very different, and the mixture of the three cannot meet the single use requirement.
  • the initiator is usually a free radical initiator such as azobisisobutyronitrile (SADT is 50 ° C, 10 h half-life) Decomposition temperature is 65 ° C), dicumyl hydroperoxide (SADT is 75 ° C, 10 h half-life decomposition temperature is 117 ° C), etc., if not removed into the final product will also affect product quality and performance, and second, water and other impurities will Influencing the reaction rate, which in turn affects the production efficiency.
  • SADT azobisisobutyronitrile
  • Decomposition temperature is 65 ° C
  • water and other impurities will Influencing the reaction rate, which in turn affects the production efficiency.
  • the product obtained after the oxidation process is a mixture containing alkyl peroxides, impurities, and a large amount of water, in order to ensure the condensation process.
  • a purification process is required to remove impurities and a large amount of water from the mixture to prepare an alkyl peroxide which meets the standards of commercial industrial products (for example, commercially available t-butyl hydroperoxide is as follows: di-tert-butyl peroxide) ⁇ 0.08%, tert-butanol ⁇ 0.5%, other organic matter ⁇ 0.4%).
  • the purification process may be gas-liquid separation, acid-base method, vacuum distillation or distillation, flash separation, etc., the purification process usually adopts a batch process, and the Chinese patent CN106588734 mentions the purification step of cumene hydroperoxide. Including gas-liquid separation, flash separation and concentration, Chinese patent CN102617432 mentions the synthesis of t-butyl hydroperoxide, which is allowed to stand still to obtain the upper organic phase, and the alkali solution is added to the organic phase at a reaction temperature of 10 to 50 ° C.
  • the existing condensation process only obtains crude peroxycarboxylate, peroxycarbonate or peroxyketal, contains water, alkyl peroxide, salt, etc., and needs to be post-treated to obtain the city.
  • Standard products such as commercially available tert-butyl peroxy neodecanoate are required as follows: chloride ion content ⁇ 0.05%, tert-butyl hydroperoxide content ⁇ 0.1%)
  • the post-treatment process may be separation, alkali washing, Washing, vacuum distillation or distillation, flash separation, drying, etc.
  • Chinese patent CN102558399 mentioned that the post-treatment method of peroxy neodecanoate tert-butyl ester is to stand for 20-40 min after the end of the reaction, and the mother liquor is separated and the reaction is carried out.
  • the product is washed to a pH of 5-7, and a solvent of a solvent-type peroxy neodecanoate is obtained by adding an alkane solvent and stirring at 0 ° C for 20-30 min.
  • the post-treatment time is greater than 40 min; the Chinese patent CN102336694 mentions 1,1-
  • the post-treatment method of bis(tert-butylperoxy)cyclohexane is the alkali washing of the reaction mother liquid and washing with water to obtain a neutral reaction liquid, and the colorless liquid is obtained by distillation under reduced pressure to obtain the product 1,1-di(tert-butyl group).
  • Oxidation of cyclohexane refer to existing post-treatment processes 1-2 hours.
  • the existing post-treatment process takes a long time and has low efficiency.
  • separate equipment such as a rectification tower is required, and different post-treatment processes of peroxy carboxylic acid ester, peroxycarbonate or peroxy ketal are also different, and the existing production process is also There is no universal equipment and process that can purify a variety of different peroxycarboxylic acid esters, peroxycarbonates or peroxyketals.
  • the prior art process for producing peroxycarboxylic acid esters, peroxycarbonates or peroxyketals in accordance with commercially available standards needs to be divided into four steps, the first step being an oxidation process, the products of which are comprising alkyl peroxides and impurities.
  • the second step is a purification process, in addition to impurities and a large amount of water, to obtain an alkyl peroxide (ie, an intermediate product) that meets the requirements of a commercially available industrial product, and stores it for use;
  • the crude product of the target product peroxycarboxylic acid ester, peroxycarbonate or peroxyketal
  • the fourth step of the post-treatment process removes impurities and water to obtain peroxidation in accordance with the requirements of commercially available industrial products. Carboxylic acid ester, peroxycarbonate or peroxyketal.
  • alkyl peroxides are flammable and explosive dangerous materials, so there is a great safety risk in the process of accumulation, storage and purification of such compounds, and since the alkyl peroxides are flammable and explosive Temperatures are extremely sensitive and require cold chain storage and transportation, which greatly increases the cost of use and production.
  • the accumulation, storage and purification of alkyl peroxides are not possible, and the oxidation process and the condensation process cannot be seamlessly coupled to realize the direct continuous preparation of peroxycarboxylic acid esters, peroxycarbonates and peroxidation from alcohols or alkanes.
  • alkyl peroxide is of the formula R(OOH) n , wherein R is selected from a saturated or unsaturated C 1 -C 12 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted hetero Cycloaryl, unsubstituted or substituted saturated heterocycloalkyl, unsubstituted or substituted partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl.
  • R is selected from a saturated or unsaturated C 3 -C 8 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocycloalkyl group, Substituting or substituting partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl.
  • R is selected from the group consisting of t-butyl, tert-amyl, cumyl, 1,4-diisopropylphenyl, 2,4,4-trimethyl-2-pentyl, 2,5-dimethyl Base group.
  • alkyl peroxide is selected from the group consisting of:
  • the most important characteristics of the batch process are two points. One is that there is “stay” or “interruption” in the process, and the second is that the production of the products is spaced apart, that is, the product has a batch and only one fixed quantity of product can be obtained in one batch. That is, for each batch of production, a fixed amount of the raw materials is reacted in the order of the reaction steps, resulting in a limited fixed amount of product (product); then a fixed amount of the raw material is put, and the same step is followed. The batch reacted to produce a limited fixed product.
  • each step in one reactor there are two ways to achieve a batch process: 1) using multiple reactors (eg, flasks, reactors, etc.), each step in one reactor; 2) using a reactor (eg, flask, reaction) In the reactor, etc., each step of the reaction is sequentially completed in the reactor, and a plurality of raw materials need to be sequentially added according to the progress of the reaction, that is, after each step of the reaction, there is a “stay”, waiting for further addition of the raw materials of the subsequent reaction. .
  • Some literatures also refer to mode 2) as continuous, which is also intermittent in nature, because there is "stay” in the process, waiting for feeding, or adjusting to the appropriate temperature for the next reaction (for example, heating, cooling) Or keep warm).
  • the first step oxidation process Whether using oxygen auto-oxidation method or hydrogen peroxide oxidation method, the batch process reactor has a large liquid holding capacity, and a single reaction requires a large amount of pure oxygen or hydrogen peroxide, so the batch process has great safety hazards.
  • the third step of the condensation process is mostly exothermic, and the reactor needs to have good heat transfer performance to ensure that the reaction does not fly. Once the temperature is too high, the product will decompose and the yield will decrease.
  • the existing batch process mainly controls the reaction temperature by controlling the addition rate of the oxidant (slow drop or slow aeration) in combination with the corresponding heat transfer device, so that the operation time is greatly prolonged and the production efficiency is lowered; A large amount of peroxide exists for a long time, and the process safety hazard is very large, and the process safety problem is not fundamentally solved. That is, intermittent process safety, product yield and quality stability are in urgent need of improvement.
  • the amplification effect refers to the results obtained by using small equipment for chemical process (ie, small-scale) experiments (such as laboratory scale), and the results obtained under the same operating conditions with large-scale production devices (such as industrial scale). There are often big differences. The effect of these differences is called the amplification effect.
  • the reason is mainly that the temperature, concentration, and material residence time distribution in small-scale experimental equipment are different from those in large-scale equipment. That is to say, under the same operating conditions, the results of small-scale experiments cannot be completely repeated on the industrial scale; if the results of the same or similar results as the small-scale experiments are obtained on the industrial scale, it is necessary to optimize the adjustment and change the process parameters and Operating conditions.
  • the amplification effect is a difficult and urgent problem to be solved.
  • Local production means that the manufacturer places the equipment in the nearest or same location for the end consumer (or downstream user), thus greatly reducing the number of products from the manufacturer to the end consumer (or downstream users).
  • Intermediate links such as warehousing, logistics, etc., save a lot of costs.
  • local production still cannot avoid the storage and transportation of a small number of products, for example, from one workshop of the factory to another, taking products from the production equipment of synthetic products and transporting them to downstream production equipment.
  • On-line manufacturing as a kind of on-site production, refers to the production and use of products at the same time, seamlessly connecting with downstream processes, and synchronous production methods, so that the products are ready for use (produce- To-use), ready-to-use flexible manufacturing.
  • the so-called ready-to-use that is, the output is the use, the production and use of the product at the same time; with the production, it is always ready to produce, no need to wait, on-demand production of zero inventory; plug-and-production production equipment, is Immediately after the production device is started, the product is obtained and produced on demand. After the demand is met, the vehicle can be stopped.
  • the production time of online production can be shortened to more than ten minutes or even minutes, which can be seamlessly connected with the production equipment and production process of downstream users, which fundamentally avoids the storage and transportation of products, saves costs and improves production.
  • the safety also increases production efficiency.
  • the production time refers to the time required from the entry of the raw material into the reactor to the output of the commercially available product, including the reaction time and the post-treatment time, which is also referred to as the residence time in the continuous flow process.
  • the organic peroxide integrated full continuous flow process and reactor of the invention can be directly and seamlessly connected to the process and reactor of the downstream end user, realizes ready-to-use use, and may even realize that the whole process has not been macroscopically
  • the integrated continuous flow process can be directly connected with the polymerizer in the field of polymer materials, the vulcanizer of the film industry, etc., forming a continuous and continuous production and use of organic peroxides, subverting existing production-storage-transport-storage-use. Production mode, realize the new production mode of production and use, organic peroxide online production, ready-to-use, on-demand production, zero inventory and no logistics.
  • tert-butyl 2-ethylhexyl carbonate as a crosslinking agent is the most critical core material for EVA film in solar modules.
  • the integrated continuous flow reactor of the present invention can be seamlessly coupled with an EVA film vulcanizer.
  • the tert-butyl peroxy 2-ethylhexyl carbonate meets the commercially available standard and is directly connected to the batching kettle of the vulcanizer after being discharged from the integrated continuous flow reactor, and then vacuum laminating into the vulcanizer to obtain an EVA film, and finally cutting the package.
  • Real production is the use, without the accumulation and storage of tert-butyl 2-ethylhexyl carbonate, on the one hand greatly improving the safety of the overall process, on the other hand further reducing the production costs and greatly improving the production efficiency .
  • Organic peroxides are very reactive compounds that are easily decomposed into highly reactive free radicals and oxygen. During this process, a large amount of heat is released and even an explosion is caused. Therefore, organic peroxides are extremely sensitive to temperature and must be stored and transported at low temperatures. .
  • the existing process involves the accumulation, purification, storage and transportation of a large number of oxidation reaction products (alkyl peroxides) and products (peroxycarboxylic acid esters, peroxycarbonates or peroxyketals), both of which are flammable. Explosive organic peroxides, so one-third of the cost of existing organic peroxides is used for cold chain storage and transportation of intermediate products and products. On-line production is produced on demand when the product is needed.
  • Chinese patent CN101479239 describes a method for continuously preparing an organic peroxide using a plate heat exchanger having high heat exchange capacity, which is continuously prepared at a given temperature by introducing different reactants at different positions (plates) of the plate heat exchanger. Selected peroxide.
  • the temperature is given to a temperature above which the organic peroxide becomes thermally sensitive. This indicates that the reaction temperature is lower than the corresponding organic peroxide SDAT, and the final preferred reaction temperature ranges from 5 to 60 °C.
  • the yield is close to the higher temperature, but lower than the corresponding organic peroxide SADT.
  • the synthesis reaction time is in the range of 1 second to 45 seconds in the laboratory scale, and up to 2 minutes to 3 minutes on the industrial scale.
  • the reaction time refers to the time required for the reaction material to enter the reactor until the end of the reaction to obtain the crude product of the target product, excluding the time of the post-treatment.
  • the continuous preparation method has certain advantages in production efficiency and safety.
  • the industrial scale reaction time is 2 to 180 times of the laboratory scale, and there is a large
  • the amplification effect of determining greatly increases the difficulty of industrialization.
  • This large-scale and uncertain amplification effect will bring many disadvantages to the industrial application of the process. For example, when industrialization is amplified, only multiple steps of amplification can be adopted, and in order to achieve consistency with the laboratory scale.
  • each process of amplification must be re-adjusted to optimize process conditions and parameters, which will greatly consume manpower and material resources and project development time; even if multiple step-by-step amplification is used, the magnification effect may be too large, which may eventually lead to amplification. Afterwards, the results of the laboratory scale cannot be achieved; at the same time, the large-scale uncertain amplification effect will affect the stability and reliability of the process, resulting in unstable product quality and difficult to control; in addition, it will bring potential safety to the production process. risk.
  • the production time takes 3 to 18 hours, the reaction time is long, the production efficiency is low, and it is impossible to achieve on-line production, that is, ready to use.
  • the existing processes all have different degrees of amplification effects, resulting in a large amount of manpower and material resources and a lot of uncertainty when industrialization is amplified; the process reliability after amplification also has problems, resulting in unstable product quality, difficult to control; and production
  • the process lacks flexibility and has potential safety risks; due to the low reaction temperature, the total reaction time is too long and the yield is not high, which reduces the production efficiency, which increases the difficulty of industrialization.
  • the inability to achieve mass production limits its application. Therefore, it is necessary to find a fully continuous flow production process of an organic peroxide which is simple, safe, efficient, and capable of on-line production, is easy to mass-produce, and has no amplification effect.
  • the technical problem to be solved by the present invention is to provide an in-line continuous continuous flow production process for directly preparing an organic peroxide from an alcohol or an alkane, wherein the organic peroxide is a peroxycarboxylic acid ester.
  • peroxycarbonate or peroxyketal the production process directly from the safe starting materials (alcohols or alkanes) to produce high-risk organic peroxides, macroscopically non-hazardous alkyl peroxides (ie intermediate products)
  • safe starting materials alcohols or alkanes
  • macroscopically non-hazardous alkyl peroxides ie intermediate products
  • Flexible manufacturing the process is simple, safe and efficient, and there is no amplification effect.
  • the obtained organic peroxide product has high yield and content, and is easy to mass produce. Low production cost and improve the safety of an organic peroxide and downstream production of products.
  • aryl refers to an all-carbon monocyclic or fused polycyclic group of 5 to 12 carbon atoms having a fully conjugated pi-electron system.
  • aromatic rings are: benzene rings, naphthalene rings, and anthracene rings. The aromatic ring may be unsubstituted or substituted.
  • the substituent of the aromatic ring is selected from the group consisting of halogen, nitro, amino, cyano, hydroxy, C 1 -C 6 alkyl, C 1 -C 6 alkoxy, halogenated C 1 -C 6 alkyl, halogenated C 1 -C 6 alkoxy, C 3 -C 6 cycloalkyl, halogenated C 3 -C 6 cycloalkyl.
  • heterocyclic aryl refers to an unsaturated carbocyclic ring of 5 to 12 ring atoms in which one or more carbon atoms are replaced by a hetero atom such as N, O, S or the like.
  • the heteroaryl ring may be a single ring or a double ring, that is, fused by two rings.
  • Specific heterocyclic aryl groups may be: pyridyl, pyrimidinyl, pyrazinyl, isoxazolyl, isothiazolyl, pyrazolyl, thiazolyl, oxazolyl and imidazolyl, and the like.
  • the heterocyclic aryl group can be unsubstituted or substituted.
  • the substituent of the heterocyclic aryl group is selected from the group consisting of halogen, nitro, amino, cyano, hydroxy, C 1 -C 6 alkyl, C 1 -C 6 alkoxy, halogenated C 1 -C 6 alkyl, halogenated C 1 -C 6 alkoxy, C 3 -C 6 cycloalkyl, halogenated C 3 -C 6 cycloalkyl.
  • heterocycloalkyl refers to a monocyclic or fused ring radical having from 5 to 12 ring atoms in the ring wherein one or both ring atoms are selected from N, O or S(O) m ( Wherein m is a hetero atom of 0 to 2 integers, and the remaining ring atoms are C. These rings may contain one or more double bonds, but these rings do not have a fully conjugated pi-electron system.
  • the unsubstituted heterocycloalkyl group may be a pyrrolidinyl group, a piperidinyl group, a piperazinyl group, a morpholino group, a thiomorpholino group, a homopiperazinyl group or the like.
  • the heterocyclic ring can be unsubstituted or substituted.
  • the substituent of the heterocyclic ring is selected from the group consisting of halogen, nitro, amino, cyano, hydroxy, C 1 -C 6 alkyl, C 1 -C 6 alkoxy, halogenated C 1 -C 6 alkyl, halogenated C 1 -C 6 alkoxy, C 3 -C 6 cycloalkyl, halogenated C 3 -C 6 cycloalkyl.
  • cycloalkyl refers to a saturated monocyclic carbocyclic ring having from 3 to 12 carbon atoms unless a different number of atoms are indicated.
  • the cycloalkyl group includes a cyclopropyl group, a cyclobutyl group, a cyclopentyl group, a cyclohexyl group, a cycloheptyl group, a cyclooctyl group and the like.
  • a cycloalkyl group can be unsubstituted or substituted.
  • the cycloalkyl group can also be optionally substituted on any available carbon with one or more substituents selected from the group consisting of alkoxy, halogen, haloalkyl such as perfluoroalkyl.
  • alkyl as used in this patent includes both straight chain alkyl and branched alkyl groups.
  • a single alkyl group such as "propyl”
  • a single branched-chain alkyl group such as "isopropyl”
  • C1-6 alkyl includes C1-4 alkyl, C1-3 alkyl, methyl, ethyl, n-propyl, isopropyl and t-butyl.
  • alkoxy refers to an -O-alkyl group wherein alkyl is as defined above.
  • alkoxy as used in this patent include, but are not limited to, methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy and tert-butoxy.
  • Alkoxy also includes substituted alkoxy groups. The alkoxy group may be optionally substituted by one or more halogen atoms.
  • the continuous process refers to the connection between the production steps of the production system in the production process, and the continuous operation is ensured as a whole, but the waiting is allowed in each step.
  • continuous flow production process continuous-flow process
  • the raw materials are continuously produced continuously, and the materials in the process (that is, the reaction mixture containing raw materials, intermediates, products, solvents, etc.) are continuously flowing without interruption, and there is no waiting, that is, the products are continuously produced. Come out, it is a kind of "pipeline" type of chemical production process.
  • the state parameters such as composition and temperature of the material at any position in the reactor do not change with time, which is a steady state process, and thus the production process and product quality are stable.
  • the process can be referred to as a semi-continuous process; and only all steps are continuous
  • the material is continuously flowing throughout the process, that is, continuous addition of raw materials, continuous product, can be called continuous flow process (or full process continuous process).
  • the present invention innovatively provides an in-line full continuous flow production process for directly preparing an organic peroxide from an alcohol or an alkane, starting from a very safe material alcohol or alkane.
  • the reaction raw materials are successively successively subjected to two processes of oxidative condensation and post-treatment to prepare an organic peroxide, and the production process is carried out in a plug-and-production integrated continuous flow reactor in which the integrated continuous flow reactor is The feed inlet, the oxidant and the condensing agent are continuously added to the feed port, and the target product organic peroxide is continuously obtained at the outlet of the integrated continuous flow reactor, and the production process has no amplification effect, and the organic
  • the peroxide is selected from the group consisting of a peroxycarboxylic acid ester, a peroxycarbonate, a peroxyketal, the reaction substrate is an alcohol or an alkane, and the condensing agent is in the production of a peroxycarboxylic acid ester or a peroxycarbon
  • the invention thoroughly improves the prior art process for producing organic peroxide by integrating the reaction process and the advantages of the plug-and-production integrated continuous flow reactor, and can realize the online continuous continuous flow production of the organic peroxide, which will oxidize
  • the condensation process and the post-treatment process are effectively integrated into one process, which not only directly produces a highly dangerous organic peroxide from a safe starting material (alcohol or alkane), but also macroscopically non-hazardous alkyl peroxide (middle)
  • the process of accumulation, purification and residence of the product avoids the steps of purification, storage and transportation of the alkyl peroxide, realizes the ready-to-use use of the organic peroxide, and overcomes the amplification effect problem, and at the same time realizes On-line manufacturing, production and use of products at the same time, seamlessly coupled with downstream processes and equipment, synchronized production methods, so that the product is ready-to-use, useless Ready-to-use flexible manufacturing.
  • the production process of the invention has the following formula:
  • a 1 is an alcohol or an alkane
  • a 2 is selected from the group consisting of an acid chloride, a chloroformate, an alcohol, a ketone
  • the oxidizing agent is selected from hydrogen peroxide and oxygen
  • C is selected from the group consisting of a peroxycarboxylic acid ester, a peroxycarbonate, and a peroxyketal.
  • R is selected from saturated or unsaturated C 1 -C 12 alkyl, unsubstituted or substituted aryl, unsubstituted or substituted heterocyclic aryl, unsubstituted or substituted saturated heterocycloalkyl, unsubstituted or substituted Partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl;
  • R 1 is selected from a saturated or unsaturated C 1 -C 20 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group;
  • R 2 is selected from a saturated or unsaturated C 1 -C 20 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocycloalkyl group, an unsubstituted or Substituting a partially saturated heterocycloalkyl group, an unsubstituted or substituted cycloalkyl group;
  • R 3 is selected from saturated or unsaturated C 1 -C 12 alkyl, unsubstituted or substituted aryl, unsubstituted or substituted heterocyclic aryl, unsubstituted or substituted saturated heterocycloalkyl, unsubstituted or Substituting a partially saturated heterocycloalkyl group, an unsubstituted or substituted cycloalkyl group;
  • R 4 or R 4 ' is selected from a saturated or unsaturated C 1 -C 12 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocycloalkyl group. , unsubstituted or substituted partially saturated heterocycloalkyl, unsubstituted or substituted cycloalkyl;
  • R is selected from a saturated or unsaturated C3-C8 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocyclic ring, an unsubstituted or substituted partially saturated hetero Ring, unsubstituted or substituted cycloalkyl;
  • R 1 is selected from a saturated or unsaturated C 1 -C 18 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group;
  • R 2 is selected from a saturated or unsaturated C 1 -C 18 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocyclic ring, an unsubstituted or substituted partially saturated Heterocyclic, unsubstituted or substituted cycloalkyl;
  • R 3 is selected from a saturated or unsaturated C 3 -C 8 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocyclic ring, an unsubstituted or substituted moiety. a saturated heterocyclic ring, an unsubstituted or substituted cycloalkyl group;
  • R 4 or R 4 ' is selected from a saturated or unsaturated C 3 -C 8 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocyclic ring, Substituting or substituting a partially saturated heterocyclic ring, an unsubstituted or substituted cycloalkyl group;
  • R is selected from the group consisting of t-butyl, tert-amyl, cumyl, 1,4-diisopropylphenyl, 2,4,4-trimethyl-2-pentyl, 2,5-dimethylhexyl, 1,3-diisopropylphenyl;
  • R 1 is selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, tert-butyl, isopentyl, n-pentyl, isoheptyl, octyl, isooctyl, 2,2 - dimethylheptyl, decyl, undecyl, phenyl, 2-methylphenyl, 4-methylphenyl, 4-chlorophenyl, 2,4-dichlorophenyl, naphthyl;
  • R 2 is selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, 2-ethylhexyl, isotridecyl, heptadecyl, cyclohexyl, 4-tert-butylcyclohexyl, Benzyl, phenoxyethyl;
  • R 3 is selected from the group consisting of t-butyl, tert-amyl, 2,5-dimethylhexyl, 1,4-diisopropylphenyl, 1,3-diisopropylphenyl;
  • R 4 or R 4 ' is selected from the group consisting of methyl and ethyl;
  • R 4 is selected from -(CH 2 ) 5 -, -CH 2 -C(CH 3 ) 2 -CH 2 -CH(CH 3 )-CH 2 -;
  • R(OH) n is selected from the group consisting of tert-butanol, tert-amyl alcohol, 2,4,4-trimethyl-2-pentanol, 2,5-dimethyl-2,5-dihydroxyhexane, dihydroxy-1 , 4-diisopropylbenzene, dihydroxy-1,3-diisopropylbenzene;
  • R(H) n is selected from the group consisting of cumene, 1,4-diisopropylbenzene, and 1,3-diisopropylbenzene;
  • R 1 COCl is selected from the group consisting of acetyl chloride, propionyl chloride, butyryl chloride, isobutyryl chloride, valeryl chloride, 2-methylbutyryl chloride, pivaloyl chloride, 2-methylpentanoyl chloride, 2-ethylbutyryl chloride, 2-ethyl Hexanoyl chloride, decanoyl chloride, 2,4,4-trimethylpentanoyl chloride, 3,5,5-trimethylhexanoyl chloride, neodecanoyl chloride, decanoyl chloride, lauroyl chloride, benzoyl chloride, 2-methylbyl Acid chloride, 4-methylbenzoyl chloride, 4-chlorobenzoyl chloride, 2,4-dichlorobenzoyl chloride, naphthoyl chloride;
  • R 2 OCOCl is selected from the group consisting of methyl chloroformate, ethyl chloroformate, n-propyl chloroformate, isopropyl chloroformate, n-butyl chloroformate, sec-butyl chloroformate, 2-ethylhexyl chloroformate, chloroformic acid.
  • R 3 (OH) n is selected from the group consisting of tert-butanol, tert-amyl alcohol, 2,4,4-trimethyl-2-pentanol, 2,5-dimethyl-2,5-dihydroxyhexane, dihydroxy- 1,4-diisopropylbenzene, dihydroxy-1,3-diisopropylbenzene;
  • R 4 R 4' (CO) is selected from methyl ethyl ketone; R 4 (CO) is selected from cyclohexanone, 3,3,5-trimethylcyclohexanone.
  • organic peroxide is selected from the group consisting of:
  • the process of accumulating, purifying and waiting for the alkyl peroxide (intermediate product) which is macroscopically non-hazardous in the production process of the invention realizes the reaction substrate with alcohol or alkane as the starting substrate, and continuously produces the organic peroxide.
  • Peroxycarboxylic acid esters, peroxycarbonates, peroxy ketals innovative online production of organic peroxides, ready to use, breaking through the limitations of existing processes.
  • the alkyl peroxide is of the formula R(OOH) n , wherein R is selected from a saturated or unsaturated C 1 -C 12 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group.
  • R is selected from a saturated or unsaturated C 1 -C 12 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group.
  • R is selected from a saturated or unsaturated C 3 -C 8 alkyl group, an unsubstituted or substituted aryl group, an unsubstituted or substituted heterocyclic aryl group, an unsubstituted or substituted saturated heterocyclic ring, an unsubstituted or Substituting partially saturated heterocyclic, unsubstituted or substituted cycloalkyl.
  • R is selected from the group consisting of t-butyl, tert-amyl, cumyl, 1,4-diisopropylphenyl, 2,4,4-trimethyl-2-pentyl, 2,5-dimethyl Base group.
  • alkyl peroxide is selected from the group consisting of:
  • the target product organic peroxide obtained by the process of the invention is a product conforming to the standard of commercial industrial products, and further, the chloride ion content of the target product organic peroxide is ⁇ 0.05wt%, and other organic peroxide impurities The content is ⁇ 0.1% by weight, and the other organic peroxide impurities are selected from any one or any of H 2 O 2 , alkane peroxide, and dialkyl hydrocarbon peroxide.
  • the production time of the process of the present invention is ⁇ 15 min, preferably the production time is ⁇ 10 min; more preferably, the production time is 3 to 13 min; more preferably, the production time is 4 to 11 min; More preferably, the production time is 5 to 10 minutes.
  • the production time refers to the time required from the reaction raw materials (reaction substrate, oxidizing agent and condensing agent) to enter the integrated continuous flow reactor to produce a target product which meets the commercially available standard, including the oxidative condensation process. Time and time of the post-processing process.
  • the yield of the organic peroxide is ⁇ 64%; preferably, the yield of the organic peroxide is ⁇ 75%; more preferably, the yield of the organic peroxide is ⁇ 81%.
  • the content of the organic peroxide is ⁇ 77%; preferably, the content of the organic peroxide is ⁇ 85%; and the content of the organic peroxide is ⁇ 97%.
  • the temperature of the oxidative condensation process is 0 to 200 ° C, preferably 0 to 180 ° C, more preferably 0 to 160 ° C, still more preferably 0 to 140 ° C, still more preferably 5 to 130 ° C.
  • the post-treatment temperature is 0 to 60 ° C, preferably 0 to 50 ° C, more preferably 0 to 40 ° C, still more preferably 0 to 30 ° C, still more preferably 5 to 30 ° C.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metals
  • the hydroxide or water-soluble metal carbonate is more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the alkali liquid has a mass concentration of 5% to 45%, preferably 15% to 35%, more preferably 20% to 30%.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the acid solution has a mass concentration of 50% to 90%, preferably 60% to 80%, more preferably 70% to 80%.
  • the oxidizing agent is selected from the group consisting of hydrogen peroxide and oxygen.
  • reaction substrate is selected from the group consisting of t-butanol, tert-amyl alcohol, cumene, 1,4-diisopropylbenzene, p-mentane, decane, tetrahydronaphthalene, 2,4,4-trimethyl Base-2-pentanol, 1,3-diisopropylbenzene, dihydroxy-1,4-diisopropylbenzene, dihydroxy-1,3-diisopropylbenzene.
  • the acyl compound in the condensing agent is selected from the group consisting of acetyl chloride, propionyl chloride, butyryl chloride, isobutyryl chloride, valeryl chloride, 2-methylbutyryl chloride, pivaloyl chloride, 2-methylpentanoyl chloride, 2-B Butyryl chloride, 2-ethylhexanoyl chloride, decanoyl chloride, 2,4,4-trimethylpentanoyl chloride, 3,5,5-trimethylhexanoyl chloride, neodecanoyl chloride, decanoyl chloride, lauroyl chloride, benzoyl Acid chloride, 2-methylbenzoyl chloride, 4-methylbenzoyl chloride, 4-chlorobenzoyl chloride, 2,4-dichlorobenzoyl chloride, naphthoyl chloride, methyl chloroformate, ethyl chloroformate, chlorine N-propyl format
  • the molar ratio of the acid to the reaction substrate is from 0.3:1 to 1.5:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1.
  • the molar ratio of the oxidizing agent to the reaction substrate is from 0.8:1 to 2.2:1, preferably from 0.9:1 to 2.1:1, more preferably from 1:1 to 2:1, still more preferably from 1.3:1 to 1.8:1.
  • the molar ratio of the base to the reaction substrate is from 0.7:1 to 2:1, preferably from 0.9:1 to 1.8:1, more preferably from 1:1 to 1.6:1, still more preferably from 1:1 to 1.4:1.
  • the molar ratio of the acyl compound to the reaction substrate is from 0.5:1 to 1.2:1, preferably from 0.6:1 to 1.1:1, more preferably from 0.7:1 to 1:1.
  • the molar ratio of the condensation raw material to the reaction substrate is from 0.5:1 to 1.2:1, preferably from 0.6:1 to 1.1:1, more preferably from 0.7:1 to 1:1.
  • reaction substrate has a flow rate of 0.2 to 10 L/h, preferably 0.5 to 8 L/h, more preferably 1 to 6 L/h.
  • the acid flow rate is 0.2 to 5 L/h, preferably 0.4 to 4 L/h, more preferably 0.5 to 3 L/h.
  • the lye flow rate is 0.2 to 12 L/h, preferably 0.3 to 9 L/h, more preferably 0.5 to 8 L/h.
  • the flow rate of the acyl compound or the condensation raw material is 0.2 to 8 L/h, preferably 0.3 to 6 L/h, more preferably 0.5 to 4 L/h.
  • the target product of the online full continuous flow production process is t-butyl peroxy neodecanoate
  • the reaction substrate is t-butanol
  • the acyl compound is neodecanoyl chloride
  • the oxidant is hydrogen peroxide, wherein , preferred:
  • the hydrogen peroxide has a mass concentration of 30% to 50%
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the tert-butyl peroxy neodecanoate is ⁇ 68%; preferably, the yield of t-butyl peroxy neodecanoate is ⁇ 81%.
  • the content of the tert-butyl peroxy neodecanoate is ⁇ 87%; preferably, the content of t-butyl peroxy neodecanoate is ⁇ 91%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in tert-butyl peroxy neodecanoate, a content of other organic peroxide impurities of 0.05 to 0.08% by weight, and the other organic peroxide impurity is H 2 . O 2 and di-tert-butyl peroxide.
  • the temperature of the oxidative condensation process is from 0 to 160 ° C, preferably from 20 to 130 ° C, more preferably from 40 to 120 ° C, still more preferably from 60 to 100 ° C, still more preferably from 70 to 90 ° C.
  • the post-treatment temperature is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the t-butanol flow rate is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the neodecanoyl chloride flow rate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to tert-butanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-butanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-butanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of the neodecanoyl chloride to tert-butanol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the reaction substrate is 2,4,4-trimethyl Base-2-pentanol
  • the acyl compound is neodecanoyl chloride
  • the oxidizing agent is hydrogen peroxide
  • the hydrogen peroxide concentration is 30% to 50%
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the peroxynonanoic acid-1,1,3,3-tetramethylbutyl ester is ⁇ 65%; preferably, neodecanoic acid-1,1,3,3-tetramethylbutyl ester The yield is ⁇ 70%.
  • the content of the peroxy neodecanoic acid-1,1,3,3-tetramethylbutyl ester is ⁇ 80%; preferably, the peroxy neodecanoic acid-1,1,3,3-tetramethylbutyl ester The content is ⁇ 90%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in neodecanoic acid-1,1,3,3-tetramethylbutyl ester, and the content of the other organic peroxide impurities is 0.05 to 0.1 wt. %, the other organic peroxide impurity is H 2 O 2 .
  • the temperature of the oxidative condensation process is from 0 to 160 ° C, preferably from 20 to 130 ° C, more preferably from 40 to 120 ° C, still more preferably from 60 to 100 ° C, still more preferably from 70 to 90 ° C.
  • the post-treatment temperature is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the flow rate of the 2,4,4-trimethyl-2-pentanol is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 11 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the neodecanoyl chloride flow rate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to 2,4,4-trimethyl-2-pentanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, more It is preferably 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the 2,4,4-trimethyl-2-pentanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, more Preferably 1.05:1 to 1.2:1.
  • the molar ratio of the base to 2,4,4-trimethyl-2-pentanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of the neodecanoyl chloride to 2,4,4-trimethyl-2-pentanol is from 0.7:1 to 1.1:1, preferably from 0.8:1 to 1:1, more preferably from 0.8:1 to 0.95:1. .
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is tert-butyl 2-ethylhexyl carbonate
  • the reaction substrate is t-butanol
  • the acyl compound is 2-ethylhexyl chloroformate.
  • An ester, the oxidizing agent being hydrogen peroxide, wherein:
  • the hydrogen peroxide has a mass concentration of 30% to 50%.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the tert-butyl 2-ethylhexylcarbonate is ⁇ 70%; preferably, the yield of tert-butyl 2-ethylhexylcarbonate is ⁇ 81%.
  • the content of the tert-butyl 2-ethylhexyl carbonate is ⁇ 95%; preferably, the content of tert-butyl 2-ethylhexyl carbonate is ⁇ 97%.
  • the target product has a chloride ion content of 0.03 to 0.05 wt% in 2-ethylhexylcarbonate tert-butyl ester and a content of other organic peroxide impurities of 0.05 to 0.08 wt%, and the other organic peroxide impurities. It is H 2 O 2 and di-tert-butyl peroxide.
  • the temperature of the oxidative condensation process is from 0 to 160 ° C, preferably from 20 to 130 ° C, more preferably from 40 to 120 ° C, still more preferably from 60 to 100 ° C, still more preferably from 70 to 90 ° C.
  • the post-treatment temperature is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the t-butanol flow rate is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the flow rate of the 2-ethylhexyl chloroformate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to tert-butanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-butanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-butanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of 2-ethylhexyl chloroformate to tert-butanol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is peroxyphenyl neodecanoate
  • the reaction substrate is cumene
  • the acyl compound is neodecanoyl chloride
  • the oxidant is oxygen.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5 ⁇ 7min.
  • the yield of the cumene peroxy neodecanoate is ⁇ 79%; preferably, the yield of cumene peroxy neodecanoate is ⁇ 81%.
  • the content of the cumene peroxy neodecanoate is ⁇ 89%; preferably, the content of cumene peroxy neodecanoate is ⁇ 94%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in cumene neodecanoate, a content of other organic peroxide impurities of 0.05 to 0.1% by weight, and the other peroxide impurities are two different.
  • Propylbenzene hydrogen peroxide is a compound that has a chloride ion content of 0.03 to 0.05% by weight in cumene neodecanoate, a content of other organic peroxide impurities of 0.05 to 0.1% by weight, and the other peroxide impurities are two different.
  • Propylbenzene hydrogen peroxide Propylbenzene hydrogen peroxide.
  • the temperature of the oxidative condensation process is 0 to 180 ° C, preferably 0 to 150 ° C, preferably 20 to 130 ° C, more preferably 40 to 120 ° C, still more preferably 60 to 100 ° C, still more preferably 70 to 90 ° C.
  • the post-treatment temperature is 0 to 60 ° C, preferably 0 to 50 ° C, more preferably 0 to 40 ° C, still more preferably 0 to 30 ° C, still more preferably 5 to 30 ° C.
  • the cumene flow rate is 0.2 to 8 L/h, preferably 0.5 to 6 L/h, more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the neodecanoyl chloride flow rate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of oxygen to cumene is from 0.8:1 to 2.2:1, preferably from 1.3:1 to 2.1:1, more preferably from 1.5:1 to 2:1.
  • the molar ratio of the base to cumene is from 1:1 to 1.8:1, preferably from 1.2:1 to 1.6:1, more preferably from 1.3:1 to 1.5:1.
  • the molar ratio of the neodecanoyl chloride to cumene is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates, water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides. Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is t-butyl isopropyl acrylate
  • the reaction substrate is t-butanol
  • the acyl compound is isopropyl chloroformate
  • the oxidant is hydrogen peroxide
  • the hydrogen peroxide has a mass concentration of 30% to 50%.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the tert-butyl isopropyl peroxycarbonate is ⁇ 70.5%; preferably, the yield of tert-butyl isopropylperoxycarbonate is ⁇ 80%.
  • the content of the tert-butyl peroxyperoxycarbonate is ⁇ 95%; preferably, the content of t-butyl isopropylperoxycarbonate is ⁇ 97%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in tert-butyl peroxydicarbonate, a content of other organic peroxide impurities of 0.05 to 0.08% by weight, and the other organic peroxide impurity is H. 2 O 2 and di-tert-butyl peroxide.
  • the temperature of the oxidative condensation process is from 0 to 160 ° C, preferably from 20 to 130 ° C, more preferably from 40 to 120 ° C, still more preferably from 60 to 100 ° C, still more preferably from 70 to 90 ° C.
  • the post-treatment temperature is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the molar ratio of the acid to tert-butanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-butanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-butanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of isopropyl chloroformate to tert-butanol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates, water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides. Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is t-amyl 2-ethylhexyl carbonate
  • the reaction substrate is tert-amyl alcohol
  • the acyl compound is 2-ethylhexyl chloroformate.
  • the oxidizing agent is hydrogen peroxide, wherein: preferred:
  • the hydrogen peroxide has a mass concentration of 30% to 50%.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the target product has a chloride ion content of 0.03 to 0.05 wt% in 2-ethylhexylcarbonate t-amyl ester and a content of other organic peroxide impurities of 0.05 to 0.08 wt%, and the other organic peroxide impurities It is H 2 O 2 and di-tert-amyl peroxide.
  • the temperature of the oxidative condensation process is from 0 to 160 ° C, preferably from 20 to 130 ° C, more preferably from 40 to 120 ° C, still more preferably from 60 to 100 ° C, still more preferably from 70 to 90 ° C.
  • the post-treatment temperature is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the yield of the tert-amyl 2-ethylhexylcarbonate is ⁇ 70%; preferably, the yield of tert-amyl 2-ethylhexylcarbonate is ⁇ 81%.
  • the content of the tert-amyl 2-ethylhexyl carbonate is ⁇ 95%; preferably, the content of the tert-amyl 2-ethylhexyl carbonate is ⁇ 97%
  • the molar ratio of the acid to tert-amyl alcohol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-amyl alcohol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-amyl alcohol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of 2-ethylhexyl chloroformate to tert-amyl alcohol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates, water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides. Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • mass concentration of the reaction substrate, oxidant and condensing agent used in actual production will have a deviation of mass concentration of ⁇ 3 percentage points; ⁇ 3 °C deviation; production time will have a deviation of ⁇ 3 s.
  • the production scale can be flexibly changed without re-adjusting the optimized process conditions and parameters, and the production process is flexible; no amplification effect makes the production process stable and reliable, and fluctuations in process conditions and parameters will not affect product quality.
  • the quality of the product is easy to control; this also greatly enhances the safety of the production process.
  • the continuous flow process of the invention has good stability and reliability, and thus the product quality is stable and reproducible; the process has no amplification effect, and the problem of the amplification effect of the industrial process of the organic peroxide continuous flow process is solved;
  • the production-type integrated continuous flow reactor has short production time, small volume and small floor space because it does not need to delay the pipeline, which greatly saves the plant land and improves the production efficiency.
  • the present invention has developed a specialized integrated reactor.
  • the reactor may be a modular structure, the structure and quantity of the design module, the modules included in each temperature zone, and the development of specific process conditions and parameters, including the division and temperature setting of each temperature zone, etc.
  • the synergy of various factors makes this continuous flow process possible. It is also possible to further combine the temperature and material concentration, the material ratio and the material flow rate to match the reaction progress, and obtain a better reaction effect.
  • the production process of the invention can complete the reaction of preparing organic peroxide quickly and continuously at high temperature, and the total reaction time can be shortened to 15 minutes or even shortened by the optimization of functional unit division and temperature setting and the synergy of functional units. In a few minutes, the efficiency of the process is greatly improved. It can be seen that the production process of the present invention breaks through the limitations of the prior art, and achieves high efficiency and high quality production of organic peroxides under the harsh and dangerous conditions that cannot be realized by the prior art, and avoids alkyl groups.
  • the steps of purification, storage and transportation of peroxides enable the production and use of organic peroxides, which not only ensures high-quality and efficient production of organic peroxides, but also seamlessly links with downstream processes and synchronizes with each other. Avoid the storage and transportation steps of the target product organic peroxide. Moreover, the production process does not have an amplification effect, is very suitable for industrial production, and can realize the ready-to-use use of organic peroxides, without the need of cold chain transportation and storage, greatly improving the safety of production and use, and reducing the cost. Is a major breakthrough in this field.
  • the plug-and-production integrated continuous flow reactor adopts a unitized structure including an oxidative condensation unit and a post-processing unit, wherein:
  • the oxidative condensation unit is used to react the reaction substrate, the oxidizing agent and the condensing agent to form a peroxycarboxylic acid ester, a peroxycarbonate and a peroxyketal
  • the post-treatment unit is used for purification and washing of the organic peroxide.
  • the organic peroxide is selected from the group consisting of peroxycarboxylic acid esters, peroxycarbonates, and peroxyketals.
  • the temperature of the oxidative condensation unit is 0 to 200 ° C, preferably 0 to 180 ° C, more preferably 0 to 160 ° C, still more preferably 0 to 140 ° C, still more preferably 5 to 130 ° C.
  • the temperature of the post-treatment unit is 0 to 60 ° C, preferably 0 to 50 ° C, more preferably 0 to 40 ° C, still more preferably 0 to 30 ° C, still more preferably 5 to 30 ° C.
  • the plug-and-play integrated continuous flow reactor employs a unitized structure, each of the units independently comprising more than one reactor A module or a set of reactor modules, wherein the reactor module group is composed of a plurality of reactor modules connected in series or in parallel, and the units are connected in series with each other.
  • the plug-and-play integrated continuous flow reactor employs a unitized structure, each of the units comprising at least one temperature zone, each The temperature zone independently comprises more than one reactor module or group of reactor modules, wherein the reactor module group consists of a plurality of reactor modules connected in series or in parallel, with each temperature zone being connected in series with each other.
  • the unit further includes a buffer between the units, and the buffer is a container having a certain volume, which is mainly used for buffering the pressure fluctuation of the system and balancing the flow difference, so that the system works more smoothly.
  • the number of the integrated continuous flow reactor feed ports is one or more, and the number of the integrated continuous flow reactor discharge ports is one or more.
  • the reactor module is optionally any reactor capable of realizing a continuous flow process, the reactor being selected from the group consisting of a microreactor, a Tandem loop reactor, and a tube. Any one or any of a variety of reactors (Tubularreactor).
  • the microreactor also known as a microstructure reactor or a microchannel reactor, is a device in which a chemical reaction occurs in a limited area with a general lateral dimension of 1 mm or less. The form is a miniature size channel.
  • a tandem coil reactor that is, a reactor in which a coil reactor is connected in series by a pipe, wherein the coil reactor is in the form of a tubular reactor.
  • the tubular reactor is a continuous operation reactor with a tubular shape and a large aspect ratio which appeared in the middle of the last century.
  • Such a reactor can be very long; it can be a single tube or a plurality of tubes in parallel; it can be an empty tube or a filling tube.
  • the reactor may be one or more.
  • the reactor channel is made of single crystal silicon, special glass, ceramic, stainless steel or metal alloy coated with a corrosion resistant coating, and polytetrafluoroethylene.
  • reactor modules, the reactor module groups, the reactor modules and the reactor module groups are respectively connected in series or in parallel.
  • continuous flow production process is carried out in a plug-and-play integrated continuous flow reactor comprising six temperature zones.
  • the oxidative condensation reaction unit of the continuous flow production process comprises four temperature zones, namely a temperature zone 1, a temperature zone 2, a temperature zone 3 and a temperature zone 4, and the post-processing unit comprises two temperature zones, respectively Temperature zone 5 and temperature zone 6.
  • the integrated reactor is actually 5 temperature zones, and the temperature zone 1 (temperature zone 1) + Temperature zone 2), temperature zone 3, temperature zone 4, temperature zone 5 and temperature zone 6, others and so on.
  • the continuous flow production process includes the following steps:
  • reaction substrate is an alcohol or an alkane
  • condensing agent is an alkali liquid and an acyl compound in the production of a peroxycarboxylic acid ester or a peroxycarbonate, and an acid liquid and a condensation raw material in the production of a peroxy ketal.
  • the condensation feedstock is an alcohol or a ketone.
  • reaction liquid flowing out of the temperature zone 4 enters the aftertreatment unit, and is post-treated through the temperature zone 5 and the temperature zone 6 to obtain the target product organic peroxide, and the organic peroxide is selected from the group consisting of peroxycarboxylic acid esters. , peroxycarbonate, peroxy ketal.
  • the target product organic peroxide is a product conforming to the standard of commercial industrial products. Further, the chloride ion content of the target product organic peroxide is ⁇ 0.05wt%, and the content of other organic peroxide impurities is ⁇ 0.1. Wt%, the other organic peroxide impurities are selected from any one or any of a plurality of H 2 O 2 , an alkane peroxide, a dialkyl peroxide.
  • the temperature of the temperature zone 1 is 0 to 100 ° C, preferably 0 to 80 ° C, more preferably 0 to 60 ° C, still more preferably 0 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 10 to 200 ° C, preferably 20 to 180 ° C, more preferably 30 to 160 ° C, still more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, More preferably, it is 70 to 100 ° C, and more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 60 ° C, preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 5 to 100 ° C, preferably 20 to 90 ° C, more preferably 30 to 80 ° C, still more preferably 40 to 70 ° C, still more preferably 50 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 60 ° C, preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 60 ° C, preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature in the temperature zone will have a deviation of ⁇ 3 °C.
  • reaction substrate of the step (a) is preferably selected from the group consisting of tert-butanol, tert-amyl alcohol, cumene, 1,4-diisopropylbenzene, p-mentane, decane, tetrahydronaphthalene, 2, 4, 4-trimethyl-2-pentanol, 1,3-diisopropylbenzene, dihydroxy-1,4-diisopropylbenzene, dihydroxy-1,3-diisopropylbenzene.
  • reaction substrate has a flow rate of 0.2 to 10 L/h, preferably 0.5 to 8 L/h, more preferably 1 to 6 L/h.
  • the acid of step (a) is selected from all known organic and inorganic acids, preferably sulfuric acid, acetic acid or hydrochloric acid.
  • the acid solution has a mass concentration of 50% to 90%, preferably 60% to 80%, more preferably 70% to 80%.
  • the acid flow rate is 0.2 to 5 L/h, preferably 0.4 to 4 L/h, more preferably 0.5 to 3 L/h.
  • the base of the step (a) is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides.
  • the material, the alkaline earth metal hydroxide or the water-soluble metal carbonate is more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the alkali liquid has a mass concentration of 5% to 45%, preferably 15% to 35%, more preferably 20% to 30%.
  • the lye flow rate is 0.2 to 10 L/h, preferably 0.3 to 9 L/h, more preferably 0.5 to 8 L/h.
  • the acyl compound in the condensing agent in the step (a) is selected from the group consisting of acetyl chloride, propionyl chloride, butyryl chloride, isobutyryl chloride, valeryl chloride, 2-methylbutyryl chloride, pivaloyl chloride, 2-methylpentanoyl chloride , 2-ethylbutyryl chloride, 2-ethylhexanoyl chloride, decanoyl chloride, 2,4,4-trimethylpentanoyl chloride, 3,5,5-trimethylhexanoyl chloride, neodecanoyl chloride, decanoyl chloride, laurel Acid chloride, benzoyl chloride, 2-methylbenzoyl chloride, 4-methylbenzoyl chloride, 4-chlorobenzoyl chloride, 2,4-dichlorobenzoyl chloride, naphthoyl chloride, methyl chloroformate, chloroformic acid Ethyl
  • the flow rate of the acyl compound or the condensation raw material is 0.2 to 8 L/h, preferably 0.3 to 6 L/h, more preferably 0.5 to 4 L/h.
  • the molar ratio of the acid to the reaction substrate is from 0.3:1 to 1.5:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1.
  • the molar ratio of the oxidizing agent to the reaction substrate is from 0.8:1 to 2.2:1, preferably from 0.9:1 to 2.1:1, more preferably from 1:1 to 2:1, still more preferably from 1.3:1 to 1.8:1.
  • the molar ratio of the base to the reaction substrate is from 0.7:1 to 2:1, preferably from 0.9:1 to 1.8:1, more preferably from 1:1 to 1.6:1, still more preferably from 1:1 to 1.4:1.
  • the molar ratio of the acyl compound to the reaction substrate is from 0.5:1 to 1.2:1, preferably from 0.6:1 to 1.1:1, more preferably from 0.7:1 to 1:1.
  • the molar ratio of the condensation raw material to the reaction substrate is from 0.5:1 to 1.2:1, preferably from 0.6:1 to 1.1:1, more preferably from 0.7:1 to 1:1.
  • the oxidizing agent is selected from the group consisting of hydrogen peroxide and oxygen.
  • the target product of the online full continuous flow production process is t-butyl peroxy neodecanoate
  • the reaction substrate is t-butanol
  • the acyl compound is neodecanoyl chloride
  • the oxidant is hydrogen peroxide
  • the temperature of the temperature zone 1 is preferably 5 to 70 ° C, more preferably 5 to 60 ° C, still more preferably 5 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 30 to 160 ° C, more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, still more preferably 70 to 100 ° C, still more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 20 to 90 ° C, more preferably 30 to 80 ° C, still more preferably 40 to 70 ° C, still more preferably 50 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the tert-butyl peroxy neodecanoate is ⁇ 68%; preferably, the yield of t-butyl peroxy neodecanoate is ⁇ 81%.
  • the content of the tert-butyl peroxy neodecanoate is ⁇ 87%; preferably, the content of t-butyl peroxy neodecanoate is ⁇ 91%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in tert-butyl peroxy neodecanoate, a content of other organic peroxide impurities of 0.05 to 0.08% by weight, and the other organic peroxide impurity is H 2 . O 2 and di-tert-butyl peroxide.
  • the post-treatment temperature is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the t-butanol flow rate is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the neodecanoyl chloride flow rate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to tert-butanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-butanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-butanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of the neodecanoyl chloride to tert-butanol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the hydrogen peroxide concentration is 30% to 50%
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the reaction substrate is 2,4,4-trimethyl Base-2-pentanol
  • the acyl compound is neodecanoyl chloride
  • the oxidizing agent is hydrogen peroxide
  • the temperature of the temperature zone 1 is preferably 5 to 70 ° C, more preferably 5 to 60 ° C, still more preferably 5 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 30 to 160 ° C, more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, still more preferably 70 to 100 ° C, still more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 20 to 90 ° C, more preferably 30 to 80 ° C, still more preferably 40 to 70 ° C, still more preferably 50 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the peroxynonanoic acid-1,1,3,3-tetramethylbutyl ester is ⁇ 65%; preferably, neodecanoic acid-1,1,3,3-tetramethylbutyl ester The yield is ⁇ 70%.
  • the content of the peroxy neodecanoic acid-1,1,3,3-tetramethylbutyl ester is ⁇ 80%; preferably, the peroxy neodecanoic acid-1,1,3,3-tetramethylbutyl ester The content is ⁇ 90%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in neodecanoic acid-1,1,3,3-tetramethylbutyl ester, and the content of the other organic peroxide impurities is 0.05 to 0.1 wt. %, the other organic peroxide impurity is H 2 O 2 .
  • the hydrogen peroxide concentration is 30% to 50%
  • the flow rate of the 2,4,4-trimethyl-2-pentanol is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 11 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the neodecanoyl chloride flow rate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to 2,4,4-trimethyl-2-pentanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, more It is preferably 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the 2,4,4-trimethyl-2-pentanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, more Preferably 1.05:1 to 1.2:1.
  • the molar ratio of the base to 2,4,4-trimethyl-2-pentanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of the neodecanoyl chloride to 2,4,4-trimethyl-2-pentanol is from 0.7:1 to 1.1:1, preferably from 0.8:1 to 1:1, more preferably from 0.8:1 to 0.95:1. .
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is tert-butyl 2-ethylhexyl carbonate, the reaction substrate is tert-butanol, and the acyl compound is 2-ethylhexyl chloroformate.
  • the oxidizing agent is hydrogen peroxide, wherein, preferred:
  • the temperature of the temperature zone 1 is preferably 5 to 70 ° C, more preferably 5 to 60 ° C, still more preferably 5 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 30 to 160 ° C, more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, still more preferably 70 to 100 ° C, still more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 10 to 90 ° C, more preferably 20 to 80 ° C, still more preferably 30 to 70 ° C, still more preferably 40 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the hydrogen peroxide concentration is 30% to 50%
  • the yield of the tert-butyl 2-ethylhexylcarbonate is ⁇ 70%; preferably, the yield of tert-butyl 2-ethylhexylcarbonate is ⁇ 81%.
  • the content of the tert-butyl 2-ethylhexyl carbonate is ⁇ 95%; preferably, the content of tert-butyl 2-ethylhexyl carbonate is ⁇ 97%.
  • the target product has a chloride ion content of 0.03 to 0.05 wt% in 2-ethylhexylcarbonate tert-butyl ester and a content of other organic peroxide impurities of 0.05 to 0.08 wt%, and the other organic peroxide impurities. It is H 2 O 2 and di-tert-butyl peroxide.
  • the t-butanol flow rate is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the flow rate of the 2-ethylhexyl chloroformate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to tert-butanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-butanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-butanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of 2-ethylhexyl chloroformate to tert-butanol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is peroxyphenyl neodecanoate
  • the reaction substrate is cumene
  • the acyl compound is neodecanoyl chloride
  • the oxidant is oxygen.
  • the temperature of the temperature zone 1 is preferably 0 to 80 ° C, more preferably 10 to 70 ° C, still more preferably 20 to 60 ° C, still more preferably 30 to 40 ° C.
  • the temperature of the temperature zone 2 is preferably 20 to 180 ° C, more preferably 30 to 150 ° C, still more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, still more preferably 70 to 100 ° C, more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is preferably from 10 to 100 ° C, more preferably from 20 to 80 ° C, still more preferably from 30 to 60 ° C, still more preferably from 40 to 50 ° C.
  • the temperature of the temperature zone 5 is preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the cumene peroxy neodecanoate is ⁇ 79%; preferably, the yield of cumene peroxy neodecanoate is ⁇ 81%.
  • the content of the cumene peroxy neodecanoate is ⁇ 89%; preferably, the content of cumene peroxy neodecanoate is ⁇ 94%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in cumene neodecanoate, a content of other organic peroxide impurities of 0.05 to 0.1% by weight, and the other peroxide impurities are two different.
  • Propylbenzene hydrogen peroxide is a compound that has a chloride ion content of 0.03 to 0.05% by weight in cumene neodecanoate, a content of other organic peroxide impurities of 0.05 to 0.1% by weight, and the other peroxide impurities are two different.
  • Propylbenzene hydrogen peroxide Propylbenzene hydrogen peroxide.
  • the cumene flow rate is 0.2 to 8 L/h, preferably 0.5 to 6 L/h, more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the neodecanoyl chloride flow rate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of oxygen to cumene is from 0.8:1 to 2.2:1, preferably from 1.3:1 to 2.1:1, more preferably from 1.5:1 to 2:1.
  • the molar ratio of the base to cumene is from 1:1 to 1.8:1, preferably from 1.2:1 to 1.6:1, more preferably from 1.3:1 to 1.5:1.
  • the molar ratio of the neodecanoyl chloride to cumene is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is t-butyl isopropyl acrylate
  • the reaction substrate is t-butanol
  • the acyl compound is isopropyl chloroformate
  • the oxidant is hydrogen peroxide
  • the temperature of the temperature zone 1 is preferably 5 to 70 ° C, more preferably 5 to 60 ° C, still more preferably 5 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 30 to 160 ° C, more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, still more preferably 70 to 100 ° C, still more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 20 to 90 ° C, more preferably 30 to 80 ° C, still more preferably 40 to 70 ° C, still more preferably 50 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the tert-butyl isopropyl peroxycarbonate is ⁇ 70.5%; preferably, the yield of tert-butyl isopropylperoxycarbonate is ⁇ 80%.
  • the content of the tert-butyl peroxyperoxycarbonate is ⁇ 95%; preferably, the content of t-butyl isopropylperoxycarbonate is ⁇ 97%.
  • the target product has a chloride ion content of 0.03 to 0.05% by weight in tert-butyl peroxydicarbonate, a content of other organic peroxide impurities of 0.05 to 0.08% by weight, and the other organic peroxide impurity is H. 2 O 2 and di-tert-butyl peroxide.
  • the t-butanol flow rate is from 1 to 8 L/h, preferably from 1.5 to 6 L/h, more preferably from 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the flow rate of the isopropyl chloroformate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to tert-butanol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-butanol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-butanol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of isopropyl chloroformate to tert-butanol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the hydrogen peroxide concentration is 30% to 50%
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • the target product of the online full continuous flow production process is t-amyl 2-ethylhexyl carbonate
  • the reaction substrate is tert-amyl alcohol
  • the acyl compound is 2-ethylhexyl chloroformate.
  • the oxidizing agent is hydrogen peroxide, wherein: preferred:
  • the temperature of the temperature zone 1 is preferably 5 to 70 ° C, more preferably 5 to 60 ° C, still more preferably 5 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 30 to 160 ° C, more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, still more preferably 70 to 100 ° C, still more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 20 to 90 ° C, more preferably 30 to 80 ° C, still more preferably 40 to 70 ° C, still more preferably 50 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the production time of the production process is ⁇ 10 min, preferably, the production time is 3-9 min; more preferably, the production time is 4-8 min; more preferably, the production time is 5-7 min. .
  • the yield of the tert-amyl 2-ethylhexylcarbonate is ⁇ 70%; preferably, the yield of tert-amyl 2-ethylhexylcarbonate is ⁇ 81%.
  • the content of the tert-amyl 2-ethylhexylcarbonate is ⁇ 95%; preferably, the content of the tert-amyl 2-ethylhexylcarbonate is ⁇ 97%.
  • the target product has a chloride ion content of 0.03 to 0.05 wt% in 2-ethylhexylcarbonate t-amyl ester and a content of other organic peroxide impurities of 0.05 to 0.08 wt%, and the other organic peroxide impurities It is H 2 O 2 and di-tert-amyl peroxide.
  • the flow rate of the tert-amyl alcohol is 1 to 8 L/h, preferably 1.5 to 6 L/h, more preferably 2 to 4 L/h.
  • the acid flow rate is 0.4 to 5 L/h, preferably 0.5 to 4 L/h, more preferably 1 to 3 L/h, still more preferably 1.5 to 2.5 L/h.
  • the lye flow rate is 0.4 to 9 L/h, preferably 0.8 to 7 L/h, more preferably 1 to 6 L/h, still more preferably 1.2 to 5 L/h, still more preferably 1.5 to 3 L/h.
  • the flow rate of the 2-ethylhexyl chloroformate is 0.4 to 7 L/h, preferably 0.8 to 6 L/h, more preferably 1 to 5 L/h, still more preferably 1.5 to 4 L/h, still more preferably 2 to 3 L/h.
  • the molar ratio of the acid to tert-amyl alcohol is from 0.3:1 to 1.3:1, preferably from 0.4:1 to 1.2:1, more preferably from 0.5:1 to 1:1, still more preferably from 0.5:1 to 0.8:1.
  • the molar ratio of the hydrogen peroxide to the tert-amyl alcohol is from 0.8:1 to 1.5:1, preferably from 0.9:1 to 1.4:1, more preferably from 1:1 to 1.3:1, still more preferably from 1.05:1 to 1.2:1.
  • the molar ratio of the base to tert-amyl alcohol is from 0.9:1 to 1.6:1, preferably from 1:1 to 1.4:1, more preferably from 1.2:1 to 1.3:1.
  • the molar ratio of 2-ethylhexyl chloroformate to tert-amyl alcohol is from 0.5:1 to 1.1:1, preferably from 0.6:1 to 1:1, more preferably from 0.7:1 to 0.9:1.
  • the hydrogen peroxide concentration is 30% to 50%
  • the base is selected from the group consisting of water-soluble metal hydroxides, water-soluble quaternary ammonium hydroxides, water-soluble tertiary amines, water-soluble metal carbonates or water-soluble metal phosphates, preferably alkali metal hydroxides, alkaline earth metal hydroxides Or a water-soluble metal carbonate, more preferably sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lithium hydroxide.
  • the acid is selected from all known organic and inorganic acids, preferably sulfuric acid, phosphoric acid or trifluoroacetic acid.
  • reaction substrate, oxidant and condensing agent used in actual production have a deviation of ⁇ 2 percentage points of mass concentration; the temperature of the temperature zone will be ⁇ 3. Deviation of °C; production time will have a deviation of ⁇ 5s.
  • the present invention provides a scheme for the direct and continuous production of an organic peroxide from a reaction substrate, i.e., a plurality of reactants are continuously fed into the reactor, and the reaction product is continuously collected.
  • a reaction substrate i.e., a plurality of reactants are continuously fed into the reactor, and the reaction product is continuously collected.
  • the stability and reliability are good, so the product quality is stable and reproducible; the process has no amplification effect, and the problem of the amplification effect of the industrial process of the organic peroxide continuous flow process is also solved; and the integrated continuous flow reaction Because there is no need to delay the pipeline, the volume is small and the floor space is small, which greatly saves the land for the plant.
  • a second object of the present invention is to provide a plug-and-play integrated continuous flow reactor dedicated to any one form of online full continuous flow production process as described above, said integrated continuous flow reactor
  • a unitary structure comprising an oxidative condensation unit and a post-treatment unit, wherein: the oxidative condensation unit is used to react a reaction substrate, an oxidizing agent and a condensing agent to form a peroxycarboxylic acid ester, a peroxycarbonate and a peroxy ketal
  • the post-treatment unit is used for purification and washing of the organic peroxide, and the organic peroxide is selected from the group consisting of a peroxycarboxylic acid ester, a peroxycarbonate, and a peroxyketal.
  • a third object of the present invention is to provide a plug-and-play integrated continuous flow reactor dedicated to any form of on-line full continuous flow production as described above, said integrated continuous flow reactor
  • each of the units independently comprises more than one reactor module or group of reactor modules, wherein the reactor module group is composed of a plurality of reactor modules connected in series or in parallel, and the units are connected in series with each other.
  • a fourth object of the present invention is to provide a plug-and-play integrated continuous flow reactor dedicated to any one form of online full continuous flow production process as described above, said integrated continuous flow reactor Using a unitized structure, each of said units comprises at least one temperature zone, each temperature zone independently comprising more than one reactor module or group of reactor modules, wherein the reactor module group is connected in series or in parallel by a plurality of reactor modules Composition, each temperature zone is connected in series with each other.
  • the above three continuous flow reactors can further be:
  • the unit further includes a buffer between the units, and the buffer is a container having a certain volume, which is mainly used for buffering the pressure fluctuation of the system and balancing the flow difference, so that the system works more smoothly.
  • the number of the integrated continuous flow reactor feed ports is one or more, and the number of the integrated continuous flow reactor discharge ports is one or more.
  • the reactor module is optionally any reactor capable of realizing a continuous flow process, the reactor being selected from the group consisting of a microreactor, a Tandem loop reactor, and a tube. Any one or any of a variety of reactors (Tubularreactor).
  • the microreactor also known as a microstructure reactor or a microchannel reactor, is a device in which a chemical reaction occurs in a limited area with a general lateral dimension of 1 mm or less. The form is a miniature size channel.
  • a tandem coil reactor that is, a reactor in which a coil reactor is connected in series by a pipe, wherein the coil reactor is in the form of a tubular reactor.
  • the tubular reactor is a continuous operation reactor with a tubular shape and a large aspect ratio which appeared in the middle of the last century.
  • Such a reactor can be very long; it can be a single tube or a plurality of tubes in parallel; it can be an empty tube or a filling tube.
  • the reactor may be one or more.
  • the reactor channel is made of single crystal silicon, special glass, ceramic, stainless steel or metal alloy coated with a corrosion resistant coating, and polytetrafluoroethylene.
  • reactor modules, the reactor module groups, the reactor modules and the reactor module groups are respectively connected in series or in parallel.
  • the integrated continuous flow reactor comprises six temperature zones.
  • the oxidative condensation reaction unit of the integrated continuous flow reactor comprises four temperature zones, namely, a temperature zone 1, a temperature zone 2, a temperature zone 3 and a temperature zone 4, and the post-processing unit comprises two temperature zones. It is temperature zone 5 and temperature zone 6, respectively.
  • the temperature of the temperature zone 1 is 0 to 100 ° C, preferably 0 to 80 ° C, more preferably 0 to 60 ° C, still more preferably 0 to 40 ° C, still more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 2 is 10 to 200 ° C, preferably 20 to 180 ° C, more preferably 30 to 160 ° C, still more preferably 40 to 130 ° C, still more preferably 50 to 120 ° C, still more preferably 60 to 110 ° C, More preferably, it is 70 to 100 ° C, and more preferably 80 to 90 ° C.
  • the temperature of the temperature zone 3 is 0 to 60 ° C, preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 4 is 5 to 100 ° C, preferably 20 to 90 ° C, more preferably 30 to 80 ° C, still more preferably 40 to 70 ° C, still more preferably 50 to 60 ° C.
  • the temperature of the temperature zone 5 is 0 to 60 ° C, preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • the temperature of the temperature zone 6 is 0 to 60 ° C, preferably 0 to 50 ° C, preferably 0 to 40 ° C, more preferably 5 to 30 ° C, still more preferably 5 to 20 ° C.
  • a fifth object of the present invention is to provide a chemical production process comprising the online continuous continuous flow production process for directly preparing an organic peroxide from an alcohol or an alkane according to the present invention, and one or more Subsequent production process.
  • the chemical production process may be a polymerization process, and the organic peroxide produced by the online full continuous flow production process of the present invention acts as an initiator of the polymerization process, and seamlessly interfaces the process of the present invention with the polymerization process. It can form a complete continuous production and use of organic peroxides, subvert the existing production-storage-transport-storage-use production mode, and realize a new production mode of production and use.
  • a sixth object of the present invention is to provide a chemical production facility comprising the plug-and-production integrated continuous flow reactor of the online full continuous flow production process of any one of the forms described in the present invention, And one or more subsequent production equipment.
  • the chemical production equipment may be a polymer production equipment
  • the plug-and-play integrated continuous flow reactor of the present invention can directly interface with the polymerization tank, and can form an organic peroxide production and use.
  • the full continuous production equipment subverting the existing production-storage-transport-storage-use production mode, to achieve a new production mode of production and use.
  • the present invention has the following beneficial effects:
  • the invention completely improves the prior art process for producing organic peroxide by integrating the reaction process and the advantages of the plug-and-production integrated continuous flow reactor, and realizes the safe starting material (alcohol or alkane for the first time).
  • Direct production of highly hazardous organic peroxides, macroscopically non-hazardous alkyl peroxides (intermediate products) accumulation, purification and residence waiting processes, avoiding the purification, storage and transport steps of alkyl peroxides It realizes the production and use of organic peroxides at the same time, and realizes the on-line manufacturing.
  • the production and use of the products are carried out at the same time, and the downstream processes and equipment are seamlessly connected and synchronized to the production mode.
  • the production process of the present invention is completely different from the prior art process, only through one-step reaction, and the reaction process and the post-treatment process are integrated into a complete production process, which is directly produced in a short time (within 15 minutes). Products that meet the standards of commercially available industrial products have achieved high quality and high efficiency production.
  • the production process of the invention has strong versatility, and the organic integration of the reaction process and the reactor organically breaks the existing defects that the production process of different organic peroxides cannot be universalized, by adjusting different process parameters and reactor parameters.
  • the production of different kinds of organic peroxides can be realized on the same plug-and-production integrated continuous flow reactor, which meets various needs of users and improves production efficiency.
  • the production process of the invention is safe and efficient, and the obtained organic peroxide product has high yield and content, greatly reduces production cost, improves safety of production of organic peroxides and production of downstream products, and realizes organic peroxidation. High efficiency, high quality and large-scale production.
  • the invention solves the problem of industrialized amplification of the organic peroxide continuous flow process, the production process of the invention has no amplification effect, greatly reduces the difficulty of industrial application, and does not need to go through complicated and complicated times when it is enlarged to industrialization. Step-by-step amplification and adjustment of process conditions and parameters can be scaled up to the required production scale, greatly saving manpower and material resources and project development time.
  • the safety of the production process of the present invention is greatly improved, the relatively small liquid holding capacity and excellent heat transfer characteristics of the continuous flow reactor, and the shorter reaction time (within 15 minutes) make the process more Safety.
  • the liquid holding capacity of the reactor refers to the total volume of the reaction materials stored in the reactor at any time when the operation reaches a steady state.
  • the reaction time of the invention is greatly shortened, the reaction time is shortened by 95%, and the reaction efficiency is greatly improved.
  • the product quality is stable and reproducible due to stable flow rate and stable production process.
  • the integrated continuous flow reactor is small in size and small in area, which greatly saves the land for the plant.
  • Figure 1 is a process diagram of the continuous production process of the present invention
  • Figure 2 is a schematic illustration of the integrated reactor of the present invention.
  • NSC904 2,4,4-trimethyl-2-pentanol
  • IPCF isopropyl chloroformate
  • ACL Acetyl chloride
  • the concentrations in the examples of the present invention are all mass concentrations, and the content of the target product is measured by effective oxygen content titration (iodine method), the chloride ion content is detected by an ion detector, and other organic peroxides are passed through high performance liquid chromatography (HPLC), the target product of the present invention has a chloride ion content of 0.03 to 0.05%, and other organic peroxide content of 0.05 to 0.1%, and the other organic peroxide impurities are selected from the group consisting of H 2 O 2 and alkane peroxide. Any one or any of a plurality of dialkyl peroxides. There is no need to delay the line in the reactor.
  • reaction substrate, oxidant and condensing agent used in actual production have a deviation of ⁇ 2 percentage points of mass concentration; the temperature of the temperature zone will be ⁇ 3. Deviation of °C; production time will have a deviation of ⁇ 5s.
  • the raw material 1 sulfuric acid solution
  • the raw material 2 reaction substrate
  • the raw material 3 aqueous hydrogen peroxide solution
  • the raw material 4 alkaline solution
  • the raw material 5 acyl compound
  • the feed rate 1 represents the feed rate of the feedstock 1
  • the feed rate 2 represents the feed rate of the feedstock 2
  • the feed rate 3 represents the feed rate of the feedstock 3
  • the feed rate 4 represents the feed rate of the feedstock 4
  • Feed rate 5 represents the feed rate of feedstock 5.
  • raw material 1 sulfur solution
  • raw material 2 reaction substrate
  • raw material 3 aqueous hydrogen peroxide solution
  • raw material 4 acid solution
  • raw material 5 condensation raw material
  • the feed rate 1 represents the feed rate of the feedstock 1
  • the feed rate 2 represents the feed rate of the feedstock 2
  • the feed rate 3 represents the feed rate of the feedstock 3
  • the feed rate 4 represents the feed rate of the feedstock 4
  • Feed rate 5 represents the feed rate of feedstock 5.
  • the raw material 1 (alkaline solution), the raw material 2 (reaction substrate), the raw material 3 (oxygen), the raw material 4 (alkaline solution), and the raw material 5 (acyl compound) are sequentially conveyed by a constant flow pump.
  • the continuous reactor enters the temperature zone 1 to the temperature zone 4 in turn, and the reaction is complete; the reaction liquid flowing out of the temperature zone 4 enters the temperature zone 5 and the temperature zone 6 for post-treatment to obtain a pure product.
  • the feed rate 1 represents the feed rate of the feedstock 1
  • the feed rate 2 represents the feed rate of the feedstock 2
  • the feed rate 3 represents the feed rate of the feedstock 3
  • the feed rate 4 represents the feed rate of the feedstock 4
  • Feed rate 5 represents the feed rate of feedstock 5.
  • Examples 84 and 85 employ the procedures of Examples 27-28, and Examples 78-83 and Examples 86-92 employ the procedures of Examples 1-12.
  • the continuous flow production of the organic peroxide of the present invention has a great advantage in time, from several hours or even ten hours of the existing process to less than 10 minutes, and in the overall The yield and content are somewhat improved compared to the prior art. Meanwhile, it can be seen from Examples 11 and 12, 25 and 26, 37 and 38, 49 and 50, 61 and 62, 73 and 74, 76 and 77, 91 and 92 that the yield does not change after scale-up, and the production time is also Not increasing again, indicating that the present invention does not have an amplification effect.

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Abstract

公开了一种由醇或烷烃直接制备有机过氧化物的全连续流生产工艺，所述的生产工艺以非常安全的醇或烷烃为起始原料，直接反应得到指定过氧化物，所述的生产工艺在一体化连续流反应器中进行，在所述一体化连续流反应器的进料口不间断加入安全的起始原料醇或烷烃，在所述一体化连续流反应器出料口不间断得到指定过氧化物，所述的生产工艺安全高效，可实现就地生产且无放大效应。与传统的生产工艺相比，生产时间缩短为15分钟内，可现做现用完全零库存，且无放大效应，产品指标稳定、重现性好。

Description

一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺 技术领域
本发明涉及化学领域，具体涉及一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺，所述的有机过氧化物为易燃易爆的化合物。
背景技术
有机过氧化物是指过氧化氢中的氢原子被烷基、酰基、芳香基等有机基团置换而形成的含有-O-O-过氧官能团的有机化合物。特征是受热超过一定温度后会分解产生含氧自由基，不稳定、易分解。化工生产的有机过氧化物主要是用来作合成树脂的聚合引发剂、催化剂。在高分子材料领域，有机过氧化物用作自由基聚合的引发剂、接枝反应的引发剂、橡胶和塑料的交联剂、不饱和聚酯的固化剂以及纺丝级聚丙烯制备中的分子量及分子量分布调节剂。有机过氧化物是用于下面用途中自由基的来源：①乙烯基与二烯单体的自由基聚合和共聚合引发剂；②热固性树脂的硫化剂；③弹性体和聚乙烯的交联剂。
除上述高分子材料工业外，有机过氧化物作为光引发剂和增感剂用于胶片工业，用于感光性高分子材料，感光树脂等，也常用于环氧树脂的生产；医用材料方面，有机过氧化物与药物组成的引发剂，用于合成药物缓释给药基质(如微球、微丸、药膜)；有机合成方面,有机过氧化物主要用作氧化剂和环氧化剂。另外，有机过氧化物还应用于医疗器械和食品的消毒、纺织品、纸张等日化工业的漂白剂、脱色剂、杀菌剂、清洗剂等。
过氧化羧酸酯和过氧化碳酸酯是重要的有机过氧化物，如过氧化～2～乙基己基碳酸叔丁酯、过氧化新癸酸异丙苯酯和过氧化新癸酸-1,1,3,3-四甲基丁酯。过氧化羧酸酯和过氧化碳酸酯是自由基聚合反应的低温引发剂，广泛用于聚乙烯(LDPE)、聚氯乙烯(PVC)、聚苯乙烯(PS)、苯乙烯共聚物(如，ABS)、聚甲基丙烯酸酯(PMMA)和聚醋酸乙烯酯(PVAc)等生产领域。同时，其也是不饱和聚酯的高温固化剂。而过氧化缩酮主要用于不饱和聚酯的交联剂、橡胶和塑料的引发剂。目前国内外市场对于过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮需求越来越大，所以开发有机过氧化物的连续生产工艺具有现实意义和远大的前景。
有机过氧化物是非常活泼的化合物，极易分解为高反应活性的自由基和氧，该过程中会释放大量的热甚至引发爆炸。作为有机过氧化物，其重要特征是自加速分解温度(SADT)，在等于或高于自加速分解温度下，有机过氧化物分解反应放热速率与环境散热速率是失衡的，即体系热量在不断累积，此时，有机过氧化物可通过热分解导致危险的自加速分解反应和在不利环境下的爆炸或起火。与不相容的物质接触以及提高机械应力可导致在等于或低于SADT下的分解。
有机过氧化物在温度的作用下会发生分解，这是由于存在可在约84～184kJ/mol的能量范围△H内打开的氧-氧键，所述能量范围取决于该有机过氧化物的性质。这就是说不同的有机过氧化物发生分解打开氧-氧键时所需的能量是因各自性质而不同的。因此，不同有机过氧化物，自分解加速温度和热稳定性会有很大差异。例如，过氧化羧酸酯类过氧化物过氧化新癸酸异丙苯酯(CNP)的自分解加速温度(SADT)为10℃，10小时半衰期对应的温度为38℃；过氧化新戊酸叔丁酯(TBPV)的自分解加速温度(SADT)为20℃，10小时半衰期对应的温度为57℃；过氧化新癸酸叔丁酯的自分解加速温度(SADT)则为15℃，10小时半衰期对应的温度为46℃；过氧化碳酸酯类过氧化物过氧化2-乙基己基碳酸叔丁酯(TBEC)自分解加速温度(SADT)则为60℃，10小时半衰期对应的温度为100℃；过氧化缩酮类过氧化物1,1-二(叔丁基过氧化)环己烷自分解加速温度(SADT)则为70℃，10小时半衰期对应的温度为94℃。同时由于结构差异，不同有机过氧化物的合成路线和所需原料都不同的，原料的物理、化学性质也千差万别。这众多差异导致不存在一个所谓“通用”的工艺过程能适用所有的有机过氧化物，导致不同的有机过氧化物的生产工艺难以相互移植套用。每个具体有机过氧化物的生产都需要根据其自加速分解温度和热稳定性以及使用原料的物理、化学性质来专门设计开发个性化的适用工艺过程、条件和参数。
现有技术制备过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮包括以下两步反应：
第一步是氧化反应，醇或烷烃与氧化剂反应合成烷基过氧化物R(OOH) n和二烷基过氧化物ROOR，经过分离纯化步骤，去除二烷基过氧化物ROOR等杂质和水，得到氧化反应的产品烷基过氧化物R(OOH) n，反应通式如下：
Figure PCTCN2018100115-appb-000001
第二步是缩合反应，烷基过氧化物R(OOH) n与碱和酰基化合物反应，合成过氧化羧酸酯或过氧化碳酸 酯，反应通式如下：
Figure PCTCN2018100115-appb-000002
烷基过氧化物R(OOH) n与酸和醇或酮反应合成过氧化缩酮，反应通式如下：
Figure PCTCN2018100115-appb-000003
其中，R选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基、无取代或取代的环烷基。
R 1选自饱和或不饱和的C 1-C 20烷基、无取代或取代的芳基、无取代或取代的杂环芳基。
R 2选自饱和或不饱和的C 1-C 20烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基。
R 3选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基。
R 4或R 4’选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基。
化工产品的工业化生产过程的改进，主要指的是对工艺的改进。所述的工艺是指利用各种设备将原料进行加工或反应，得到最终产品的方法与过程，是化学反应或物理过程结合设备通过调整温度、压力、物料配比等技术参数得到产品的一个过程，也就是，生产工艺是指将化学反应或物理过程在工业化尺度实现的过程。生产工艺与反应并非一一对应关系，一个工艺可以包含一个反应，也可以包含多个反应。化学产品的制备过程包含的反应和对应的反应路线是由其反应机理所决定的，但对于相同的反应路线，可以由不同的生产工艺来实现。生产工艺优化改进可能达到的效果有：第一，提高生产效率，增加产能，降低生产成本；第二，改善工艺安全性；第三，提高产品质量；第四，降低“三废”排放。
工业化生产过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮的过程中，氧化反应、缩合反应分别对应氧化工艺和缩合工艺。其中，氧化反应和缩合反应都是油水两相反应，反应效率低，反应体系中存在大量的水。第一步氧化反应所用的氧化剂为液体氧化剂(例如：双氧水)或气体氧化剂(例如：氧气)，氧化反应带来的两个问题是：1)受氧化工艺所限，氧化剂必然无法全部转化，并且不可避免地会生成二烷基过氧化物，二烷基过氧化物、没有反应完全的氧化剂就成为了氧化工艺的杂质，必须要除去这些杂质才能进行下一步缩合反应。例如，使用双氧水作为氧化剂时，过氧化物杂质(二烷基过氧化物和双氧水)会直接影响最终产品(过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮)的品质。由于不同有机过氧化物自加速分解温度和半衰期不同，使用有机过氧化物就是利用这不同的自加速分解温度和半衰期等特性，因此有机过氧化物一般不能混用，尤其是自加速分解温度和半衰期等相差很大的有机过氧化物更不能混用，否则会严重影响使用效果。例如，目标产物为过氧化新癸酸叔丁酯，过氧化新癸酸叔丁酯的SADT为15℃，10h半衰期对应的温度为46℃，制备过氧化新癸酸叔丁酯过程生成的二叔丁基过氧化氢的SADT为80℃，10h半衰期对应的温度为121℃，不同浓度双氧水的SADT和半衰期各不相同，常温下(通常为25℃)双氧水在淡水中的半衰期为8小时到20天，可见三者SADT和半衰期相差很大，三者混合物无法满足单一使用需求。因此在过氧化新癸酸叔丁酯的合成过程中，氧化反应后必须要去除二烷基过氧化物和双氧水，否则，会严重影响过氧化新癸酸叔丁酯的品质性能。2)大量的水和杂质会影响缩合反应浓度，进而影响反应速率，导致生产效率大大降低。而使用氧气作为氧化剂时其主要杂质是碳酸钠、引发剂和水，同样存在以上两个问题，一是引发剂通常为自由基引发剂如偶氮二异丁氰(SADT为50℃，10h半衰期分解温度为65℃)、二异丙苯过氧化氢(SADT为75℃，10h半衰期分解温度为117℃)等，如不除去混入最终产品中也会影响产品品质性能，二是水等杂质会影响反应速率，进而影响生产效率，如文献中提到高压釜中加入500g二异丙苯、200g水、20gNa 2CO 3和6g偶氮二异丁氰加压反应60h合成二过氧化氢二异丙苯，静止，分离水相得到上层油相才能进行下一步反应(新型交联剂双叔丁基过氧化二异丙苯的合成研究,化学世界,2008(1):38～41)。
现有合成过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮的生产工艺中，氧化工艺后得到的产物为包含烷基过氧化物、杂质、大量的水的混合物，为了保证缩合工艺的有效进行，需经过纯化过程去除混合物中的杂质和大量的水，制得符合市售工业品标准的烷基过氧化物(如市售叔丁基过氧化氢要求如下：二叔丁基过氧化物≤0.08％，叔丁醇≤0.5％，其他有机物≤0.4％)。所述的纯化工艺可以是气液分离、酸碱法、减压精馏或蒸馏、闪蒸分离等，纯化过程通常采用的是间歇工艺，中国专利CN106588734中提到异丙苯过氧化氢提纯步骤包括气液分离、闪蒸分离和浓缩，中国专利CN102617432中提到合成叔丁基过氧化氢后静置分层得到上层有机相，向有机相中加入碱液反应温度10～50℃，反应时间0.5～4h，静置分层，去除上层有机相，下层水相和氯代酯进一步反应得到过氧化2-乙基己基碳酸叔丁酯。可见，制备不同的烷基过氧化物所需的纯化工艺不同，还需要单独的设备如精馏塔等，并且所需的设备也大多不同，现有工艺没有一种通用的设备和工艺能做到可以纯化各种烷基过氧化物。
同时，现有缩合工艺后得到的只是过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮粗品，含有水、烷基过氧化物、盐等，还需进行后处理工艺后才能得到符合市售标准的产品(如市售过氧化新癸酸叔丁酯要求如下：氯离子含量≤0.05％，叔丁基过氧化氢含量≤0.1％)，所述后处理工艺可以是分离、碱洗、水洗、减压精馏或蒸馏、闪蒸分离、干燥等，中国专利CN102558399中提到过氧化新癸酸叔丁酯的后处理方法为在反应结束后静置20-40min，分离母液，将反应生成物洗至pH值5～7，加入烷烃溶剂在0℃以下搅拌20-30min得到溶剂型过氧化新癸酸叔丁酯产品，后处理时间大于40min；中国专利CN102336694中提到1,1-二(叔丁基过氧化)环己烷的后处理方法为反应母液碱洗、水洗，得到中性反应液，经减压蒸馏得到无色液体即为产品1,1-二(叔丁基过氧化)环己烷，参考现有后处理工艺常规时间为1-2小时。现有后处理工艺耗时长，效率低，同时还需要单独设备如精馏塔等，不同过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮后处理工艺也不同，现有生产工艺中也没有一种通用的设备和工艺能做到可以纯化各种不同过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮。
因此，现有工艺生产得到符合市售标准的过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮需要分成四步，第一步为氧化工艺，其产物为包含烷基过氧化物、杂质和大量的水的混合物；第二步为纯化工艺，除杂质和大量的水，制得符合市售工业品要求的烷基过氧化物(即中间产品)，并将其存储备用；第三步为缩合工艺，制得目标产物(过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮)粗品；第四步后处理工艺，除去杂质和水，制得符合市售工业品要求的过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮。现有生产工艺中，在氧化工艺后必然累积一定量的烷基过氧化物，即宏观上存在中间产品的累积和存储；烷基过氧化物经过纯化后才用于下一步缩合工艺，即过程中存在中间产品纯化工艺和相关操作流程。这说明氧化工艺和缩合工艺实质上是两个相互独立工艺，因此，现有工艺制备过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮从整体上来说都是间歇工艺。此外所述的烷基过氧化物属于易燃易爆危险品，因此该类化合物累积、存储和纯化等过程存在很大的安全风险，并且由于所述的烷基过氧化物易燃易爆对温度异常敏感，需要冷链储存和运输，这大大增加了使用和生产成本。现有技术存在烷基过氧化物的累积、存储和纯化，无法将氧化工艺和缩合工艺无缝衔接，实现从醇或烷烃全连续直接制备过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮；同时由于现有工艺没有一种通用的后处理设备和工艺，无法将氧化、缩合工艺和后处理工艺结合在一起实现全连续，因此需要储存一定量的过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮，而且所述的过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮属于易燃易爆危险品，因此该类化合物存储和后处理等过程存在很大的安全风险，并且由于所述的过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮易燃易爆对温度异常敏感，需要冷链储存和运输，这进一步增加了使用和生产成本。
其中，所述烷基过氧化物通式为R(OOH) n，其中，R选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基、无取代或取代的环烷基。
进一步地，R选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基、无取代或取代的环烷基。
进一步地，R选自叔丁基、叔戊基、异丙苯基、1，4-二异丙苯基、2,4,4-三甲基-2-戊基、2,5-二甲基己基。
进一步地，烷基过氧化物选自：
叔丁基过氧化氢CAS No.：75-91-2、叔戊基过氧化氢CAS No.：3425-61-4、CAS No.：4212-43-5、1，1，3，3-四甲基丁基过氧化氢CAS No.：5809-08-5、异丙苯过氧化氢CAS No.：80-15-9、2,5-二甲基-2,5双(过氧化氢)己烷CAS No.：3025-88-5、二羟基-1,4-二异丙基苯CAS No.：3159-98-6。
间歇工艺最重要的特征有两点，一是过程中存在“停留”或“中断”，二是产品生产是间隔开的，即产品存在批次并且一个批次生产只能得到固定数量的产品。也就是，对于每一批次的生产，固定数量的原料按 照反应步骤的顺序进行反应，最终得到有限的固定数量的产品(产物)；然后再投入固定数量的原料，按照同样的步骤进行下一批次的反应，制得有限的固定品。
间歇工艺实现的方式有两种：1)分别用多个反应器(例如，烧瓶、反应釜等)实现，每一步反应在一个反应器中进行；2)用一个反应器(例如，烧瓶、反应釜等)实现，在该反应器中依次完成每步反应，反应过程中需要根据反应进程依次添加多个原料，也就是每一步反应后，就会有“停留”，等待进一步添加后续反应的原料。有的文献也把方式2)称作连续(continuous)，其实质也是间歇的，因为过程中存在“停留”，需等待加料，或者需要为下一步反应调节到合适的温度(例如，升温、降温或保温)。
间歇工艺主要存在以下问题:
1.间歇批次操作效率不高，反应时间很长，生产周期非常长，工艺过程中必然有氧化产物(即中间产品)烷基过氧化物的存在，而且还需要冷链储存和运输大量的氧化产物和最终产品，造成产品使用和生产成本长期居高不下。
2.第一步氧化工艺无论是使用氧气自氧化法，还是使用双氧水氧化法，间歇工艺反应器持液量大，单次反应需要大量纯氧或双氧水，因此间歇工艺存在很大的安全隐患。
3.第三步缩合工艺大都是放热反应，需要反应器具有很好的换热性能，保证反应不飞温。一旦温度过高，产品会发生分解，使收率降低。现有间歇工艺主要通过控制氧化剂的加入速度(缓慢滴加或缓慢通气)结合相应的移热装置来实现对反应温度的控制，这样一是大大延长了操作时间，降低了生产效率；二是由于大量过氧化物长时间存在，工艺安全隐患很大，并没有从根本上解决工艺安全性问题。即间歇工艺安全性、产品收率和质量稳定性都亟待改善。
4.间歇工艺不可避免地会带来放大效应(Scaling up Effect)，给工业上生产规模放大带来很大障碍。
所述的放大效应是指利用小型设备进行化工过程(即小规模)实验(例如实验室规模)得出的研究结果，在相同的操作条件下与大型生产装置(例如工业化规模)得出的结果往往有很大差别。有关这些差别的影响称为放大效应。其原因主要是小规模的实验设备中的温度、浓度、物料停留时间分布与大规模设备中的不同。也就是说，相同的操作条件下，无法在工业化规模上完全重复小规模实验的研究结果；若要在工业化规模上得到与小规模实验相同或近似的结果，需要通过优化调整，改变工艺参数和操作条件。对于化工过程来说，放大效应是一个难度较大而且迫切需要解决的问题。如果不解决，会导致生产过程和产品质量具有很大的不确定性，一是直接导致下游产品的质量不稳定，难以控制；二是不确定性会带来生产过程工艺参数波动，进而导致无法有效控制生产过程，使得生产安全性不能得到保证，为生产过程埋下诸多安全隐患。
现地生产是指生产厂家将设备安置到终端消费者(或下游使用者)就近或同一地点进行生产，从而很大程度减少了从生产厂家到终端消费者(或下游使用者)之间的众多中间环节如仓储，物流等，节约了大量成本。但是现地生产仍无法避免少量产品的储存和运输，例如，从工厂的一个车间运送到另一个车间，从合成产品的生产设备取出产品并运送至下游的生产设备。在线生产(on-line manufacturing)作为现地生产的一种，是指产品的生产和使用同时进行，与下游工艺无缝衔接、同步联动的生产方式，从而实现产品的即产即用(produce-to-use)、随用随产(ready-to-use)的弹性生产模式(flexible manufacturing)。实现在线生产，需要借助于即插即产型生产装置(plug-and-produce system)。所谓即产即用，就是产出即使用，产品的生产和使用同时进行；随用随产，就是随时需要随时产出，无须等待，按需生产零库存；即插即产型生产装置，就是生产装置开动后即时获得产品，按需生产，满足需求后即可停车。在线生产的生产时间可以缩短至十余分钟甚至数分钟内，可以和下游使用者的生产设备和生产工艺实现无缝对接，从根本上避免了产品的储存和运输，节约了成本、提高了生产的安全性，也提高了生产效率。所述的生产时间是指从原料进入反应器到符合市售产品输出所需的时间，包括反应时间和后处理时间，在连续流工艺中也称其为停留时间(residence time)。在线生产作为一种高度灵活的生产方式，除了与其它现地生产方式一样可以节约大量仓储、物流等成本外，同时能有效地满足快速、个性化和定制化的产品需求，也符合工业化4.0和智能制造主导的第四次工业革命的发展方向。
本发明的有机过氧化物一体化全连续流工艺和反应器，可以直接无缝衔接到下游终端用户的工艺和反应器上，实现即产即用，甚至可能实现整个工艺过程中宏观上没有过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮的累积和累积过程。一体化全连续流工艺可直接与高分子材料领域的聚合釜，胶片工业的硫化机等连接，形成有机过氧化物的生产和使用的全连续，颠覆现有生产-存储-运输-储存-使用生产模式，实现生产即使用的新型生产模式，有机过氧化物在线生产，即产即用，按需生产，零库存无物流。例如过氧化2-乙基己基碳酸叔丁酯作为交联剂，是目前太阳能组件中EVA胶膜最关键的核心原料，本发明的一体化连续流反应器可以与EVA膜硫化机无缝衔接，符合市售标准的过氧化2-乙基己基碳酸叔丁酯从一体化连续流反应器流出后，直接与硫化机的配料釜相连，随后进入硫化机真空层压得到EVA膜，最后裁剪包装。真正做到生产就是使用，没有过氧化2-乙基己基碳酸叔丁酯的累积和储存，一方面大大提高了整体工艺的安全 性，另一方面进一步降低了生产成本，大幅度提高了生产效率。
有机过氧化物是非常活泼的化合物，极易分解为高反应活性的自由基和氧，该过程中会释放大量的热甚至引发爆炸，因此有机过氧化物对温度异常敏感，必须低温储存和运输。现有工艺过程存在大量氧化反应产品(烷基过氧化物)和产品(过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮)的累积、纯化、存储和运输，两者均为易燃易爆的有机过氧化物，因此现有有机过氧化物生产成本的1/3用于中间产品和产品的冷链储存和运输。而在线生产是在需要使用产品时按需进行生产，即产即用、随用随产，实现产品零库存、无运输，这将大大降低有机过氧化物生产和使用中的库存和物流成本，同时也将其中的安全风险降到了最低。但现有工艺尚无法实现从醇或烷烃直接生产过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮连续流工艺以及与之匹配适用的即插即产型反应器，因此无法做到上述有机过氧化物的真正意义上的在线生产，也就无法从根本上解决有机过氧化物的生产和使用中巨大的安全风险并降低生产和使用成本。
中国专利CN101479239描述了使用具有高热交换能力的板式换热器来连续制备有机过氧化物的方法，通过在板式换热器不同位置(板块)引入不同的反应物，在给定的温度下连续制备选定的过氧化物。其温度给定值为这样的温度，即高于该温度时有机过氧化物变得热敏感。这表明其反应温度给定值均低于相应有机过氧化物SDAT，最终优选的反应温度范围为5～60℃。相比较间歇工艺，产率接近虽温度更高，不过要低于相应有机过氧化物SADT。合成反应时间在实验室规模为1秒到45秒的范围内，而在工业规模上最高达2分钟到3分钟。所述反应时间是指反应物料进入反应器中到反应结束得到目标产品粗品所需的时间，不包括后处理的时间。相比间歇工艺，该连续制备方法在生产效率和安全性上有一定的优势，但是由于不可避免地存在了放大效应，其工业规模反应时间是实验室规模的2～180倍，存在大幅度不确定(反应时间2～180倍极宽范围的延长)的放大效应，大大增加了工业化的难度。这种大幅度不确定的放大效应会给该工艺的工业化应用带来诸多不利，例如，在向工业化放大时，只能采取多次逐级放大的方法，并且为了获得与实验室规模一致性的结果，每次放大过程都要重新调整优化工艺条件和参数，这会极大地消耗人力物力和项目开发的时间；即使采用多次逐级放大，由于放大效应变化幅度太大，也可能最终导致放大后无法达到实验室规模的好结果；同时大幅度不确定的放大效应会影响工艺的稳定性和可靠性，导致产品质量不稳定，难以控制；另外，这也会给生产过程带来潜在的安全风险。同时，该专利仅报道醇或烷烃生产烷基过氧化物的连续工艺或烷基过氧化物生产过氧酯的连续工艺，但不能实现以醇或烷烃为起始原料全连续直接生产过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮。
中国专利CN102617432描述了以叔丁醇为原料生产过氧化2-乙基己基碳酸叔丁酯的方法，但该专利存在的问题如下：
一是生产工艺中在相当一段时间内仍存在大量氧化产物叔丁基过氧化氢累积、纯化和停留等待等流程，正如上面所说这带来了很大的安全隐患，并且为保证生产安全，这些过程中需要维持低温，大大增加了生产成本；
二是从叔丁醇到生产过氧化2-乙基己基碳酸叔丁酯的整个过程都是间歇工艺，在工业放大时必然会存在放大效应，极大地增加了工业放大的难度；
三是生产时间需要3～18小时，反应时间长，生产效率低，不可能实现在线生产，即产即用。
综上，有机过氧化物现有生产工艺中存在诸多问题：相当一段时间内仍存在有机过氧化物(包括氧化反应产品和产品)的累积、纯化、存储和运输过程；使得工艺存在极大的安全隐患；尚无法实现从醇或烷烃直接生产过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮全连续流工艺以及与之匹配适用的即插即产型反应器，因此无法做到上述有机过氧化物的真正意义上的在线生产，这些都造成其无法从根本上解决有机过氧化物的生产和使用中巨大的安全风险并降低生产和使用成本。此外，现有工艺均存在不同程度的放大效应，导致向工业化放大时会消耗大量人力物力且存在诸多不确定性；放大后工艺可靠性也存在问题，导致产品质量不稳定，难以控制；并且生产过程缺乏灵活性并且会有潜在的安全风险；由于反应温度低，导致反应总时间过长且产率不高，降低了生产效率，这些都增加了工业化的难度。而无法实现大规模生产，就限制了其应用。因此，需要寻找一种操作简单安全，高效，能够在线生产，易于大规模生产且无放大效应的有机过氧化物的全连续流生产工艺。
发明内容
针对现有技术是不足，本发明所要解决的技术问题是，提供一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺，所述的有机过氧化物为过氧化羧酸酯、过氧化碳酸酯或过氧化缩酮，该生产工艺从安全的起始物(醇或烷烃)直接生产危险程度高的有机过氧化物，宏观上没有危险的烷基过氧化物(即中间产品)的累积、纯化和停留等待的过程，实现了有机过氧化物的即产即用，而且还克服了放大效应问题，同时实现了在线生产(on-line manufacturing)，所述有机过氧化物产品的生产和使用同时进行，与下游工艺无缝衔接、同步联动的生产方式，从而实现产品的即产即用(produce-to-use)、随用随产(ready-to-use) 的弹性生产模式(flexible manufacturing)，该工艺操作简单安全、高效，不存在放大效应，制得的有机过氧化物产品产率和含量高，易于大规模生产，大幅度降低生产成本、提高有机过氧化物生产和下游产品生产的安全性。
术语说明：
本文所用术语“芳基”是指5到12个碳原子的全碳单环或稠合多环基团，具有完全共轭的π电子系统。芳环的非限制性实例有：苯环、萘环和蒽环。芳环可以是无取代或取代的。芳环的取代基选自卤素、硝基、氨基、氰基、羟基、C 1-C 6烷基、C 1-C 6烷氧基、卤代C 1-C 6烷基、卤代C 1-C 6烷氧基、C 3-C 6环烷基、卤代C 3-C 6环烷基。
本文所用术语“杂环芳基”指5到12个环原子的不饱和的碳环，其中一个或多个碳原子被杂原子如N、O、S等置换。杂芳环可以是单环，也可以是双环，即通过两个环稠合而成。具体的杂环芳基可以是：吡啶基，嘧啶基，吡嗪基，异恶唑基，异噻唑基、吡唑基、噻唑基、恶唑基和咪唑基等。杂环芳基可以是无取代或取代的。杂环芳基的取代基选自卤素、硝基、氨基、氰基、羟基、C 1-C 6烷基、C 1-C 6烷氧基、卤代C 1-C 6烷基、卤代C 1-C 6烷氧基、C 3-C 6环烷基、卤代C 3-C 6环烷基。
本文所用术语“杂环烷基”指单环或稠合环基团，在环中具有5到12个环原子，其中一个或两个环原子是选自N、O或S(O) m(其中m是0至2的整数)的杂原子，其余环原子是C。这些环可以包含一个或多个双键，但这些环不具有完全共轭的π电子系统。无取代的杂环烷基的可以是吡咯烷基、哌啶基、哌嗪基、吗啉代基、硫代吗啉代基、高哌嗪基等。杂环可以是无取代或取代的。杂环的取代基选自卤素、硝基、氨基、氰基、羟基、C 1-C 6烷基、C 1-C 6烷氧基、卤代C 1-C 6烷基、卤代C 1-C 6烷氧基、C 3-C 6环烷基、卤代C 3-C 6环烷基。
本文所用术语“环烷基”是指具有3到12个碳原子的饱和单环碳环，除非指明不同数目的原子。环烷基包括环丙基、环丁基、环戊基、环己基、环庚基和环辛基等。环烷基可以是无取代或取代的。环烷基还可任选在任何可利用碳上被一个或多个选自烷氧基、卤素、卤代烷基如全氟烷基等取代基取代。
本专利所用术语“烷基”包括直链烷基和支链烷基。如提及单个烷基如“丙基”，则只特指直链烷基，如提及单个支链烷基如“异丙基”，则只特指支链烷基。例如，“C1-6烷基”包括C1-4烷基、C1-3烷基、甲基、乙基、正丙基、异丙基和叔丁基。
本专利所用术语“烷氧基”是指含有-O-烷基基团，其中烷基如上所定义。本专利所用“烷氧基”的实例包括但不限于甲氧基、乙氧基、正丙氧基、异丙氧基、正丁氧基和叔丁氧基。“烷氧基”还包括取代烷氧基。烷氧基可任选被一个或多个卤素原子取代。
连续生产工艺(连续工艺，continuous process)是指生产过程中生产系统各生产步骤之间相互衔接，整体上保证持续运行，但每个步骤中允许停留等待。连续流生产工艺(连续流工艺，continuous-flowprocess)作为连续工艺的一种，是一种快速高效的全流程连续工艺，具有用时短、效率高、易操作等特点，过程中连续不间断地加入原料，连续不间断地生产制得产品，过程中物料(即包含有原料、中间体、产品、溶剂等的反应混合物)是连续流动的，没有间断，没有停留等待，即产品被源源不断地生产出来，是一种“流水线”式的化工生产过程。当工艺操作达到定态时，反应器内任何位置上物料的组成、温度等状态参数不随时间而变化，是稳态过程，因而生产过程和产品质量都是稳定的。在包含有多步反应的工艺中，如果其中某几个步骤是连续的或者只是将原有间歇工艺中的各步骤简单连接起来，该工艺可以称为半连续工艺；而只有所有步骤都是连续的并且物料在整个工艺过程中是连续流动的，即连续加入原料，连续得出产品，才能称为连续流工艺(或者全流程连续工艺)。现有技术生产过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮等有机过氧化物的工艺，氧化反应和缩合反应是分别进行的，从整个工艺过程来说，氧化和缩合是两个分别进行的步骤，因此是间歇工艺。
为解决本发明的技术问题，本发明创新性地提供一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺，所述的生产工艺以非常安全的物料醇或烷烃为起始反应原料，连续依次经氧化缩合和后处理两个过程制得有机过氧化物，所述的生产工艺在即插即产型一体化连续流反应器中进行，在所述一体化连续流反应器的进料口不间断加入反应底物、氧化剂和缩合剂，在所述一体化连续流反应器出料口不间断得到目标产品有机过氧化物，所述的生产工艺无放大效应，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮，所述的反应底物为醇或烷烃，所述缩合剂在生产过氧化羧酸酯、过氧化碳酸酯时为碱液和酰基化合物，在生产过氧化缩酮时为酸液和缩合原料，所述缩合原料为醇或酮。
本发明通过集成反应工艺和即插即产型一体化连续流反应器的优势，彻底改进了现有技术生产有机过氧化物的工艺，能够实现有机过氧化物的在线全连续流生产，将氧化缩合过程与后处理过程有效地整合为一个工艺，不仅实现了从安全的起始物(醇或烷烃)直接生产危险程度高的有机过氧化物，宏观上没有危险的烷基过氧化物(中间产品)的累积、纯化和停留等待的过程，避免了烷基过氧化物的纯化、储存和运输步骤，实现了有机过氧化物的即产即用，而且还克服了放大效应问题，同时实现了在线生产(on-line  manufacturing)，产品的生产和使用同时进行，与下游工艺和设备无缝衔接、同步联动的生产方式，从而实现产品的即产即用(produce-to-use)、随用随产(ready-to-use)的弹性生产模式(flexible manufacturing)。也就是随时需要随时产出，无须等待，按需生产零库存，按需生产，满足需求后即可停车。不仅保证了有机过氧化物的优质高效生产，还能与与下游工艺无缝衔接、同步联动，进而可以避免目标产品有机过氧化物的储存和运输步骤，从根本上解决了烷基过氧化物和最终产品(过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮)冷链仓储和运输的成本及安全性问题。
本发明生产工艺通式如下：
Figure PCTCN2018100115-appb-000004
其中，A 1为醇或烷烃，A 2选自酰氯、氯甲酸酯、醇、酮，氧化剂选自双氧水和氧气，C选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
进一步地，A 1为醇的通式为R(OH) n，其中n＝1,2,3...；A 1为烷烃的通式为R(H) n，其中n＝1,2,3...；A 2为酰氯的通式为R 1COCl；A 2为氯甲酸酯的通式为R 2OCOCl；A 2为醇的通式为R 3(OH) m，其中m＝1,2,3...；A 2为酮的通式为R 4R 4’(CO)或R 4(CO)(环内酮)；n，m为正整数。
C为过氧化羧酸酯的通式为R(OOOCR 1) n，其中n＝1,2,3...；C为过氧化碳酸酯的通式为R(OOOCOR 2) n，其中n＝1,2,3...；C为过氧化缩酮的通式为R 4(OOR) 2，其中n＝1；C为过氧化缩酮的通式为R 3(OOR) m，其中n＝1，m＝1,2,3...；C为过氧化缩酮的通式为R(OOR 3) n，其中m＝1，n＝1,2,3...；n，m为正整数。
R选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基、无取代或取代的环烷基；
R 1选自饱和或不饱和的C 1-C 20烷基、无取代或取代的芳基、无取代或取代的杂环芳基；
R 2选自饱和或不饱和的C 1-C 20烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基；
R 3选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基；
R 4或R 4’选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基；
优选的，
R选自饱和或不饱和的C3-C8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环、无取代或取代的环烷基；
R 1选自饱和或不饱和的C 1-C 18烷基、无取代或取代的芳基、无取代或取代的杂环芳基；
R 2选自饱和或不饱和的C1-C18烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环，无取代或取代的环烷基；
R 3选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环，无取代或取代的环烷基；
R 4或R 4’选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环，无取代或取代的环烷基；
更优选的，
R选自叔丁基、叔戊基、异丙苯基、1，4-二异丙苯基、2,4,4-三甲基-2-戊基、2,5-二甲基己基、1，3-二异丙苯基；
R 1选自甲基、乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异戊基、正戊基、异庚基、辛基、异辛基、2,2-二甲基庚基、壬基、十一烷基、苯基、2-甲基苯基、4-甲基苯基、4-氯苯基、2，4-二氯苯基、萘基；
R 2选自甲基、乙基、丙基、异丙基、丁基、仲丁基、2-乙基己基、异十三烷基、十七烷基、环己基、4-叔丁基环己基、苄基、苯氧乙基；
R 3选自叔丁基、叔戊基、2,5-二甲基己基、1,4-二异丙苯基、1,3-二异丙苯基；
R 4或R 4’选自甲基、乙基；R 4选自-(CH 2) 5-、-CH 2-C(CH 3) 2-CH 2-CH(CH 3)-CH 2-；
更优选的，
R(OH) n选自叔丁醇、叔戊醇、2,4,4-三甲基-2-戊醇、2,5-二甲基-2,5双羟基己烷、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯；
R(H) n选自异丙苯、1，4-二异丙苯、1，3-二异丙苯；
R 1COCl选自乙酰氯、丙酰氯、丁酰氯、异丁酰氯、戊酰氯、2-甲基丁酰氯、新戊酰氯、2-甲基戊酰氯、2-乙基丁酰氯、2-乙基己酰氯、壬酰氯，2,4,4-三甲基戊酰氯、3,5,5-三甲基己酰氯、新癸酰氯、癸酰氯、月桂酰氯、苯甲酰氯、2-甲基苯甲酰氯、4-甲基苯甲酰氯、4-氯苯甲酰氯、2，4-二氯苯甲酰氯、萘甲酰氯；
R 2OCOCl选自氯甲酸甲酯、氯甲酸乙酯、氯甲酸正丙酯、氯甲酸异丙酯、氯甲酸正丁酯、氯甲酸仲丁酯、氯甲酸2-乙基己酯、氯甲酸异十三烷基酯、氯甲酸硬脂酯、氯甲酸环己酯、氯甲酸4-叔丁基环己酯、氯甲酸苄酯、氯甲酸2-苯氧基乙酯；
R 3(OH) n选自叔丁醇、叔戊醇、2,4,4―三甲基―2-戊醇、2,5-二甲基-2,5双羟基己烷、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯；
R 4R 4’(CO)选自甲乙酮；R 4(CO)选自环己酮、3,3,5-三甲基环己酮。
进一步地，所述有机过氧化物选自：
过氧化苯甲酸叔丁酯CAS No.：614-45-9、过氧化苯甲酸叔戊酯CAS No.：4511-39-1、过氧化乙酸叔丁酯CAS No.：107-71-1、过氧化特戊酸叔丁酯CAS No.：927-07-1、过氧化特戊酸叔戊酯CAS No.：29240-17-3、过氧化新癸酸叔丁酯CAS No.：26748-41-4、过氧化新癸酸叔戊酯CAS No.：68299-16-1、过氧化2-乙基己酸叔丁酯CAS No.：3006-82-4、过氧化2-乙基己酸叔戊酯CAS No.：686-31-7、过氧化异丁酸叔丁酯CAS No.:109-13-7、过氧化新庚酸叔丁酯CAS No.：26748-38-9、过氧化3,5,5-三甲基己酸叔丁酯CAS No.：13122-18-4、过氧化2-乙基己基碳酸叔丁酯CAS No.：34443-12-4、过氧化2-乙基己基碳酸叔戊酯CAS No.：70833-40-8、1,1-二叔丁基过氧化-3,3,5-三甲基环己烷CAS No.：6731-36-8、1,1-二(叔丁基过氧化)环己烷CAS No.：3006-86-8、2,2-二(叔丁基过氧化)丁烷CAS No.：2167-23-9、过氧化新癸酸异丙苯酯CAS No.：26748-47-0、过氧化新癸酸-1,1,3,3-四甲基丁酯CAS No.：51240-95-0、过氧化特戊酸1,1,3,3-四甲基丁酯CAS No.：22288-41-1、1,1,3,3-四甲基丁基过氧化-2-乙基己酸酯CAS No.：22288-43-3、1,1-二特戊基过氧化环己烷CAS No.：15667-10-4、过氧化乙酸特戊酯CAS No.：690-83-5、过氧化异丙基碳酸叔丁酯CAS No.：2372-21-6、叔丁基过氧化异丙苯CAS No.：3457-61-2。
本发明的生产工艺宏观上没有危险的烷基过氧化物(中间产品)的累积、纯化和停留等待的过程，实现了以醇或烷烃为起始反应底物，全连续制得有机过氧化物(过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮)，创新性地实现了有机过氧化物的在线生产，即产即用，突破了现有工艺的局限性。
所述烷基过氧化物通式为R(OOH) n，其中，R选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环、无取代或取代的环烷基，n≥1，n为正整数。
进一步地，R选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环、无取代或取代的环烷基。
进一步地，R选自叔丁基、叔戊基、异丙苯基、1,4-二异丙苯基、2,4,4-三甲基-2-戊基、2,5-二甲基己基。
进一步地，烷基过氧化物选自：
叔丁基过氧化氢CAS No.：75-91-2、叔戊基过氧化氢CAS No.：3425-61-4、CAS No.：4212-43-5、1，1，3，3-四甲基丁基过氧化氢CAS No.：5809-08-5、异丙苯过氧化氢CAS No.：80-15-9、2,5-二甲基-2,5双(过氧化氢)己烷CAS No.：3025-88-5、二羟基-1,4-二异丙基苯CAS No.：3159-98-6。
本发明工艺制得的目标产品有机过氧化物是符合市售工业品标准的产品，进一步地，所述目标产品有机过氧化物中的氯离子含量≤0.05wt％，其他有机过氧化物杂质的含量≤0.1wt％，所述其他有机过氧化物杂质选自H 2O 2、烷烃过氧化物、二烷烃过氧化物的任意一种或任意多种。
进一步地，本发明工艺的生产时间≤15min，优选的所述的生产时间≤10min；更优选的，所述的生产时间为3～13min；更优选的，所述的生产时间为4～11min；更优选的，所述的生产时间为5～10min。所述的生产时间是指从反应原料(反应底物、氧化剂和缩合剂)进入所述一体化连续流反应器到制得符合市售标准的目标产品输出所需的时间，包括氧化缩合过程的时间和后处理过程的时间。
进一步地，所述有机过氧化物的收率≥64％；优选的，所述有机过氧化物的收率≥75％；更优选的，所述有机过氧化物的收率≥81％。
进一步地，所述有机过氧化物的含量≥77％；优选的，所述有机过氧化物的含量≥85％；所述有机过氧化物的含量≥97％。
进一步地，所述氧化缩合工艺的温度为0～200℃，优选0～180℃，更优选0～160℃，更优选0～140℃，更优选5～130℃。
进一步地，所述后处理的温度为0～60℃，优选0～50℃，更优选0～40℃，更优选0～30℃，更优选5～30℃。
进一步地，所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
进一步地，所述碱液质量浓度为5％～45％，优选15％～35％，更优选20％～30％。
进一步地，所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述酸液质量浓度50％～90％，优选60％～80％，更优选70％～80％。
进一步地，所述氧化剂选自双氧水、氧气。
进一步地，所述反应底物选自叔丁醇、叔戊醇、异丙苯、1，4-二异丙苯、对孟烷、蒎烷、四氢萘、2,4,4-三甲基-2-戊醇、1，3-二异丙苯、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯。
进一步地，所述缩合剂中的酰基化合物选自乙酰氯、丙酰氯、丁酰氯、异丁酰氯、戊酰氯、2-甲基丁酰氯、新戊酰氯、2-甲基戊酰氯、2-乙基丁酰氯、2-乙基己酰氯、壬酰氯，2,4,4-三甲基戊酰氯、3,5,5-三甲基己酰氯、新癸酰氯、癸酰氯、月桂酰氯、苯甲酰氯、2-甲基苯甲酰氯、4-甲基苯甲酰氯、4-氯苯甲酰氯、2，4-二氯苯甲酰氯、萘甲酰氯、氯甲酸甲酯、氯甲酸乙酯、氯甲酸正丙酯、氯甲酸异丙酯、氯甲酸正丁酯、氯甲酸仲丁酯、氯甲酸2-乙基己酯、氯甲酸异十三烷基酯、氯甲酸硬脂酯、氯甲酸环己酯、氯甲酸4-叔丁基环己酯、氯甲酸苄酯、氯甲酸2-苯氧基乙酯；所述缩合剂中的醇选自叔丁醇、叔戊醇；所述缩合剂中的酮选自环己酮，3,3,5-三甲基环己酮、甲乙酮。
进一步地，酸和反应底物的摩尔比为0.3:1～1.5:1，优选0.4:1～1.2:1，更优选0.5:1～1:1。
进一步地，氧化剂和反应底物的摩尔比为0.8:1～2.2:1，优选0.9:1～2.1:1，更优选1:1～2:1，更优选1.3:1～1.8:1。
进一步地，碱和反应底物的摩尔比为0.7:1～2:1，优选0.9:1～1.8:1，更优选1:1～1.6:1，更优选1:1～1.4:1。
进一步地，酰基化合物和反应底物的摩尔比为0.5:1～1.2:1，优选0.6:1～1.1:1，更优选0.7:1～1:1。
进一步地，缩合原料和反应底物的摩尔比为0.5:1～1.2:1，优选0.6:1～1.1:1，更优选0.7:1～1:1。
进一步地，所述反应底物流速为0.2～10L/h，优选0.5～8L/h，更优选1～6L/h。
进一步地，所述酸液流速为0.2～5L/h，优选0.4～4L/h，更优选0.5～3L/h。
进一步地，所述碱液流速为0.2～12L/h，优选0.3～9L/h，更优选0.5～8L/h。
进一步地，所述酰基化合物或缩合原料流速为0.2～8L/h，优选0.3～6L/h，更优选0.5～4L/h。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化新癸酸叔丁酯，所述反应底物为叔丁醇，所述酰基化合物为新癸酰氯，所述氧化剂为双氧水，其中，优选的：
所述双氧水质量浓度为30％～50％，
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化新癸酸叔丁酯的收率≥68％；优选的，过氧化新癸酸叔丁酯的收率≥81％。
所述过氧化新癸酸叔丁酯的含量≥87％；优选的，过氧化新癸酸叔丁酯的含量≥91％。
所述目标产品过氧化新癸酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述叔丁醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述新癸酰氯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述新癸酰氯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化新癸酸-1,1,3,3-四甲基丁酯时，所述反应底物为2,4,4-三甲基-2-戊醇，所述酰基化合物为新癸酰氯，所述氧化剂为双氧水，其中，优选的：
所述双氧水质量浓度为30％～50％；
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化新癸酸-1,1,3,3-四甲基丁酯的收率≥65％；优选的，过氧化新癸酸-1,1,3,3-四甲基丁酯的收率≥70％。
所述过氧化新癸酸-1,1,3,3-四甲基丁酯的含量≥80％；优选的，过氧化新癸酸-1,1,3,3-四甲基丁酯的含量≥90％。
所述目标产品过氧化新癸酸-1,1,3,3-四甲基丁酯中的氯离子含量为0.03～0.05wt％，所述其他有机过氧化物杂质的含量为0.05～0.1wt％，所述其他有机过氧化物杂质是H 2O 2。
所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述2,4,4-三甲基-2-戊醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～11L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述新癸酰氯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和2,4,4-三甲基-2-戊醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和2,4,4-三甲基-2-戊醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和2,4,4-三甲基-2-戊醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述新癸酰氯和2,4,4-三甲基-2-戊醇的摩尔比为0.7:1-1.1:1，优选0.8:1～1:1，更优选0.8:1～0.95:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔丁酯，所述反应底物为叔丁醇，所述酰基化合物为氯甲酸-2-乙基己酯，所述氧化剂为双氧水，其中，优选的：
所述双氧水质量浓度为30％～50％。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化2-乙基己基碳酸叔丁酯的收率≥70％；优选的，过氧化2-乙基己基碳酸叔丁酯的收率≥81％。
所述过氧化2-乙基己基碳酸叔丁酯的含量≥95％；优选的，过氧化2-乙基己基碳酸叔丁酯的含量≥97％。
所述目标产品过氧化2-乙基己基碳酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述叔丁醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述氯甲酸-2-乙基己酯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述氯甲酸-2-乙基己酯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、 碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化新癸酸异丙苯酯，所述反应底物为异丙苯，所述酰基化合物为新癸酰氯，所述氧化剂为氧气，其中，优选的：
所述生产工艺的的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化新癸酸异丙苯酯的收率≥79％；优选的，过氧化新癸酸异丙苯酯的收率≥81％。
所述过氧化新癸酸异丙苯酯的含量≥89％；优选的，过氧化新癸酸异丙苯酯的含量≥94％。
所述目标产品过氧化新癸酸异丙苯酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.1wt％，所述其他过氧化物杂质为二异丙苯过氧化氢。
所述氧化缩合工艺的温度为0～180℃，优选0～150℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
所述后处理的温度为0～60℃，优选0～50℃，更优选0～40℃，更优选0～30℃，更优选5～30℃。
所述异丙苯流速为0.2～8L/h，优选0.5～6L/h，更优选1.5～4L/h，更优选2～3L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述新癸酰氯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述氧气和异丙苯的摩尔比为0.8:1～2.2:1，优选1.3:1～2.1:1，更优选1.5:1～2:1。
所述碱和异丙苯的摩尔比为1:1～1.8:1，优选1.2:1～1.6:1，更优选1.3:1～1.5:1。
所述新癸酰氯和异丙苯的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐、水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化异丙基碳酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为氯甲酸异丙酯，氧化剂为双氧水，其中，优选的：
所述双氧水质量浓度为30％～50％。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化异丙基碳酸叔丁酯的收率≥70.5％；优选的，过氧化异丙基碳酸叔丁酯的收率≥80％。
所述过过氧化异丙基碳酸叔丁酯的含量≥95％；优选的，过氧化异丙基碳酸叔丁酯的含量≥97％。
所述目标产品过氧化异丙基碳酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述氯甲酸异丙酯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐、水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔戊酯，所述反应底物为叔戊醇，酰基化合物为氯甲酸-2-乙基己酯，氧化剂为双氧水，其中，优选的：
所述双氧水质量浓度为30％～50％。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述目标产品过氧化2-乙基己基碳酸叔戊酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔戊基。
所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述过氧化2-乙基己基碳酸叔戊酯的收率≥70％；优选的，过氧化2-乙基己基碳酸叔戊酯的收率≥81％。
所述过氧化2-乙基己基碳酸叔戊酯的含量≥95％；优选的，过氧化2-乙基己基碳酸叔戊酯的含量≥97％
所述酸和叔戊醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔戊醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔戊醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述氯甲酸-2-乙基己酯和叔戊醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐、水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
需要说明的是，实际生产中(包括实验室、中试、实际生产过程中)所用的反应底物、氧化剂和缩合剂质量浓度都会有±3个百分点的质量浓度的偏差；温区温度会有±3℃的偏差；生产时间会有±3s的偏差。
由于本发明的解决方案以非常安全的物料为起始原料生产有机过氧化物，中间无烷基过氧化物存在，也就无需危险的氧化产物——烷基过氧化物进行纯化和储存，且最终产品现做现用，没有了存储大量烷基过氧化物及产品(过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮)的安全隐患，同时也不存在放大效应，极大地降低了工业化应用的难度，在向工业化放大时，无需经历繁琐复杂的多次逐级放大和工艺条件、参数的调整优化，即可一次放大到所需要的生产规模，极大地节约了人力物力和项目开发时间；在工业化生产中，可灵活改变产品生产规模，无需重新调整优化工艺条件和参数，生产过程灵活性好；无放大效应使得生产过程稳定可靠，工艺条件和参数的波动也不会影响产品质量，产品质量易于控制；这也极大地提升了生产过程的安全性。
本发明的连续流工艺稳定性和可靠性好，因而产品质量稳定、重现性好；工艺也没有放大效应，也解决了有机过氧化物连续流工艺工业化存在放大效应的问题；同时该即插即产型一体化连续流反应器由于无需延迟管线，生产时间短，体积小，占地面积小，极大地节约了厂房用地和提高了生产效率。
为满足本发明连续流工艺的条件。本发明开发了专门的一体化反应器。所述的反应器可以是模块化的结构，需要设计模块的组织方式、数量，各温区包含的模块，还需要开发针对性的工艺条件和参数，包括各温区的划分和温度设置，以上各种因素发生协同作用，使得这一连续流工艺得以实现。还可以进一步地结合各温度与物料浓度、物料配比和物料流速，使之与反应进程相匹配，得到更好的反应效果。
本发明的生产工艺可以在高温下快速、连续地完成制备有机过氧化物的反应，利用功能单元划分和温度设置的优化以及功能单元的协同作用，反应总时间可缩短至15分钟内，甚至缩短至数分钟内，大大提升了工艺的效率。可见，本发明的生产工艺突破了现有技术的限制，在现有技术无法实现的苛刻、危险的条件下，成功了实现了有机过氧化物的高效率、高质量的生产，避免了烷基过氧化物的纯化、储存和运输步骤，实现了有机过氧化物的即产即用，不仅保证了有机过氧化物的优质高效生产，还能与与下游工艺无缝衔接、同步联动，进而可以避免目标产品有机过氧化物的储存和运输步骤。并且所述的生产工艺不存在放大效应，非常适合工业化生产，而且能够实现有机过氧化物的即产即用，无需冷链运输和储存，大幅度提高了生产和使用的安全性、降低了成本，是本领域的一项重大突破。
进一步地，为与有机过氧化物的全连续流生产工艺相匹配，所述即插即产型一体化连续流反应器采用单元化结构，包括氧化缩合单元和后处理单元，其中：所述的氧化缩合单元用于实现反应底物、氧化剂和缩合剂反应生成过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮，所述后处理单元用于所述有机过氧化物的纯化和清洗，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
进一步地，所述氧化缩合单元的温度为0～200℃，优选0～180℃，更优选0～160℃，更优选0～140℃，更优选5～130℃。
进一步地，所述后处理单元的温度为0～60℃，优选0～50℃，更优选0～40℃，更优选0～30℃，更优选5～30℃。
进一步地，为与有机过氧化物的全连续流生产工艺相匹配，所述即插即产型一体化连续流反应器采用单元化结构，每个所述的单元独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各单元之间相互串联。
进一步地，为与有机过氧化物的全连续流生产工艺相匹配，所述即插即产型一体化连续流反应器采用单元化结构，每个所述的单元包含至少一个温区，每个温区独立地包含一个以上的反应器模块或反应器模 块组，其中反应器模块组由多个反应器模块串联或并联组成，各温区之间相互串联。
进一步地，所述的单元之间还进一步包含缓冲器(Buffervessel)，所述的缓冲器为具有一定容积的容器，主要用于缓冲系统的压力波动和平衡流量差异，使系统工作更平稳。
进一步地，所述一体化连续流反应器进料口的数量为1个或多个，所述一体化连续流反应器出料口的数量为1个或多个。
进一步地，所述的反应器模块任选是任意一种能实现连续流工艺的反应器，所述的反应器选自微反应器(Microreactor)，串联盘管反应器(Tandem loop reactor)，管式反应器(Tubularreactor)的任意一种或任意多种。所述的微反应器，又称微结构反应器或微通道反应器，是一种在其中化学反应发生在普遍侧向尺寸在1mm及以下的有限区域内的设备，这类有限区域最典型的形式即是微型尺寸通道。串联盘管反应器，即用管道将盘管反应器串联起来组成的反应器，其中盘管反应器是将管式反应器做成盘管的形式。管式反应器是上个世纪中叶出现的一种呈管状、长径比很大的连续操作反应器。这种反应器可以很长；可以单管也可以多管并联；可以空管，也可以是填充管。
进一步地，反应器可以是一台或多台。
进一步地，所述反应器通道的材质为单晶硅、特种玻璃、陶瓷、涂有耐腐涂层的不锈钢或金属合金、聚四氟乙烯。
进一步地，所述的反应器模块之间、反应器模块组之间、反应器模块和反应器模块组之间均分别是串联或并联。
进一步地，所述的连续流生产工艺在包含6个温区的即插即产型一体化连续流反应器中进行。
进一步地，所述的连续流生产工艺的氧化缩合反应单元包含4个温区，分别为温区1，温区2，温区3和温区4，后处理单元包含2个温区，分别为温区5和温区6。当存在连续温区温度相同时，可视为同一个温区，例如温区1和温区2温度相同时，那么此时一体化反应器实际为5个温区，温区1(温区1+温区2)，温区3，温区4，温区5和温区6，其他的以此类推。
进一步地，所述的连续流生产工艺包括如下步骤：
(a)将反应底物、氧化剂和缩合剂输送进氧化缩合单元，依次经过温区1-温区4，完全反应生成相应的过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮；所述的反应底物为醇或烷烃，所述缩合剂在生产过氧化羧酸酯、过氧化碳酸酯时为碱液和酰基化合物，在生产过氧化缩酮时为酸液和缩合原料，所述缩合原料为醇或酮。
(b)流出温区4的反应液进入后处理单元，依次经过温区5和温区6进行后处理，得到目标产品有机过氧化物，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
所述的目标产品有机过氧化物是符合市售工业品标准的产品，进一步地，所述目标产品有机过氧化物中的氯离子含量≤0.05wt％，其他有机过氧化物杂质的含量≤0.1wt％，所述其他有机过氧化物杂质选自H 2O 2、烷烃过氧化物、二烷烃过氧化物的任意一种或任意多种。
进一步地，所述温区1的温度为0～100℃，优选0～80℃，更优选0～60℃，更优选0～40℃，更优选5～30℃，更优选5～20℃。
进一步地，所述温区2的温度为10～200℃，优选20～180℃，更优选30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
进一步地，所述温区3的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
进一步地，所述温区4的温度为5～100℃，优选20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
进一步地，所述温区5的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
进一步地，所述温区6的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
需要说明的是，实际生产中(包括实验室、中试、实际生产过程中)温区温度会有±3℃的偏差。
进一步地，步骤(a)所述反应底物优选自叔丁醇、叔戊醇、异丙苯、1，4-二异丙苯、对孟烷、蒎烷、四氢萘、2,4,4-三甲基-2-戊醇、1，3-二异丙苯、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯。
进一步地，所述反应底物流速为0.2～10L/h，优选0.5～8L/h，更优选1～6L/h。
进一步地，步骤(a)所述酸选自所有已知的有机酸和无机酸，优选硫酸、醋酸或盐酸。
进一步地，所述酸液质量浓度50％～90％，优选60％～80％，更优选70％～80％。
进一步地，所述酸液流速为0.2～5L/h，优选0.4～4L/h，更优选0.5～3L/h。
进一步地，步骤(a)所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性 金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
进一步地，所述碱液质量浓度为5％～45％，优选15％～35％，更优选20％～30％。
进一步地，所述碱液流速为0.2～10L/h，优选0.3～9L/h，更优选0.5～8L/h。
进一步地，步骤(a)所述缩合剂中的酰基化合物选自乙酰氯、丙酰氯、丁酰氯、异丁酰氯、戊酰氯、2-甲基丁酰氯、新戊酰氯、2-甲基戊酰氯、2-乙基丁酰氯、2-乙基己酰氯、壬酰氯，2,4,4-三甲基戊酰氯、3,5,5-三甲基己酰氯、新癸酰氯、癸酰氯、月桂酰氯、苯甲酰氯、2-甲基苯甲酰氯、4-甲基苯甲酰氯、4-氯苯甲酰氯、2，4-二氯苯甲酰氯、萘甲酰氯、氯甲酸甲酯、氯甲酸乙酯、氯甲酸正丙酯、氯甲酸异丙酯、氯甲酸正丁酯、氯甲酸仲丁酯、氯甲酸2-乙基己酯、氯甲酸异十三烷基酯、氯甲酸硬脂酯、氯甲酸环己酯、氯甲酸4-叔丁基环己酯、氯甲酸苄酯、氯甲酸2-苯氧基乙酯；所述缩合剂中的醇选自叔丁醇、叔戊醇；所述缩合剂中的酮选自环己酮，3,3,5-三甲基环己酮、甲乙酮。
进一步地，所述酰基化合物或缩合原料流速为0.2～8L/h，优选0.3～6L/h，更优选0.5～4L/h。
进一步地，酸和反应底物的摩尔比为0.3:1～1.5:1，优选0.4:1～1.2:1，更优选0.5:1～1:1。
进一步地，氧化剂和反应底物的摩尔比为0.8:1～2.2:1，优选0.9:1～2.1:1，更优选1:1～2:1，更优选1.3:1～1.8:1。
进一步地，碱和反应底物的摩尔比为0.7:1～2:1，优选0.9:1～1.8:1，更优选1:1～1.6:1，更优选1:1～1.4:1。
进一步地，酰基化合物和反应底物的摩尔比为0.5:1～1.2:1，优选0.6:1～1.1:1，更优选0.7:1～1:1。
进一步地，缩合原料和反应底物的摩尔比为0.5:1～1.2:1，优选0.6:1～1.1:1，更优选0.7:1～1:1。
进一步地，所述的氧化剂选自双氧水、氧气。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化新癸酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为新癸酰氯，氧化剂为双氧水，其中，优选的：
所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化新癸酸叔丁酯的收率≥68％；优选的，过氧化新癸酸叔丁酯的收率≥81％。
所述过氧化新癸酸叔丁酯的含量≥87％；优选的，过氧化新癸酸叔丁酯的含量≥91％。
所述目标产品过氧化新癸酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述叔丁醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述新癸酰氯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述新癸酰氯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述双氧水质量浓度为30％～50％；
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化新癸酸-1,1,3,3-四甲基丁酯时，所述反应底物为2,4,4-三甲基-2-戊醇，所述酰基化合物为新癸酰氯，所述氧化剂为双氧水，其中，优选的：
所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化新癸酸-1,1,3,3-四甲基丁酯的收率≥65％；优选的，过氧化新癸酸-1,1,3,3-四甲基丁酯的收率≥70％。
所述过氧化新癸酸-1,1,3,3-四甲基丁酯的含量≥80％；优选的，过氧化新癸酸-1,1,3,3-四甲基丁酯的含量≥90％。
所述目标产品过氧化新癸酸-1,1,3,3-四甲基丁酯中的氯离子含量为0.03～0.05wt％，所述其他有机过氧化物杂质的含量为0.05～0.1wt％，所述其他有机过氧化物杂质是H 2O 2。
所述双氧水质量浓度为30％～50％；
所述2,4,4-三甲基-2-戊醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～11L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述新癸酰氯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和2,4,4-三甲基-2-戊醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和2,4,4-三甲基-2-戊醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和2,4,4-三甲基-2-戊醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述新癸酰氯和2,4,4-三甲基-2-戊醇的摩尔比为0.7:1-1.1:1，优选0.8:1～1:1，更优选0.8:1～0.95:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔丁酯，所述反应底物为叔丁醇，所述酰基化合物为氯甲酸-2-乙基己酯，所述氧化剂为双氧水，其中，优选的：
所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
所述温区4的温度为10～90℃，更优选20～80℃，更优选30～70℃，更优选40～60℃。
所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述双氧水质量浓度为30％～50％；
所述过氧化2-乙基己基碳酸叔丁酯的收率≥70％；优选的，过氧化2-乙基己基碳酸叔丁酯的收率≥81％。
所述过氧化2-乙基己基碳酸叔丁酯的含量≥95％；优选的，过氧化2-乙基己基碳酸叔丁酯的含量≥97％。
所述目标产品过氧化2-乙基己基碳酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
所述叔丁醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述氯甲酸-2-乙基己酯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述氯甲酸-2-乙基己酯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化新癸酸异丙苯酯，所述反应底物为异丙苯，所述酰基化合物为新癸酰氯，所述氧化剂为氧气，其中，优选的：
所述温区1的温度优选0～80℃，更优选10～70℃，更优选20～60℃，更优选30～40℃。
所述温区2的温度优选20～180℃，更优选30～150℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
所述温区3的温度优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区4的温度优选10～100℃，更优选20～80℃，更优选30～60℃，更优选40～50℃。
所述温区5的温度优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区6的温度优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化新癸酸异丙苯酯的收率≥79％；优选的，过氧化新癸酸异丙苯酯的收率≥81％。
所述过氧化新癸酸异丙苯酯的含量≥89％；优选的，过氧化新癸酸异丙苯酯的含量≥94％。
所述目标产品过氧化新癸酸异丙苯酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.1wt％，所述其他过氧化物杂质为二异丙苯过氧化氢。
所述异丙苯流速为0.2～8L/h，优选0.5～6L/h，更优选1.5～4L/h，更优选2～3L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述新癸酰氯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述氧气和异丙苯的摩尔比为0.8:1～2.2:1，优选1.3:1～2.1:1，更优选1.5:1～2:1。
所述碱和异丙苯的摩尔比为1:1～1.8:1，优选1.2:1～1.6:1，更优选1.3:1～1.5:1。
所述新癸酰氯和异丙苯的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化异丙基碳酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为氯甲酸异丙酯，氧化剂为双氧水，其中，优选的：
所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化异丙基碳酸叔丁酯的收率≥70.5％；优选的，过氧化异丙基碳酸叔丁酯的收率≥80％。
所述过过氧化异丙基碳酸叔丁酯的含量≥95％；优选的，过氧化异丙基碳酸叔丁酯的含量≥97％。
所述目标产品过氧化异丙基碳酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
所述叔丁醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述氯甲酸异丙酯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述氯甲酸异丙酯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述双氧水质量浓度为30％～50％；
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
进一步地，所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔戊酯，所述反应底物为叔戊醇，酰基化合物为氯甲酸-2-乙基己酯，氧化剂为双氧水，其中，优选的：
所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
所述过氧化2-乙基己基碳酸叔戊酯的收率≥70％；优选的，过氧化2-乙基己基碳酸叔戊酯的收率≥81％。
所述过氧化2-乙基己基碳酸叔戊酯的含量≥95％；优选的，过氧化2-乙基己基碳酸叔戊酯的含量≥97％。
所述目标产品过氧化2-乙基己基碳酸叔戊酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔戊基。
所述叔戊醇流速为1～8L/h，优选1.5～6L/h，更优选2～4L/h。
所述酸液流速为0.4～5L/h，优选0.5～4L/h，更优选1～3L/h，更优选1.5～2.5L/h。
所述碱液流速为0.4～9L/h，优选0.8～7L/h，更优选1～6L/h,更优选1.2～5L/h,更优选1.5～3L/h。
所述氯甲酸-2-乙基己酯流速为0.4～7L/h，优选0.8～6L/h，更优选1～5L/h,更优选1.5～4L/h,更优选2～3L/h。
所述酸和叔戊醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
所述双氧水和叔戊醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
所述碱和叔戊醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
所述氯甲酸-2-乙基己酯和叔戊醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
所述双氧水质量浓度为30％～50％；
所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、碱土金属氢氧化物或水溶性金属碳酸盐，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
需要说明的是，实际生产中(包括实验室、中试、实际生产过程中)所用的反应底物、氧化剂和缩合剂均有±2个百分点的质量浓度的偏差；温区温度会有±3℃的偏差；生产时间会有±5s的偏差。
本发明提供了一个由反应底物直接全连续生产有机过氧化物的方案，即，多种反应物不断地输入反应器里，并连续地收集反应产物。借助于功能单元温区划分和温度设置的优化以及功能单元的协同作用，短时间内就能够充分反应，反应总时间缩短至15分钟内，大大提升了工艺的效率。
在连续流工艺稳定性和可靠性好，因而产品质量稳定、重现性好；工艺没有放大效应，也解决了有机过氧化物连续流工艺工业化存在放大效应的问题；同时该一体化连续流反应器由于无需延迟管线，体积小，占地面积小，极大地节约了厂房用地。
本发明的第二个目的是提供一种专用于如前所述任何一种形式的在线全连续流生产工艺的即插即产型一体化连续流反应器，所述的一体化连续流反应器采用单元化结构，包括氧化缩合单元和后处理单元，其中：所述的氧化缩合单元用于实现反应底物、氧化剂和缩合剂反应生成过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮，所述后处理单元用于所述有机过氧化物的纯化和清洗，所述的有机过氧化物选自过氧化羧酸 酯、过氧化碳酸酯、过氧化缩酮。
本发明的第三个目的是提供一种专用于如前所述任何一种形式的在线全连续流生产工艺的即插即产型一体化连续流反应器，所述的一体化连续流反应器采用单元化结构，每个所述的单元独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各单元之间相互串联。
本发明的第四个目的是提供一种专用于如前所述任何一种形式的在线全连续流生产工艺的即插即产型一体化连续流反应器，所述的一体化连续流反应器采用单元化结构，每个所述的单元包含至少一个温区，每个温区独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各温区之间相互串联。
以上三种连续流反应器进一步可以是：
进一步地，所述的单元之间还进一步包含缓冲器(Buffervessel)，所述的缓冲器为具有一定容积的容器，主要用于缓冲系统的压力波动和平衡流量差异，使系统工作更平稳。
进一步地，所述一体化连续流反应器进料口的数量为1个或多个，所述一体化连续流反应器出料口的数量为1个或多个。
进一步地，所述的反应器模块任选是任意一种能实现连续流工艺的反应器，所述的反应器选自微反应器(Microreactor)，串联盘管反应器(Tandem loop reactor)，管式反应器(Tubularreactor)的任意一种或任意多种。所述的微反应器，又称微结构反应器或微通道反应器，是一种在其中化学反应发生在普遍侧向尺寸在1mm及以下的有限区域内的设备，这类有限区域最典型的形式即是微型尺寸通道。串联盘管反应器，即用管道将盘管反应器串联起来组成的反应器，其中盘管反应器是将管式反应器做成盘管的形式。管式反应器是上个世纪中叶出现的一种呈管状、长径比很大的连续操作反应器。这种反应器可以很长；可以单管也可以多管并联；可以空管，也可以是填充管。
进一步地，反应器可以是一台或多台。
进一步地，所述反应器通道的材质为单晶硅、特种玻璃、陶瓷、涂有耐腐涂层的不锈钢或金属合金、聚四氟乙烯。
进一步地，所述的反应器模块之间、反应器模块组之间、反应器模块和反应器模块组之间均分别是串联或并联。
进一步地，所述的一体化连续流反应器包含6个温区。
进一步地，所述的一体化连续流反应器的氧化缩合反应单元包含4个温区，分别为温区1，温区2，温区3和温区4，后处理单元包含2个温区，分别为温区5和温区6。
进一步地，所述温区1的温度为0～100℃，优选0～80℃，更优选0～60℃，更优选0～40℃，更优选5～30℃，更优选5～20℃。
进一步地，所述温区2的温度为10～200℃，优选20～180℃，更优选30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
进一步地，所述温区3的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
进一步地，所述温区4的温度为5～100℃，优选20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
进一步地，所述温区5的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
进一步地，所述温区6的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
本发明的第五个目的是提供一种化工生产工艺，所述的化工生产工艺包含本发明所述的由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺，以及一个或多个后续的生产工艺。例如，所述的化工生产工艺可以是聚合工艺，本发明所述的在线全连续流生产工艺生产的有机过氧化物作为聚合工艺的引发剂，将本发明的工艺与聚合反应工艺无缝对接，可以形成有机过氧化物的生产和使用的全连续，颠覆现有生产-存储-运输-储存-使用生产模式，实现生产即使用的新型生产模式。
本发明的第六个目的是提供一种化工生产设备，所述的化工生产设备包含本发明所述任何一种形式的在线全连续流生产工艺的即插即产型一体化连续流反应器，以及一个或多个后续的生产设备。例如，所述的化工生产设备可以是聚合物生产设备，本发明所述的即插即产型一体化连续流反应器可直接与聚合釜无缝对接，可以形成有机过氧化物的生产和使用的全连续生产设备，颠覆现有生产-存储-运输-储存-使用生产模式，实现生产即使用的新型生产模式。
本发明与现有技术的比较，有益效果如下：
1.本发明通过集成反应工艺和即插即产型一体化连续流反应器的优势，彻底改进了现有技术生产有机过氧化物的工艺，首次实现了从安全的起始物(醇或烷烃)直接生产危险程度高的有机过氧化物，宏观上没有危险的烷基过氧化物(中间产品)的累积、纯化和停留等待的过程，避免了烷基过氧化物的纯化、储存和运输步骤，实现了有机过氧化物的即产即用，同时实现了在线生产(on-line manufacturing)，产品的生产和使用同时进行，与下游工艺和设备无缝衔接、同步联动的生产方式，从而实现产品的即产即用(produce-to-use)、随用随产(ready-to-use)的弹性生产模式(flexible manufacturing)。也就是随时需要随时产出，无须等待，按需生产零库存，按需生产，满足需求后即可停车。不仅保证了有机过氧化物的优质高效生产，还能与与下游工艺无缝衔接、同步联动，进而可以避免目标产品有机过氧化物的储存和运输步骤，从根本上解决了烷基过氧化物和最终产品(过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮)冷链仓储和运输的成本及安全性问题。
2.本发明的生产工艺完全不同于现有技术的工艺，仅通过一步反应，并且将反应过程与后处理工艺整合成为一套完整的生产工艺，在短时间内(15分钟内)直接制得符合市售市售工业品标准的产品，实现了高质量、高效率的生产。
3.本发明的生产工艺通用性强，通过将反应工艺与反应器进行有机的整合，打破了不同有机过氧化物的生产工艺无法通用的现有缺陷，通过调整不同的工艺参数和反应器参数，可以在同一台即插即产型一体化连续流反应器上实现不同种有机过氧化物的生产，满足了用户的多种需求，提高了生产效率。
4.本发明的生产工艺安全、高效，制得的有机过氧化物产品产率和含量高，大幅度降低生产成本、提高有机过氧化物生产和下游产品生产的安全性，实现了有机过氧化物的高效率、高质量、大规模生产。
5.本发明解决了有机过氧化物连续流工艺工业化放大的问题，本发明的生产工艺不存在放大效应，极大地降低了工业化应用的难度，在向工业化放大时，无需经历繁琐复杂的多次逐级放大和工艺条件、参数的调整优化，即可一次放大到所需要的生产规模，极大地节约了人力物力和项目开发时间。
6.本发明的生产工艺安全性得到了极大提升，连续流反应器相对较小的持液量和优良的传热特性，加之较短的反应时间(15分钟以内)使得该工艺过程更为安全。其中所述的反应器持液量是指当操作达到定态时，任一时刻反应器中存有的反应物料的总体积。
7.相比于现有技术，本发明的反应时间大大缩短，反应时间缩短了95％，大幅度提高了反应效率。
8.在一体化连续流反应器中，由于流速稳定、生产过程稳定，因而产品质量稳定、重现性好。
9.该一体化连续流反应器体积小，占地面积小，极大地节约了厂房用地。
附图说明
图1本发明连续生产工艺工艺图；
图2是本发明所述的一体化反应器的示意图。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应该理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明的讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例中使用下列缩写：
TBA：叔丁醇
TAA：叔戊醇
NDCl：新癸酰氯
2-EHCF：2-乙基己基氯甲酸酯
CYC:环己酮
CBO：苯甲酰氯
Cumene：异丙苯
NSC904：2,4,4-三甲基-2-戊醇
PVCL:特戊酰氯
2-CHC:2-乙基己酰氯
IBCL:异丁酰氯
U535：新庚酰氯
INCL:3,5,5-三甲基己酰氯
335TCYC:3,3,5-三甲基环己酮
MEK:甲乙酮
IPCF：氯甲酸异丙酯
ACL：乙酰氯
本发明实施例中的浓度均为质量浓度，目标产品的含量利用有效含氧量滴定(碘量法)测得，氯离子含量通过离子检测仪检测，其他有机过氧化物通过高效液相色谱(HPLC)检测，本发明目标产品中的氯离子含量为0.03～0.05％，其他有机过氧化物含量为0.05～0.1％，所述其他有机过氧化物杂质选自H 2O 2、烷烃过氧化物、二烷烃过氧化物的任意一种或任意多种。反应器中无需延迟管线。
需要说明的是，实际生产中(包括实验室、中试、实际生产过程中)所用的反应底物、氧化剂和缩合剂均有±2个百分点的质量浓度的偏差；温区温度会有±3℃的偏差；生产时间会有±5s的偏差。
实施例1-12过氧化新癸酸叔丁酯的制备
如图1和图2所示，将原料1(硫酸溶液)、原料2(反应底物)、原料3(双氧水水溶液)、原料4(碱溶液)和原料5(酰基化合物)以恒流泵先后输送连续反应器，依次进入温区1至温区4中，反应完全；流出温区4反应液进入温区5和温区6进行后处理，得到纯的产品。其中，进料速率1代表原料1的进料速率，进料速率2代表原料2的进料速率，进料速率3代表原料3的进料速率，进料速率4代表原料4的进料速率，进料速率5代表原料5的进料速率。
Figure PCTCN2018100115-appb-000005
Figure PCTCN2018100115-appb-000006
实施例13～14过氧化苯甲酸叔戊酯的制备采用实施例1～12的操作方法。
Figure PCTCN2018100115-appb-000007
Figure PCTCN2018100115-appb-000008
实施例15～26过氧化-2-乙基己基碳酸叔丁酯的制备采用实施例1～12的操作方法。
Figure PCTCN2018100115-appb-000009
Figure PCTCN2018100115-appb-000010
实施例27～281,1-二(叔丁基过氧化)环己烷的制备
如图1和图2所示，将原料1(硫溶液)、原料2(反应底物)、原料3(双氧水水溶液)、原料4(酸溶液)和原料5(缩合原料)以恒流泵先后输送连续反应器，依次进入温区1至温区4中，反应完全；流出温区4反应液进入温区5和温区6进行后处理，得到纯的产品。其中，进料速率1代表原料1的进料速率，进料速率2代表原料2的进料速率，进料速率3代表原料3的进料速率，进料速率4代表原料4的进料速率，进料速率5代表原料5的进料速率。
Figure PCTCN2018100115-appb-000011
Figure PCTCN2018100115-appb-000012
实施例29～38过氧化新癸酸异丙苯酯的制备
如图1和图2所示，将原料1(碱溶液)、原料2(反应底物)、原料3(氧气)、原料4(碱溶液)和原料5(酰基化合物)以恒流泵先后输送连续反应器，依次进入温区1至温区4中，反应完全；流出温区4反应液进入温区5和温区6进行后处理，得到纯的产品。其中，进料速率1代表原料1的进料速率，进料速率2代表原料2的进料速率，进料速率3代表原料3的进料速率，进料速率4代表原料4的进料速率，进料速率5代表原料5的进料速率。
Figure PCTCN2018100115-appb-000013
Figure PCTCN2018100115-appb-000014
Figure PCTCN2018100115-appb-000015
实施例39～50过氧化新癸酸-1,1,3,3-四甲基丁酯的制备采用实施例1～12的操作方法。
Figure PCTCN2018100115-appb-000016
Figure PCTCN2018100115-appb-000017
实施例51～62过氧化异丙基碳酸叔丁酯的制备采用实施例1～12的操作方法。
Figure PCTCN2018100115-appb-000018
Figure PCTCN2018100115-appb-000019
实施例63～74过氧化2-乙基己基碳酸叔戊酯的制备采用实施例1～12的操作方法。
Figure PCTCN2018100115-appb-000020
Figure PCTCN2018100115-appb-000021
Figure PCTCN2018100115-appb-000022
实施例75-77：叔丁基过氧化异丙苯的制备采用实施例29～38的操作方法。
Figure PCTCN2018100115-appb-000023
实施例78-92
具体实施例对应有机过氧化物如下：其中实施例84和85采用实施例27～28的操作方法，实施例78-83和实施例86-92均采用实施例1～12的操作方法。
Figure PCTCN2018100115-appb-000024
Figure PCTCN2018100115-appb-000025
Figure PCTCN2018100115-appb-000026
从上述实施例中可以看到，本发明所述连续流生产有机过氧化物在时间有着巨大的的优势，从现有工艺的数个小时甚至10几个小时缩短到了10分钟以内，且在总体收率和含量较现有技术有一定的提升。同时，从实施例11和12，25和26，37和38，49和50，61和62，73和74，76和77，91和92可见，放大规模后收率并没有变化，生产时间也没又增加，说明本发明不存在放大效应。

Claims (170)

  1. 一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺，其特征在于：所述的生产工艺在即插即产型一体化连续流反应器中进行，在所述一体化连续流反应器的进料口不间断加入反应底物、氧化剂和缩合剂，连续依次经氧化缩合和后处理两个过程，在所述一体化连续流反应器出料口不间断得到目标产品有机过氧化物，所述的生产工艺无放大效应，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮，所述的反应底物为醇或烷烃，所述缩合剂在生产过氧化羧酸酯、过氧化碳酸酯时为碱液和酰基化合物，在生产过氧化缩酮时为酸液和缩合原料，所述缩合原料为醇或酮，所述生产工艺的通式如下：
    Figure PCTCN2018100115-appb-100001
    其中，A 1为醇或烷烃，A 2选自酰氯、氯甲酸酯、醇、酮，氧化剂选自双氧水和氧气，C选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
  2. 根据权利要求1所述的在线全连续流生产工艺，其特征在于：
    A 1为醇的通式为R(OH) n，其中n＝1,2,3...；A 1为烷烃的通式为R(H) n，其中n＝1,2,3...；
    A 2为酰氯的通式为R 1COCl；A 2为氯甲酸酯的通式为R 2OCOCl；A 2为醇的通式为R 3(OH) m，其中m＝1,2,3...；A 2为酮的通式为R 4R 4’(CO)或R 4(CO)(环内酮)；n,m为正整数。
    C为过氧化羧酸酯的通式为R(OOOCR 1) n，其中n＝1,2,3...；C为过氧化碳酸酯的通式为R(OOOCOR 2) n，其中n＝1,2,3...；C为过氧化缩酮的通式为R 4(OOR) 2，其中n＝1；C为过氧化缩酮的通式为R 3(OOR) m，其中n＝1，m＝1,2,3...；C为过氧化缩酮的通式为R(OOR 3) n，其中m＝1，n＝1,2,3...；n，m为正整数。
    R选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基、无取代或取代的环烷基；
    R 1选自饱和或不饱和的C 1-C 20烷基、无取代或取代的芳基、无取代或取代的杂环芳基；
    R 2选自饱和或不饱和的C 1-C 20烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基；
    R 3选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基；
    R 4或R 4’选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环烷基、无取代或取代部分饱和的杂环烷基，无取代或取代的环烷基；
    优选的，
    R选自饱和或不饱和的C3-C8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环、无取代或取代的环烷基；
    R 1选自饱和或不饱和的C 1-C 18烷基、无取代或取代的芳基、无取代或取代的杂环芳基；
    R 2选自饱和或不饱和的C1-C18烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环，无取代或取代的环烷基；
    R 3选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环，无取代或取代的环烷基；
    R 4或R 4’选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环，无取代或取代的环
    烷基；
    更优选的，
    R选自叔丁基、叔戊基、异丙苯基、1，4-二异丙苯基、2,4,4-三甲基-2-戊基、2,5-二甲基己基、1，3-二异丙苯基；
    R 1选自甲基、乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异戊基、正戊基、异庚基、辛基、异辛基、2,2-二甲基庚基、壬基、十一烷基、苯基、2-甲基苯基、4-甲基苯基、4-氯苯基、2,4-二氯苯基、萘基；
    R 2选自甲基、乙基、丙基、异丙基、丁基、仲丁基、2-乙基己基、异十三烷基、十七烷基、环己基、4-叔丁基环己基、苄基、苯氧乙基；
    R 3选自叔丁基、叔戊基、2,5-二甲基己基、1,4-二异丙苯基、1,3-二异丙苯基；
    R 4或R 4’选自甲基、乙基；R 4选自-(CH 2) 5-、-CH 2-C(CH 3) 2-CH 2-CH(CH 3)-CH 2-；
    更优选的，
    R(OH) n选自叔丁醇、叔戊醇、2,4,4-三甲基-2-戊醇、2,5-二甲基-2,5双羟基己烷、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯；
    R(H) n选自异丙苯、1,4-二异丙苯、1,3-二异丙苯；
    R 1COCl选自乙酰氯、丙酰氯、丁酰氯、异丁酰氯、戊酰氯、2-甲基丁酰氯、新戊酰氯、2-甲基戊酰氯、2-乙基丁酰氯、2-乙基己酰氯、壬酰氯，2,4,4-三甲基戊酰氯、3,5,5-三甲基己酰氯、新癸酰氯、癸酰氯、月桂酰氯、苯甲酰氯、2-甲基苯甲酰氯、4-甲基苯甲酰氯、4-氯苯甲酰氯、2，4-二氯苯甲酰氯、萘甲酰氯；
    R 2OCOCl选自氯甲酸甲酯、氯甲酸乙酯、氯甲酸正丙酯、氯甲酸异丙酯、氯甲酸正丁酯、氯甲酸仲丁酯、氯甲酸2-乙基己酯、氯甲酸异十三烷基酯、氯甲酸硬脂酯、氯甲酸环己酯、氯甲酸4-叔丁基环己酯、氯甲酸苄酯、氯甲酸2-苯氧基乙酯；
    R 3(OH) n选自叔丁醇、叔戊醇、2,4,4―三甲基―2-戊醇、2,5-二甲基-2,5双羟基己烷、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯；
    R 4R 4’(CO)选自甲乙酮；R 4(CO)选自环己酮、3,3,5-三甲基环己酮。
  3. 根据权利要求1所述的在线全连续流生产工艺，其特征在于：所述有机过氧化物C选自：
    过氧化苯甲酸叔丁酯CAS No.：614-45-9、过氧化苯甲酸叔戊酯CAS No.：4511-39-1、过氧化乙酸叔丁酯CAS No.：107-71-1、过氧化特戊酸叔丁酯CAS No.：927-07-1、过氧化特戊酸叔戊酯CAS No.：29240-17-3、过氧化新癸酸叔丁酯CAS No.：26748-41-4、过氧化新癸酸叔戊酯CAS No.：68299-16-1、过氧化2-乙基己酸叔丁酯CAS No.：3006-82-4、过氧化2-乙基己酸叔戊酯CAS No.：686-31-7、过氧化异丁酸叔丁酯CAS No.:109-13-7、过氧化新庚酸叔丁酯CAS No.：26748-38-9、过氧化3,5,5-三甲基己酸叔丁酯CAS No.：13122-18-4、过氧化2-乙基己基碳酸叔丁酯CAS No.：34443-12-4、过氧化2-乙基己基碳酸叔戊酯CAS No.：70833-40-8、1,1-二叔丁基过氧化-3,3,5-三甲基环己烷CAS No.：6731-36-8、1,1-二(叔丁基过氧化)环己烷CAS No.：3006-86-8、2,2-二(叔丁基过氧化)丁烷CAS No.：2167-23-9、过氧化新癸酸异丙苯酯CAS No.：26748-47-0、过氧化新癸酸-1,1,3,3-四甲基丁酯CAS No.：51240-95-0、过氧化特戊酸1,1,3,3-四甲基丁酯CAS No.：22288-41-1、1,1,3,3-四甲基丁基过氧化-2-乙基己酸酯CAS No.：22288-43-3、1,1-二特戊基过氧化环己烷CAS No.：15667-10-4、过氧化乙酸特戊酯CAS No.：690-83-5、过氧化异丙基碳酸叔丁酯CAS No.：2372-21-6、叔丁基过氧化异丙苯CAS No.：3457-61-2。
  4. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述的生产工艺宏观上没有烷基过氧化物的累积、纯化和停留等待的过程。
  5. 根据权利要求4所述的在线全连续流生产工艺，其特征在于：所述烷基过氧化物通式为R(OOH) n，其中，R选自饱和或不饱和的C 1-C 12烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环、无取代或取代的环烷基，n≥1，n为正整数；
    优选的，R选自饱和或不饱和的C 3-C 8烷基、无取代或取代的芳基、无取代或取代的杂环芳基、无取代或取代的饱和的杂环、无取代或取代部分饱和的杂环、无取代或取代的环烷基；
    更优选的，R选自叔丁基、叔戊基、异丙苯基、1,4-二异丙苯基、2,4,4-三甲基-2-戊基、2,5-二甲基己基；
    所述烷基过氧化物选自：
    叔丁基过氧化氢CAS No.：75-91-2、叔戊基过氧化氢CAS No.：3425-61-4、CAS No.：
    4212-43-5、1，1，3，3-四甲基丁基过氧化氢CAS No.：5809-08-5、异丙苯过氧化氢CAS No.：80-15-9、2,5-二甲基-2,5双(过氧化氢)己烷CAS No.：3025-88-5、二羟基-1,4-二异丙基苯CAS No.：3159-98-6。
  6. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述目标产品有机过氧化物中的氯离子含量≤0.05wt％，其他有机过氧化物杂质的含量≤0.1wt％，所述其他有机过氧化物杂质选自H 2O 2、烷烃过氧化物、二烷烃过氧化物的任意一种或任意多种。
  7. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤15min，优选的，所述生产工艺的生产时间≤10min；更优选的，所述的生产时间为3～13min；更优选的，所述的生产时间为4～11min；更优选的，所述的生产时间为5～10min。
  8. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述有机过氧化物的收率≥64％；优选的，所述有机过氧化物的收率≥75％；更优选的，所述有机过氧化物的收率≥81％
  9. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述有机过氧化物的含量≥77％；优选的，所述有机过氧化物的含量≥85％；所述有机过氧化物的含量≥97％。
  10. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～200℃，优选0～180℃，更优选0～160℃，更优选0～142℃，更优选5～130℃。
  11. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～60℃，优选0～50℃，更优选0～40℃，更优选0～30℃，更优选5～30℃。
  12. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述碱选自水溶性金属氢氧化物、水溶性季铵氢氧化物、水溶性叔胺、水溶性金属碳酸盐或水溶性金属磷酸盐，优选碱金属氢氧化物、水溶性金属碳酸盐或碱土金属氢氧化物，更优选氢氧化钠、氢氧化钾、碳酸钠、碳酸钾或氢氧化锂。
  13. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述碱液质量浓度为5％～45％，优选15％～35％，更优选20％～30％。
  14. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述酸选自所有已知的有机酸和无机酸，优选硫酸、磷酸或三氟乙酸。
  15. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述酸液质量浓度为50％～90％，优选60％～80％，更优选70％～80％。
  16. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述氧化剂选自双氧水、氧气。
  17. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述反应底物选自叔丁醇、叔戊醇、异丙苯、1，4-二异丙苯、对孟烷、蒎烷、四氢萘、2,4,4-三甲基-2-戊醇、1，3-二异丙苯、二羟基-1,4-二异丙基苯、二羟基-1,3-二异丙基苯。
  18. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：所述缩合剂中的酰基化合物选自乙酰氯、丙酰氯、丁酰氯、异丁酰氯、戊酰氯、2-甲基丁酰氯、新戊酰氯、2-甲基戊酰氯、2-乙基丁酰氯、2-乙基己酰氯、壬酰氯，2,4,4-三甲基戊酰氯、3,5,5-三甲基己酰氯、新癸酰氯、癸酰氯、月桂酰氯、苯甲酰氯、2-甲基苯甲酰氯、4-甲基苯甲酰氯、4-氯苯甲酰氯、2，4-二氯苯甲酰氯、萘甲酰氯、氯甲酸甲酯、氯甲酸乙酯、氯甲酸正丙酯、氯甲酸异丙酯、氯甲酸正丁酯、氯甲酸仲丁酯、氯甲酸2-乙基己酯、氯甲酸异十三烷基酯、氯甲酸硬脂酯、氯甲酸环己酯、氯甲酸4-叔丁基环己酯、氯甲酸苄酯、氯甲酸2-苯氧基乙酯；所述缩合剂中的醇选自叔丁醇、叔戊醇；所述缩合剂中的酮选自环己酮，3,3,5-三甲基环己酮、甲乙酮。
  19. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：酸和反应底物的摩尔比为0.3:1～1.5:1，优选0.4:1～1.2:1，更优选0.5:1～1:1。
  20. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：氧化剂和反应底物的摩尔比为0.8:1～2.2:1，优选0.9:1～2.1:1，更优选1:1～2:1，更优选1.3:1～1.8:1。
  21. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：碱和反应底物的摩尔比为0.7:1～2:1，优选0.9:1～1.8:1，更优选1:1～1.6:1，更优选1:1～1.4:1。
  22. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：酰基化合物和反应底物的摩尔比为0.5:1～1.2:1，优选0.6:1～1.1:1，更优选0.7:1～1:1。
  23. 根据权利要求1-3任一项所述的在线全连续流生产工艺，其特征在于：缩合原料和反应底物的摩尔比为0.5:1～1.2:1，优选0.6:1～1.1:1，更优选0.7:1～1:1。
  24. 根据权利要求1-23任一项所述的在线全连续流生产工艺，其特征在于：所述有机过氧化物为过氧化新癸酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为新癸酰氯，氧化剂为双氧水。
  25. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
  26. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述过氧化新癸酸叔丁酯的收率≥68％；优选的，所述过氧化新癸酸叔丁酯的收率≥81％。
  27. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述过氧化新癸酸叔丁酯的含量≥87％；优选的，所述过氧化新癸酸叔丁酯的含量≥91％。
  28. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述目标产品过氧化新癸酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
  29. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
  30. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  31. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
  32. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
  33. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
  34. 根据权利要求24所述的在线全连续流生产工艺，其特征在于：所述新癸酰氯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
  35. 根据权利要求1-23任一项所述的在线全连续流生产工艺，其特征在于：所述有机过氧化物为过氧化新癸酸-1,1,3,3-四甲基丁酯，所述反应底物为2,4,4-三甲基-2-戊醇，所述酰基化合物为新癸酰氯，所述氧化剂为双氧水。
  36. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
  37. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述过氧化新癸酸-1,1,3,3-四甲基丁酯的收率≥65％；优选的，过氧化新癸酸-1,1,3,3-四甲基丁酯的收率≥70％。
  38. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述过氧化新癸酸-1,1,3,3-四甲基丁酯的含量≥80％；优选的，过氧化新癸酸-1,1,3,3-四甲基丁酯的含量≥90％。
  39. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述目标产品过氧化新癸酸-1,1,3,3-四甲基丁酯中的氯离子含量为0.03～0.05wt％，H 2O 2的含量为0.05～0.1wt％。
  40. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
  41. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  42. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述酸和2,4,4-三甲基-2-戊醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
  43. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述双氧水和2,4,4-三甲基-2-戊醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
  44. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述碱和2,4,4-三甲基-2-戊醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
  45. 根据权利要求35所述的在线全连续流生产工艺，其特征在于：所述新癸酰氯和2,4,4-三甲基-2-戊醇的摩尔比为0.7:1-1.1:1，优选0.8:1～1:1，更优选0.8:1～0.95:1。
  46. 根据权利要求1-23任一项所述的在线全连续流生产工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔丁酯，所述反应底物为叔丁醇，所述酰基化合物为氯甲酸-2-乙基己酯，所述氧化剂为双氧水。
  47. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
  48. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述过氧化2-乙基己基碳酸叔丁酯的收率≥70％；优选的，过氧化2-乙基己基碳酸叔丁酯的收率≥81％。
  49. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述过氧化2-乙基己基碳酸叔丁酯的含量≥95％；优选的，过氧化2-乙基己基碳酸叔丁酯的含量≥97％。
  50. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述目标产品过氧化2-乙基己基碳酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
  51. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
  52. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  53. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
  54. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
  55. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
  56. 根据权利要求46所述的在线全连续流生产工艺，其特征在于：所述氯甲酸-2-乙基己酯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
  57. 根据权利要求1-23任一项所述的在线全连续流生产工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化异丙基碳酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为氯甲酸异丙酯，氧化剂为双氧水。
  58. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
  59. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述过氧化异丙基碳酸叔丁酯的收率≥70.5％；优选的，过氧化异丙基碳酸叔丁酯的收率≥80％。
  60. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述过过氧化异丙基碳酸叔丁酯的含量≥95％；优选的，过氧化异丙基碳酸叔丁酯的含量≥97％。
  61. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述目标产品过氧化异丙基碳酸叔丁酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔丁基。
  62. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
  63. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  64. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述酸和叔丁醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
  65. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述双氧水和叔丁醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
  66. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述碱和叔丁醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
  67. 根据权利要求57所述的在线全连续流生产工艺，其特征在于：所述氯甲酸异丙酯和叔丁醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
  68. 根据权利要求1-23任一项所述的在线全连续流生产工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔戊酯，所述反应底物为叔戊醇，酰基化合物为氯甲酸-2-乙基己酯，氧化剂为双氧水。
  69. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
  70. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述目标产品过氧化2-乙基己基碳酸叔戊酯中的氯离子含量为0.03～0.05wt％，其他有机过氧化物杂质的含量为0.05～0.08wt％，所述其他有机过氧化物杂质为H 2O 2和过氧化二叔戊基。
  71. 根据权利要求68所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～160℃，优选20～130℃，更优选40～120℃，更优选60～100℃，更优选70～90℃。
  72. 根据权利要求68所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  73. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述过氧化2-乙基己基碳酸叔戊酯的收率≥70％；优选的，过氧化2-乙基己基碳酸叔戊酯的收率≥81％。
  74. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述过氧化2-乙基己基碳酸叔戊酯的含量≥95％；优选的，过氧化2-乙基己基碳酸叔戊酯的含量≥97％
  75. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述酸和叔戊醇的摩尔比为0.3:1～1.3:1，优选0.4:1～1.2:1，更优选0.5:1～1:1，更优选0.5:1～0.8:1。
  76. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述双氧水和叔戊醇的摩尔比为0.8:1～1.5:1，优选0.9:1～1.4:1，更优选1:1～1.3:1，更优选1.05:1～1.2:1。
  77. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述碱和叔戊醇的摩尔比为0.9:1～1.6:1，优选1:1～1.4:1，更优选1.2:1～1.3:1。
  78. 根据权利要求68任一项所述的在线全连续流生产工艺，其特征在于：所述氯甲酸-2-乙基己酯和叔戊醇的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
  79. 根据权利要求24、35、46、57、68任一项所述的在线全连续流生产工艺，其特征在于：所述双氧水的质量浓度为30％～50％。
  80. 根据权利要求1-23任一项所述的在线全连续流生产工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化新癸酸异丙苯酯，所述反应底物为异丙苯，所述酰基化合物为新癸酰氯，所述氧化剂为氧气。
  81. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述生产工艺的生产时间≤10min，优选的，所述的生产时间为3～9min；更优选的，所述的生产时间为4～8min；更优选的，所述的生产时间为5～7min。
  82. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述过氧化新癸酸异丙苯酯的收率≥79％；优选的，过氧化新癸酸异丙苯酯的收率≥81％。
  83. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述过氧化新癸酸异丙苯酯的含量≥89％；优选的，过氧化新癸酸异丙苯酯的含量≥94％。
  84. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述目标产品过氧化新癸酸异丙苯酯中的氯离子含量为0.03～0.05wt％，二异丙苯过氧化氢的含量为0.05～0.1wt％。
  85. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述氧化缩合工艺的温度为0～180℃，优选0～150℃，优选20～150℃，更优选40～130℃，更优选60～120℃，更优选70～90℃。
  86. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述后处理的温度为0～60℃，优选0～50℃，更优选0～40℃，更优选0～30℃，更优选5～30℃。
  87. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述氧气和异丙苯的摩尔比为0.8:1～2.2:1，优选1.3:1～2.1:1，更优选1.5:1～2:1。
  88. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述碱和异丙苯的摩尔比为1:1～1.8:1，优选1.2:1～1.6:1，更优选1.3:1～1.5:1。
  89. 根据权利要求80所述的在线全连续流生产工艺，其特征在于：所述新癸酰氯和异丙苯的摩尔比为0.5:1～1.1:1，优选0.6:1～1:1，更优选0.7:1～0.9:1。
  90. 根据权利要求1-89任一项所述的在线全连续流生产工艺，其特征在于：所述即插即产型一体化连续流反应器采用单元化结构，包括氧化缩合单元和后处理单元，其中：所述的氧化缩合单元用于实现反应底物、氧化剂和缩合剂反应生成过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮，所述后处理单元用于所述有机过氧化物的后处理，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
  91. 根据权利要求90所述的在线全连续流生产工艺，其特征在于：所述氧化缩合单元的温度为0～200℃，优选0～180℃，更优选0～160℃，更优选0～140℃，更优选5～130℃。
  92. 根据权利要求90所述的在线全连续流生产工艺，其特征在于：所述后处理单元的温度为0～60℃，优选0～50℃，更优选0～40℃，更优选0～30℃，更优选5～30℃。
  93. 根据权利要求1-92任一项所述的在线全连续流合成工艺，其特征在于：所述即插即产型一体化连续流反应器采用单元化结构，每个所述的单元独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各单元之间相互串联。
  94. 根据权利要求1-92任一项所述的在线全连续流合成工艺，其特征在于：所述即插即产型一体化连续流反应器采用单元化结构，每个所述的单元对应至少一个温区，每个温区独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各温区之间相互串联。
  95. 根据权利要求1-94任一项所述的在线全连续流合成工艺，其特征在于：所述的单元之间还进一步包含缓冲器。
  96. 根据权利要求1-95任一项所述的在线全连续流合成工艺，其特征在于：所述一体化连续流反应器进料口的数量为1个或多个，所述一体化连续流反应器出料口的数量为1个或多个。
  97. 根据权利要求1-95任一项所述的在线全连续流合成工艺，其特征在于：所述的反应器模块任选是任意一种能实现连续流工艺的反应器，所述的反应器选自微反应器、串联盘管反应器、管式反应器的任意一种或任意多种。
  98. 根据权利要求1-95任一项所述的在线全连续流合成工艺，其特征在于：所述的反应器可以是一台或多台。
  99. 根据权利要求1-95任一项所述的在线全连续流合成工艺，其特征在于：所述反应器通道的材质为单晶硅、特种玻璃、陶瓷、涂有耐腐涂层的不锈钢或金属合金、聚四氟乙烯。
  100. 根据权利要求1-95任一项所述的在线全连续流合成工艺，其特征在于：所述的反应器模块之间、反应器模块组之间、反应器模块和反应器模块组之间均分别是串联或并联。
  101. 根据权利要求1-95任一项所述的在线全连续流合成工艺，其特征在于：所述的连续流生产工艺在包含6个温区的即插即产型一体化连续流反应器中进行。
  102. 根据权利要求90-101任一项所述的在线全连续流合成工艺，其特征在于：所述的连续流生产工艺的氧化缩合反应单元包含4个温区，分别为温区1，温区2，温区3和温区4，后处理单元包含2个温区，分别为温区5和温区6。
  103. 根据权利要求101或102所述的在线全连续流合成工艺，其特征在于：所述的连续流生产工艺包括如下步骤：
    (a)将反应底物、氧化剂和缩合剂输送进氧化缩合单元，依次经过温区1-温区4，完全反应生成相应的过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮；所述的反应底物为醇或烷烃，所述缩合剂在生产过氧化羧酸酯、过氧化碳酸酯时为碱液和酰基化合物，在生产过氧化缩酮时为酸液和缩合原料，所述缩合原料为醇或酮。
    (b)流出温区4的反应液进入后处理单元，依次经过温区5和温区6进行后处理，得到目标产品有机过氧化物，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
  104. 根据权利要求103所述的在线全连续流合成工艺，其特征在于：所述温区1的温度为0～100℃，优选0～80℃，更优选0～60℃，更优选0～40℃，更优选5～30℃，更优选5～20℃。
  105. 根据权利要求103所述的在线全连续流合成工艺，其特征在于：所述温区2的温度为10～200℃，优选20～180℃，更优选30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  106. 根据权利要求103所述的在线全连续流合成工艺，其特征在于：所述温区3的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  107. 根据权利要求103所述的在线全连续流合成工艺，其特征在于：所述温区4的温度为5～100℃，优选20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
  108. 根据权利要求103所述的在线全连续流合成工艺，其特征在于：所述温区5的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  109. 根据权利要求103所述的在线全连续流合成工艺，其特征在于：所述温区6的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  110. 根据权利要求101-109任一项所述的在线全连续流合成工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化新癸酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为新癸酰氯，氧化剂为双氧水。
  111. 根据权利要求110所述的在线全连续流合成工艺，其特征在于：所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
  112. 根据权利要求110所述的在线全连续流合成工艺，其特征在于：所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  113. 根据权利要求110所述的在线全连续流合成工艺，其特征在于：所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
  114. 根据权利要求110所述的在线全连续流合成工艺，其特征在于：所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
  115. 根据权利要求110所述的在线全连续流合成工艺，其特征在于：所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  116. 根据权利要求110所述的在线全连续流合成工艺，其特征在于：所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  117. 根据权利要求101-109任一项所述的在线全连续流合成工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化新癸酸-1,1,3,3-四甲基丁酯时，所述反应底物为2,4,4-三甲基-2-戊醇，所述酰基化合物为新癸酰氯，所述氧化剂为双氧水。
  118. 根据权利要求117所述的在线全连续流合成工艺，其特征在于：所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
  119. 根据权利要求117所述的在线全连续流合成工艺，其特征在于：进一步地，所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  120. 根据权利要求117所述的在线全连续流合成工艺，其特征在于：所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
  121. 根据权利要求117所述的在线全连续流合成工艺，其特征在于：所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
  122. 根据权利要求117所述的在线全连续流合成工艺，其特征在于：所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  123. 根据权利要求117所述的在线全连续流合成工艺，其特征在于：所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  124. 根据权利要求101-109任一项所述的在线全连续流合成工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔丁酯，所述反应底物为叔丁醇，所述酰基化合物为氯甲酸-2-乙基己酯，所述氧化剂为双氧水。
  125. 根据权利要求128所述的在线全连续流合成工艺，其特征在于：所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
  126. 根据权利要求128所述的在线全连续流合成工艺，其特征在于：所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  127. 根据权利要求128所述的在线全连续流合成工艺，其特征在于：所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
  128. 根据权利要求128所述的在线全连续流合成工艺，其特征在于：所述温区4的温度为10～90℃，更优选20～80℃，更优选30～70℃，更优选40～60℃。
  129. 根据权利要求128所述的在线全连续流合成工艺，其特征在于：所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  130. 根据权利要求128所述的在线全连续流合成工艺，其特征在于：所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  131. 根据权利要求101-109任一项所述的在线全连续流合成工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化新癸酸异丙苯酯，所述反应底物为异丙苯，所述酰基化合物为新癸酰氯，所述氧化剂为氧气。
  132. 根据权利要求131所述的在线全连续流合成工艺，其特征在于：所述温区1的温度优选0～80℃，更优选10～70℃，更优选20～60℃，更优选30～40℃。
  133. 根据权利要求131所述的在线全连续流合成工艺，其特征在于：所述温区2的温度优选20～180℃，更优选30～150℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。。
  134. 根据权利要求131所述的在线全连续流合成工艺，其特征在于：所述温区3的温度优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  135. 根据权利要求131所述的在线全连续流合成工艺，其特征在于：所述温区4的温度优选10～100℃，更优选20～80℃，更优选30～60℃，更优选40～50℃。
  136. 根据权利要求131所述的在线全连续流合成工艺，其特征在于：所述温区5的温度优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  137. 根据权利要求131所述的在线全连续流合成工艺，其特征在于：所述温区6的温度优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  138. 根据权利要求101-109任一项所述的在线全连续流合成工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化异丙基碳酸叔丁酯，所述反应底物为叔丁醇，酰基化合物为氯甲酸异丙酯，氧化剂为双氧水。
  139. 根据权利要求138所述的在线全连续流合成工艺，其特征在于：所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20℃。
  140. 根据权利要求138所述的在线全连续流合成工艺，其特征在于：所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  141. 根据权利要求138所述的在线全连续流合成工艺，其特征在于：所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
  142. 根据权利要求138所述的在线全连续流合成工艺，其特征在于：所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
  143. 根据权利要求138所述的在线全连续流合成工艺，其特征在于：所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  144. 根据权利要求138所述的在线全连续流合成工艺，其特征在于：所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  145. 根据权利要求101-109任一项所述的在线全连续流合成工艺，其特征在于：所述在线全连续流生产工艺的目标产品为过氧化2-乙基己基碳酸叔戊酯，所述反应底物为叔戊醇，酰基化合物为氯甲酸-2-乙基己酯，氧化剂为双氧水。
  146. 根据权利要求145所述的在线全连续流合成工艺，其特征在于：所述温区1的温度优选5～70℃，更优选5～60℃，更优选5～40℃，更优选5～30℃，更优选5～20。
  147. 根据权利要求145所述的在线全连续流合成工艺，其特征在于：所述温区2的温度为30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  148. 根据权利要求145所述的在线全连续流合成工艺，其特征在于：所述温区3的温度为0～40℃，更优选5～30℃，更优选5～20℃。
  149. 根据权利要求145所述的在线全连续流合成工艺，其特征在于：所述温区4的温度为20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
  150. 根据权利要求145所述的在线全连续流合成工艺，其特征在于：所述温区5的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20。
  151. 根据权利要求145所述的在线全连续流合成工艺，其特征在于：所述温区6的温度为0～50℃，优选0～40℃，更优选5～30℃，更优选5～20。
  152. 一种专用于权利要求1-151任一项所述的在线全连续流生产工艺的即插即产型一体化连续流反应器，其特征在于：所述的一体化连续流反应器采用单元化结构，包括氧化缩合单元和后处理单元，其中：所述的氧化缩合单元用于实现反应底物、氧化剂和缩合剂反应生成过氧化羧酸酯、过氧化碳酸酯和过氧化缩酮，所述后处理单元用于所述有机过氧化物的后处理，所述的有机过氧化物选自过氧化羧酸酯、过氧化碳酸酯、过氧化缩酮。
  153. 一种专用于权利要求1-151任一项所述的在线全连续流生产工艺的即插即产型一体化连续流反应器，其特征在于：所述的一体化连续流反应器采用单元化结构，每个所述的单元独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各单元之间相互串联。
  154. 一种专用于权利要求1-151任一项所述的在线全连续流生产工艺的即插即产型一体化连续流反应器，其特征在于：所述的一体化连续流反应器采用单元化结构，每个所述的 单元对应至少一个温区，每个温区独立地包含一个以上的反应器模块或反应器模块组，其中反应器模块组由多个反应器模块串联或并联组成，各温区之间相互串联。
  155. 根据权利要求152-154任一项所述的连续流合成工艺，其特征在于：所述的单元之间还进一步包含缓冲器。
  156. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述一体化连续流反应器进料口的数量为1个或多个，所述一体化连续流反应器出料口的数量为1个或多个。
  157. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述的反应器模块任选是任意一种能实现连续流工艺的反应器，所述的反应器选自微反应器、串联盘管反应器、管式反应器的任意一种或任意多种。
  158. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述的反应器可以是一台或多台。
  159. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述的反应器模块之间、反应器模块组之间、反应器模块和反应器模块组之间均分别是串联或并联。
  160. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述反应器通道的材质为单晶硅、特种玻璃、陶瓷、涂有耐腐涂层的不锈钢或金属合金、聚四氟乙烯。
  161. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述的一体化连续流反应器包含6个温区。
  162. 根据权利要求152-154任一项所述的一体化连续流反应器，其特征在于：所述的一体化连续流反应器的氧化缩合反应单元包含4个温区，分别为温区1，温区2，温区3和温区4，后处理单元包含2个温区，分别为温区5和温区6。
  163. 根据权利要求162所述的一体化连续流反应器，其特征在于：所述温区1的温度为0～100℃，优选0～80℃，更优选0～60℃，更优选0～40℃，更优选5～30℃，更优选5～20℃。
  164. 根据权利要求162所述的一体化连续流反应器，其特征在于：所述温区2的温度为10～200℃，优选20～180℃，更优选30～160℃，更优选40～130℃，更优选50～120℃，更优选60～110℃，更优选70～100℃，更优选80～90℃。
  165. 根据权利要求162所述的一体化连续流反应器，其特征在于：所述温区3的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  166. 根据权利要求162所述的一体化连续流反应器，其特征在于：所述温区4的温度为5～100℃，优选20～90℃，更优选30～80℃，更优选40～70℃，更优选50～60℃。
  167. 根据权利要求162所述的一体化连续流反应器，其特征在于：所述温区5的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  168. 根据权利要求162所述的一体化连续流反应器，其特征在于：所述温区6的温度为0～60℃，优选0～50℃，优选0～40℃，更优选5～30℃，更优选5～20℃。
  169. 一种化工生产工艺，其特征在于：所述的化工生产工艺包含权利要求1-168任一项所述的在线全连续流生产工艺，以及一个或多个后续的生产工艺。
  170. 一种化工生产设备，其特征在于：所述的化工生产设备包含权利要求1-168任一项所述的即插即产型一体化连续流反应器，以及一个或多个后续的生产设备。
PCT/CN2018/100115 2017-08-12 2018-08-10 一种由醇或烷烃直接制备有机过氧化物的在线全连续流生产工艺 Ceased WO2019034006A1 (zh)

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