CN120576600B - Heat exchange device for preparing peroxide and peroxide preparation method - Google Patents
Heat exchange device for preparing peroxide and peroxide preparation methodInfo
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- CN120576600B CN120576600B CN202511062677.2A CN202511062677A CN120576600B CN 120576600 B CN120576600 B CN 120576600B CN 202511062677 A CN202511062677 A CN 202511062677A CN 120576600 B CN120576600 B CN 120576600B
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Abstract
The invention belongs to the technical field of peroxide preparation, and in particular relates to a heat exchange device for preparing peroxide and a peroxide preparation method, wherein the heat exchange device for preparing peroxide comprises a heat exchange tube arranged in a reaction kettle, be provided with a plurality of heat exchangers on the heat exchange tube, the heat exchanger is including a plurality of external fins, and external fin interval sets up on the fixed plate, and fixed plate cooperation heat exchange tube is provided with the recess, and the heat exchange tube sets up inside the recess of fixed plate. The preparation method of the peroxide comprises the steps of stirring and reacting a phlegmatizer, a catalyst and an oxidant, then adding alkyl acyl chloride or alkyl chloroformate for continuous reaction, obtaining a crude product after the reaction is finished, washing the crude product, and separating to obtain the peroxide. The invention can realize the high-efficiency heat transfer performance by utilizing the heat exchanger, thereby being capable of stably preparing the peroxide product, reducing the feeding reaction time and improving the conversion efficiency from the initial raw material to the peroxide product.
Description
Technical Field
The invention belongs to the technical field of peroxide preparation, and particularly relates to a heat exchange device for preparing peroxide and a peroxide preparation method.
Background
The peroxide is an organic peroxide and belongs to the category of low-temperature organic peroxides. The compounds have important applications in industry and scientific research, for example, as initiators for high molecular polymerization, as free radical initiators and oxidants in organic synthesis, and in crosslinking of rubber.
Peroxides have a certain risk. They have low decomposition temperatures and explosiveness and are sensitive to impact, heat and friction. Therefore, special care is required during processing to avoid spontaneous combustion or explosion. In the process of producing peroxide, alkyl acyl chloride or alkyl chloroformate is often used as a raw material, hydrogen peroxide is used as an oxidant for peroxidation, and a large amount of heat can be emitted by the substances in the reaction process, so that the temperature is out of control if the substances are improperly operated. The peroxide product is very unstable in property, and the combustion and explosion accidents can be caused by the excessive temperature. Therefore, the heat exchange requirement in the reaction kettle is very high, and the reaction heat in the reaction kettle needs to be exchanged in a short time, so that the decomposition of the organic peroxide caused by the overhigh temperature in the reaction kettle is prevented.
Aiming at the strong exothermic phenomenon in the peroxide product production process, the heat exchanger in the reaction kettle is required to have higher heat exchange efficiency, and the coil heat exchanger is usually arranged in the conventional reaction kettle, so that the heat exchange efficiency is not high. In the process of producing the organic peroxide product, the performance of the heat exchanger in the reaction kettle plays an important role in the quality of the organic peroxide product, the energy utilization rate of the reaction kettle and the economical efficiency and the reliability of the system operation.
Chinese patent CN106215832a discloses a reinforced heat exchange type reaction kettle and a reinforced heat exchange method for the reaction kettle, wherein a heat exchange transfer tube, an external heat exchange tube and a heat exchange jacket are arranged on the outer surface of the kettle body, the external heat exchange tube, the heat exchange jacket and the heat exchange jacket which are adjacent up and down are communicated through an internal heat exchange tube, the internal heat exchange tube is arranged on the inner surface of the kettle body at intervals along the circumference, the external heat exchange tube, the heat exchange transfer tube and the heat exchange jacket are composed of at least two closed chambers, and heat exchange medium is sequentially and alternately circulated in the heat exchange jacket, the external heat exchange tube, the internal heat exchange tube and the heat exchange transfer tube to form a layer-by-layer progressive heat exchange cycle.
The heat exchanger commonly used in the patent adopts a finless coil pipe as a main body part of the heat exchanger, a stirring paddle in the reaction kettle drives reactants to flow through the outer surface of the coil pipe for heat exchange, the heat exchange area of the coil pipe is small, the heat transfer effect in the actual use process is not ideal, and the heat exchange efficiency is low. The reactant exchanges heat on the surface of the coil heat exchanger, the heat transfer surface of the coil is smooth, and the turbulence effect on the fluid is very small.
In the traditional process, alkyl acyl chloride or alkyl chloroformate and hydrogen peroxide are used as raw materials, strong alkali is used as a catalyst, reactants are slowly dripped at low temperature, and the improper operation easily causes overheating of the reaction, and explosion or fire disaster is caused. Because the reaction kettle has larger volume and limited heat transfer efficiency, the local reaction liquid in the reaction kettle is overhigh in temperature, so that the reaction kettle is locally overheated, and the risk of out of control is increased. In order to control the temperature in the reaction kettle, a heat exchange system needs to be frequently started, the temperature in the reaction kettle is balanced, and the operation is complex.
With increasing importance on environmental protection and safety production, development of a safe and efficient organic peroxide synthesis process is a necessary trend.
Disclosure of Invention
According to the defects in the prior art, the technical problem to be solved by the invention is to provide the heat exchange device for preparing the peroxide, and the heat dissipation fins with high heat transfer are arranged in the reaction kettle to safely synthesize the peroxide, so that the safe and efficient synthesis of a peroxide product is realized, and the invention also provides a peroxide preparation method.
The technical scheme adopted for solving the technical problems is as follows:
the heat exchange device for preparing peroxide comprises a heat exchange tube arranged in a reaction kettle, wherein a plurality of heat exchangers are arranged on the heat exchange tube, each heat exchanger comprises a plurality of external fins, the external fins are arranged on a fixed plate at intervals, the fixed plate is provided with grooves in cooperation with the heat exchange tube, and the heat exchange tube is arranged in the grooves of the fixed plate.
Wherein:
The external fins are vertically arranged on the outer side of the fixed plate, the included angle between the axis of the long side of each external fin and the axis of the heat exchange tube is 0-90 degrees, the grooves are arranged on the inner side of the fixed plate, and each groove comprises an inward concave groove, an outward convex groove and a straight groove.
When the heat exchange tube is a straight tube, the two fixing plates provided with the straight grooves are arranged oppositely, screw holes for accommodating fixing bolts are arranged on the fixing plates, the fixing bolts penetrate through the screw holes to connect the two fixing plates, and buffer gaskets are arranged between the fixing bolts and the fixing plates.
The reactor is internally provided with a stirrer, the top of the stirrer penetrates through the reactor and is connected with a motor, the top of the reactor is provided with a raw material inlet and an additive liquid inlet, and the bottom of the reactor is provided with a discharge hole.
The peroxide preparation method for preparing the peroxide heat exchange device comprises the following steps:
S1, adding a desensitizer, a catalyst and an oxidant into a reaction kettle, stirring for reaction, then adding alkyl acyl chloride or alkyl chloroformate for continuous reaction, and obtaining a crude product after the reaction is finished;
S2, washing and separating the crude product to obtain the peroxide.
The method also comprises a step S3 of mixing peroxide and an auxiliary agent to obtain the auxiliary agent peroxide, wherein the phlegmatizer in the step S1 is 2-methoxy-2-methyl heptane, the catalyst is sodium hydroxide or potassium hydroxide aqueous solution, the catalyst concentration is 20-40wt%, the oxidant is hydrogen peroxide or tert-butyl hydroperoxide, and the oxidant concentration is 27.5-80wt%.
In the step S1, the alkyl acyl chloride is one or more of 3, 5-trimethyl hexanoyl chloride, isobutyryl chloride, pivaloyl chloride, isopentanoyl chloride, 2-ethoxyacetyl chloride, 2-ethylhexyl chloride, lauroyl chloride, decanoyl chloride, benzoyl chloride, 4-methylbenzoyl chloride or 2, 4-dichlorobenzoyl chloride, the alkyl chloroformate is one or more of 2-ethylhexyl chloroformate, phenyl chloroformate, benzyl chloroformate, cyclopentyl chloroformate, cyclohexyl chloroformate, isobutyl chloroformate, n-pentyl chloroformate, 4-tert-butylcyclohexyl chloroformate, 2-ethoxyethyl chloroformate, 3-methoxybutyl chloroformate, butyl chloroformate, hexadecyl chloroformate, tetradecyl chloroformate or isopropyl chloroformate, the molar ratio of the catalyst to the alkyl acyl chloride or the alkyl chloroformate is 1.0-1.2:1, the molar ratio of the oxidant to the alkyl acyl chloride or the alkyl chloroformate is 0.5-1.2:1, the molar ratio of the oxidant to the alkyl chloroformate is 1.5-1:1, and the reaction time is 1.5-3-6 h.
Washing in the step S2 is deionized water washing, separating into standing separation, drying and filtering after separating, wherein the drying agent is one of anhydrous sodium sulfate, anhydrous magnesium sulfate, 3A molecular sieve, 5A molecular sieve or alumina drying agent, and the dosage of the drying agent is 0.8-1.2% of the mass of the alkyl acyl chloride or the alkyl chloroformate.
The auxiliary agent in the step S3 is an organic solvent or emulsion, wherein the organic solvent is one or more of 2-methoxy-2-methyl heptane, isododecane, cyclohexane or petroleum ether, and the emulsion is composed of deionized water, an emulsifying agent, a dispersing agent and an antifreezing agent;
Wherein the emulsifier is one of polyoxyethylene hydrogenated castor oil, polyoxyethylene castor oil, stearyl polyoxyethylene ether, fatty alcohol polyoxyethylene polyoxypropylene ether, polyoxyethylene polyoxypropylene copolymer, sorbitan fatty acid ester or polysorbate, the dispersing agent is polyacrylic acid, the molecular weight of the dispersing agent is 6000-8000, the antifreezing agent is ethylene glycol methyl ether or ethylene glycol ethyl ether, the amount of the emulsifying agent is 0.1-2wt%, the amount of the dispersing agent is 0.05-2wt% and the amount of the antifreezing agent is 5-25wt% based on 100wt% of the emulsion.
The auxiliary peroxide in the step S3 is solvent peroxide or water emulsion peroxide, wherein the peroxide content in the solvent peroxide is 30-80wt% and the peroxide content in the water emulsion peroxide is 25-60wt%.
In order to improve the safety level of the organic peroxide production device, the heat exchanger with the fins is arranged on the coil of the reaction kettle, so that the problem of uneven temperature regulation in the reaction kettle is solved, radial fins or axial fins are arranged on the periphery of the heat exchanger of the coil of the reaction kettle, and the heat exchange efficiency of the coil can be optimized and improved by changing the number of the fins and the size of the fins on the heat exchange coil.
The heat transfer device in the reaction kettle can generate a large amount of reaction heat by quickly transferring the mixture of the catalyst, the oxidant and the chloroformate compound in the reaction kettle, can effectively control the reaction temperature in the reaction kettle, reduces the accumulation of heat in the reaction kettle, and can reduce the decomposition risk of organic peroxide products with poor thermal stability. Meanwhile, compared with the common heat exchange coil, the heat exchange coil with the heat exchanger can improve the contact area of reactants, has good heat transfer performance, does not need to carry out secondary processing on the coil, has easy manufacturing process and low cost, improves the heat exchange area of the coil, enhances the heat transfer efficiency of the surface of the coil, increases the peroxide reaction rate, improves the synthesis efficiency of peroxide products, and reduces COD emission.
The invention has the beneficial effects that:
The external fins are vertically arranged on the outer side of the fixed plate, the included angle between the axis of the long side of each external fin and the axis of the heat exchange tube is 0-90 degrees, the grooves are arranged on the inner side of the fixed plate, and each groove comprises an inward concave groove, an outward convex groove and a straight groove.
When the heat exchange tube is a straight tube, the two fixing plates provided with the straight grooves are oppositely arranged, screw holes for accommodating fixing bolts are formed in the fixing plates, the fixing bolts penetrate through the screw holes to connect the two fixing plates, buffer gaskets are arranged between the fixing bolts and the fixing plates, the grooves can be fixed in accordance with the radian of a coil structure, so that the heat exchange tube can be fixed on the coil to realize heat exchange, when the concave grooves and the convex grooves are oppositely arranged, the two grooves form arc-shaped pipelines inside and are suitable for heat exchange on the arc-shaped coil, and when the straight grooves are oppositely arranged, the two grooves form straight pipelines inside and are suitable for heat exchange on the straight pipelines.
The invention can realize the high-efficiency heat transfer performance by utilizing the heat exchanger, thereby being capable of stably preparing the peroxide product, reducing the feeding reaction time and improving the conversion efficiency from the initial raw material to the peroxide product.
The heat exchanger with the external fins in the reaction kettle has strong heat transfer capability, the external fins are mutually arranged in parallel, a narrow channel is formed on the reaction kettle coil, when fluid passes through, reaction liquid is dispersed into liquid flow, and the liquid flow is fully contacted with the external fins to perform heat exchange, so that the heat exchange effect can be further improved by matching with a material with good heat transfer performance. Compared with the conventional coil heat exchanger, the effective heat transfer area is increased, the heat transfer coefficient is improved, the heat transfer capacity is enhanced due to the increase of the heat transfer area per unit volume, the coil length can be reduced, the coil diameter or the layout height can be reduced under the same heat load, the compactness of the reaction kettle structure is enhanced, and the arrangement is convenient.
The heat exchanger has compact structure, uses less materials, can flexibly select heat exchanger materials according to different heat transfer and process requirements, selects materials with good heat transfer performance and is matched with external fins with different angles, and the heat transfer efficiency can be further improved.
The temperature change in the reaction kettle is effectively controlled, so that the decomposition and damage of the organic peroxide product in a local high-temperature environment can be reduced, and the yield and the product quality of the organic peroxide product are improved.
The invention adopts a mode of fixing and combining a plurality of external fins, reduces the production cost of the fins, has simple process and flexible and convenient installation, can improve the reaction rate, can timely dissipate heat, shortens the whole reaction time and avoids local overheating. Effectively avoids side reaction and reduces potential safety hazard caused by instability of peroxide.
The external fin can also improve the dispersion effect of the mixed solution, increase the specific surface area of the mixed solution, further improve the mixing efficiency and the safe production of the peroxide product synthesis process, and reduce the accident potential of thermal decomposition of the peroxide product.
The invention adopts the phlegmatizer to prepare the peroxide product, which can prevent the decomposition of substances in the reaction process, ensures the production safety and high-efficiency synthesis of the peroxide product, can extract the synthesized peroxide product from the water phase in time, prevents the peroxide product from being decomposed by water phase impurities, improves the yield of the peroxide product, ensures that the peroxide product containing the phlegmatizer can be more easily mixed with the emulsifier mother liquor to form a water emulsion type product, and can be prepared into the water emulsion type alkyl peroxide or the solvent type alkyl peroxide, thereby meeting the peroxide transportation classification requirement.
The prepared water emulsion type peroxide product adopts the water-based polyacrylic acid dispersing agent, the obtained water emulsion type peroxide product has low viscosity, is easier to disperse in a PVC polymerization system, and is more suitable for the PVC polymerization process.
More importantly, the invention uses 2-methoxy-2-methyl heptane as peroxide desensitizer, which has good desensitizing effect.
1. The 2-methoxy-2-methyl heptane has good intersolubility with peroxide products, and the 2-methoxy-2-methyl heptane has good stability and compatibility after being mixed with peroxide products, and the energy release rate is reduced by diluting the peroxide.
2. The 2-methoxy-2-methyl heptane molecule has tertiary carbon group and ether bond, the chemical structure is similar to tertiary butyl or tertiary carbon alkyl structure in peroxide product, and the adsorption system can be formed through physical adsorption and hydrogen bond, so that the activity of peroxide molecule is reduced, and the risk of decomposition of peroxide molecule due to heat, light or mechanical stimulation is reduced.
3. The 2-methoxy-2-methyl heptane is added in advance before the reaction, which is favorable for the peroxidation of alkyl acyl chloride or alkyl chloroformate, and is more favorable for the formation of peroxide molecules because of tertiary carbon groups and ether bonds on the molecules, thereby playing the role of a template agent.
4. The 2-methoxy-2-methyl heptane molecule contains an oxygen atom which has stronger electronegativity and increases the reactivity of alpha hydrogen atoms. The active hydrogen atoms can react with free radicals generated by peroxide decomposition to generate stable free radicals, so that the oxidation chain reaction is blocked, and the decomposition of the peroxide is avoided.
Drawings
FIG. 1 is a schematic structural view of a reaction kettle of the invention;
FIG. 2 is a schematic view of the heat exchanger of the present invention disposed in a straight tube;
FIG. 3 is a schematic view of the heat exchanger of the present invention disposed in an arcuate tube configuration;
FIG. 4 is a schematic cross-sectional view of a heat exchanger of the present invention;
FIG. 5 is a schematic view of a heat exchanger with straight grooves according to the present invention;
FIG. 6 is a schematic diagram of a heat exchanger with straight grooves according to the present invention;
FIG. 7 is a schematic view of a heat exchanger with concave grooves according to the present invention;
FIG. 8 is a schematic view of a heat exchanger with a convex groove according to the present invention;
FIG. 9 is a schematic diagram II of a heat exchanger with concave grooves according to the present invention;
FIG. 10 is a schematic diagram of a heat exchanger with a convex groove according to the present invention;
The heat exchange tube comprises a heat exchange tube body 1, a fixing bolt 2, a heat exchanger 4, a buffer gasket 5, a reaction kettle 6, a stirrer 7, a motor 8, an additive liquid inlet 9, a raw material inlet 10, a discharge port 301, an external fin 302, a fixing plate 303, a screw hole 3021, a concave groove 3022, a convex groove 3023 and a straight groove.
Detailed Description
Embodiments of the present invention are further described below with reference to the accompanying drawings.
Example 1
As shown in fig. 1, 4, 5, 9 and 10, the heat exchange device for preparing peroxide according to the invention comprises a heat exchange tube 1 arranged in a reaction kettle 5, wherein a plurality of heat exchangers 3 are arranged on the heat exchange tube 1, each heat exchanger 3 comprises a plurality of external fins 301, the external fins 301 are arranged on a fixed plate 302 at intervals, the fixed plate 302 is provided with grooves in cooperation with the heat exchange tube 1, and the heat exchange tube 1 is arranged in the grooves of the fixed plate 302.
The external fins 301 are vertically arranged on the outer side of the fixed plate 302, the included angle between the long-side axis of each external fin 301 and the axis of the heat exchange tube 1 is 0 degrees, the grooves are arranged on the inner side of the fixed plate 302, and each groove comprises a concave groove 3021, a convex groove 3022 and a straight groove 3023.
When the heat exchange tube 1 is an arc tube, the fixing plate 302 provided with the concave groove 3021 and the fixing plate 302 provided with the convex groove 3022 are arranged oppositely, when the heat exchange tube 1 is a straight tube, the two fixing plates 302 provided with the straight groove 3023 are arranged oppositely, screw holes 303 for accommodating the fixing bolts 2 are arranged on the fixing plates 302, the fixing bolts 2 penetrate through the screw holes 303 to connect the two fixing plates 302, and buffer gaskets 4 are arranged between the fixing bolts 2 and the fixing plates 302.
Be provided with agitator 6 in reation kettle 5, agitator 6 top runs through reation kettle 5 and is connected with motor 7, and reation kettle 5 top is provided with raw materials entry 9 and additive liquid entry 8, and reation kettle 5 bottom is provided with discharge gate 10.
The peroxide preparation method adopting the heat exchange device for preparing peroxide comprises the following steps:
s1, adding 12kg of 2-methoxy-2-methyl heptane, 7.82kg of 40wt% sodium hydroxide and 4.6kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 13kg of 3, 5-trimethyl hexanoyl chloride, and continuously reacting for 6 hours at 10 ℃, thus obtaining a crude product after the reaction is finished;
s2, stirring and washing the crude product for 20min by using 13kg of deionized water, standing and separating, repeating the operation once, then adding 0.13kg of anhydrous sodium sulfate for drying, and filtering to obtain bis (3, 5-trimethylhexanoyl) peroxide containing 2-methoxy-2-methylheptane, wherein the yield is 93.1wt%;
S3, taking a part of bis (3, 5-trimethyl hexanoyl chloride) peroxide, and mixing with 2-methoxy-2-methyl heptane to obtain 3kg of solvent type bis (3, 5-trimethyl hexanoyl) peroxide, wherein the content of the bis (3, 5-trimethyl hexanoyl) peroxide is 40wt%.
Example 2
As shown in fig. 1, 2, 3, 6, 7 and 8, the included angle between the long side axis of the external fin 301 and the axis of the heat exchange tube 1 in the heat exchange device for preparing peroxide is 90 degrees, and the rest of the structure is the same as that of example 1.
Preparing emulsion:
72.5kg of deionized water, 25kg of ethylene glycol methyl ether, 2kg of polyoxyethylene castor oil and 0.5kg of aqueous polyacrylic acid dispersing agent with the molecular weight of 6000 are mixed and stirred uniformly at room temperature to obtain emulsion.
The peroxide preparation method adopting the heat exchange device for preparing peroxide comprises the following steps:
s1, adding 4kg of 2-methoxy-2-methyl heptane, 7.72kg of 40wt% sodium hydroxide and 5.2kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 12kg of 3, 5-trimethyl hexanoyl chloride, and continuously reacting for 4 hours at 20 ℃, thus obtaining a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation once, then adding 0.12kg of anhydrous sodium sulfate for drying, and filtering to obtain bis (3, 5-trimethylhexanoyl) peroxide containing 2-methoxy-2-methylheptane, wherein the yield is 93.5wt%;
S3, taking a part of bis (3, 5-trimethyl hexanoyl) peroxide, and mixing with the emulsion to obtain 3kg of water emulsion type bis (3, 5-trimethyl hexanoyl) peroxide, wherein the content of the bis (3, 5-trimethyl hexanoyl) peroxide is 60wt%.
Example 3
The included angle between the long side axis of the external fin 301 and the axis of the heat exchange tube 1 in the heat exchange device for preparing peroxide is 45 degrees, and the rest of the structure is the same as that of the example 1.
The peroxide preparation method adopting the heat exchange device for preparing peroxide comprises the following steps:
S1, adding 4.5kg of 2-methoxy-2-methyl heptane, 16.7kg of 35wt% sodium hydroxide and 7.87kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 13kg of isobutyryl chloride, and continuing to react for 3 hours at the temperature of 0 ℃ to obtain a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation once, then adding 0.11kg of 3A molecular sieve for drying, and filtering to obtain diisobutyryl peroxide containing 2-methoxy-2-methyl heptane, wherein the yield is 96.6wt%;
S3, taking a part of diisobutyryl peroxide, and mixing with 2-methoxy-2-methyl heptane to obtain 3kg of solvent-type diisobutyryl peroxide, wherein the content of the diisobutyryl peroxide is 30wt%.
Example 4
Preparing emulsion:
78kg of deionized water, 20kg of ethylene glycol methyl ether, 1kg of polyoxyethylene castor oil and 1kg of aqueous polyacrylic acid dispersing agent with molecular weight of 7500 are mixed, and stirred uniformly at room temperature to obtain emulsion.
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
S1, adding 4kg of 2-methoxy-2-methyl heptane, 16.1kg of 30wt% sodium hydroxide and 7.47kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 13kg of isobutyryl chloride, and continuing to react for 4 hours at a temperature of minus 5 ℃ to obtain a crude product after the reaction is finished;
s2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation once, then adding 0.13kg of anhydrous magnesium sulfate for drying, and filtering to obtain diisobutyryl peroxide containing 2-methoxy-2-methyl heptane, wherein the yield is 96.3wt%;
S3, taking a part of diisobutyryl peroxide, and mixing with the emulsion to obtain 3kg of water emulsion type diisobutyryl peroxide, wherein the content of the diisobutyryl peroxide is 25wt%.
Example 5
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
S1, adding 3kg of 2-methoxy-2-methyl heptane, 7.36kg of 40wt% sodium hydroxide and 6.81kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 12kg of 2-ethylhexyl chloroformate, and continuing to react for 4 hours at 10 ℃ to obtain a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 11kg of deionized water, standing and separating, repeating the operation once, then adding 0.11kg of anhydrous sodium sulfate for drying, and filtering to obtain bis (2-ethylhexyl) peroxydicarbonate containing 2-methoxy-2-methylheptane, wherein the yield is 94.9wt%;
S3, taking a part of the di (2-ethylhexyl) peroxydicarbonate, and mixing with 2-methoxy-2-methyl heptane to obtain 3kg of solvent-type di (2-ethylhexyl) peroxydicarbonate, wherein the content of the di (2-ethylhexyl) peroxydicarbonate is 70wt%.
Example 6
Preparing emulsion:
77.5kg of deionized water, 20kg of ethylene glycol methyl ether, 2kg of polyoxyethylene castor oil and 0.5kg of aqueous polyacrylic acid dispersing agent with molecular weight of 8000 are mixed and stirred uniformly at room temperature to obtain emulsion.
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
S1, adding 4kg of 2-methoxy-2-methyl heptane, 6.92kg of 40wt% sodium hydroxide and 4.81kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 12kg of 2-ethylhexyl chloroformate, and continuing to react for 4 hours at 20 ℃ to obtain a crude product after the reaction is finished;
s2, stirring and washing the crude product for 20min by using 11kg of deionized water, standing and separating, repeating the operation once, then adding 0.11kg of alumina drying agent for drying, and filtering to obtain di (2-ethylhexyl) peroxydicarbonate containing 2-methoxy-2-methylheptane, wherein the yield is 94.1wt%;
S3, taking a part of the di (2-ethylhexyl) peroxydicarbonate, and mixing with the emulsion to obtain 3kg of water emulsion type di (2-ethylhexyl) peroxydicarbonate, wherein the content of the di (2-ethylhexyl) peroxydicarbonate is 40wt%.
Example 7
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
s1, adding 5kg of 2-methoxy-2-methyl heptane, 12.38kg of 30wt% sodium hydroxide and 5.13 kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 12kg of 2-ethoxyethyl chloroformate, and continuing to react for 5 hours at 25 ℃, thus obtaining a crude product after the reaction is finished;
s2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation once, then adding 0.13kg of anhydrous magnesium sulfate for drying, and filtering to obtain bis (2-ethoxy) ethyl peroxydicarbonate containing 2-methoxy-2-methylheptane, wherein the yield is 96.2wt%;
s3, taking a part of bis (2-ethoxy) ethyl peroxydicarbonate, and mixing with 2-methoxy-2-methyl heptane to obtain 3kg of solvent bis- (2-ethoxy) ethyl peroxydicarbonate, wherein the content of the bis (2-ethoxy) ethyl peroxydicarbonate is 50wt%.
Example 8
Preparing emulsion:
83kg of deionized water, 15kg of ethylene glycol methyl ether, 1.5kg of polyoxyethylene castor oil and 0.5kg of an aqueous polyacrylic acid dispersing agent with molecular weight of 8000 are mixed and stirred uniformly at room temperature to obtain an emulsion.
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
s1, adding 3kg of 2-methoxy-2-methyl heptane, 8.13kg of 40wt% sodium hydroxide and 8.63kg of 27.5wt% hydrogen peroxide into a reaction kettle 5, stirring for reaction, then slowly adding 12kg of 3-methoxybutyl chloroformate, and continuing to react for 3 hours at 15 ℃, thus obtaining a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation for one time, then adding 0.12kg of anhydrous sodium sulfate for drying, and filtering to obtain bis (3-methoxybutyl) peroxydicarbonate with the yield of 96.7wt%;
s3, taking a part of the bis (3-methoxybutyl) peroxydicarbonate, and mixing with the emulsion to obtain 3kg of water emulsion type bis (3-methoxybutyl) peroxydicarbonate, wherein the content of the bis (3-methoxybutyl) peroxydicarbonate is 50wt%.
Example 9
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
S1, adding 1.5kg of 2-methoxy-2-methyl heptane, 13.54kg of 30wt% sodium hydroxide and 11.1kg of 80wt% tertiary butyl hydroperoxide into a reaction kettle 5, stirring for reaction, then slowly adding 12kg of pivaloyl chloride, and continuing to react for 3 hours at 20 ℃, and obtaining a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation once, then adding 0.12kg of anhydrous magnesium sulfate for drying, and filtering to obtain tert-butyl peroxypivalate containing 2-methoxy-2-methylheptane, wherein the yield is 91.7wt%;
S3, taking a part of tert-butyl peroxypivalate, and mixing with 2-methoxy-2-methyl heptane to obtain 3kg of solvent tert-butyl peroxypivalate, wherein the content of the tert-butyl peroxypivalate is 80wt%.
Example 10
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
S1, adding 0.8kg of 2-methoxy-2-methyl heptane, 7.85kg of 30wt% sodium hydroxide and 6.61kg of 70wt% tertiary butyl hydroperoxide into a reaction kettle 5, stirring for reaction, then slowly adding 10kg of 2-ethylhexyl chloroformate, and continuing to react for 5 hours at 15 ℃ to obtain a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation, adding 0.12kg of anhydrous sodium sulfate for drying, and filtering to obtain the tert-butyl peroxy-2-ethylhexyl carbonate with the yield of 97.8wt%.
Example 11
The peroxide preparation method adopting the peroxide heat exchange device comprises the following steps:
S1, adding 1.2kg of 2-methoxy-2-methyl heptane, 18.16kg of 20wt% sodium hydroxide and 10.4kg of 70wt% tertiary butyl hydroperoxide into a reaction kettle 5, stirring for reaction, then slowly adding 10kg of isopropyl chloroformate, and continuing to react for 4 hours at 20 ℃ to obtain a crude product after the reaction is finished;
S2, stirring and washing the crude product for 20min by using 10kg of deionized water, standing and separating, repeating the operation for one time, then adding 0.1kg of anhydrous sodium sulfate for drying, and filtering to obtain isopropyl tert-butyl peroxycarbonate with the yield of 97.4wt%;
S3, taking a part of tert-butyl peroxyisopropyl carbonate, and mixing with 2-methoxy-2-methyl heptane to obtain 3kg of solvent type tert-butyl peroxyisopropyl carbonate, wherein the content of the tert-butyl peroxyisopropyl carbonate is 60wt%.
In examples 4 to 11, the heat exchanger for peroxide production was constructed in the same manner as in example 1.
Comparative example 1
The procedure of example 1 was repeated except for adding no 2-methoxy-2-methylheptane to step S1, whereby the yield was 82.3%.
Comparative example 2
The procedure used was as in example 1, except that heat exchanger 3 was not used in the peroxide production heat exchanger, and the yield was 84.7wt%.
In summary, as is clear from the comparison of example 1 and example 1, the phlegmatizer added in the present invention can prevent peroxide products from being decomposed by water phase impurities during the reaction process, and improve the yield of peroxide products, and as is clear from the comparison of example 2 and example 1, the heat exchanger 3 with external fins 301 added in the reaction kettle 5 can improve the heat transfer efficiency, promote the forward progress of peroxide reaction, improve the yield of products, and the present invention is applicable to the production of various substances, has wide application, and improves the synthesis efficiency of substances.
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