CN111303060A - Preparation method of metal deactivator - Google Patents
Preparation method of metal deactivator Download PDFInfo
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- CN111303060A CN111303060A CN202010197443.XA CN202010197443A CN111303060A CN 111303060 A CN111303060 A CN 111303060A CN 202010197443 A CN202010197443 A CN 202010197443A CN 111303060 A CN111303060 A CN 111303060A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D249/00—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
- C07D249/16—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms condensed with carbocyclic rings or ring systems
- C07D249/18—Benzotriazoles
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
- C10M133/38—Heterocyclic nitrogen compounds
- C10M133/44—Five-membered ring containing nitrogen and carbon only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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Abstract
The invention discloses a preparation method of a metal deactivator, which comprises the following steps: and carrying out Mannich reaction on the methylbenzotriazole, formaldehyde and diisooctylamine to prepare the methylbenzotriazole metal deactivator. The method adopts the Mannich reaction, does not introduce an acid catalyst and a water phase, has less side reaction, high yield, simple preparation process, stable reaction, simple post-treatment and no generation of three wastes, and is a green synthesis process; has better metal corrosion inhibition, oxidation resistance, abrasion resistance and oil solubility.
Description
Technical Field
The invention belongs to the technical field of lubricating oil additives, relates to a preparation method of a metal deactivator, and particularly relates to a preparation method of a methylbenzotriazole metal deactivator.
Background
The metal deactivator is a compound containing S, P, N or other non-metal elements, and the variety mainly includes benzotriazole derivatives, thiadiazole derivatives, and the like. The deactivator has no antioxidant effect, but can 'deactivate' the activity of metal, thereby playing a role in delaying the oxidation speed of oil products.
The methyl benzotriazole metal deactivator not only improves the oil solubility of methyl benzotriazole, but also has excellent oxidation resistance, copper corrosion inhibition and metal deactivation performance. The metal deactivator has less consumption (0.01-0.05%), has outstanding synergy when being compounded with a phenolic antioxidant, can obviously reduce the consumption of the antioxidant, and simultaneously obviously improves the oxidation resistance of oil products, and is also found to play a good optimization role in a lubricating oil filterability experiment when being added into a compounding agent formula.
CN1107470A discloses a preparation method of a metal deactivator, which comprises the following steps: sodium methyl benzotriazole, secondary aliphatic amine or formaldehyde is taken as a raw material, acid is taken as a catalyst, and water is taken as a reaction medium. The reaction temperature is 70-100 ℃, the reaction time is 2-6h, and the steps of layering, washing, drying and the like are carried out after the reaction.
The preparation method has the following defects:
1. the raw material of the methylbenzotriazole sodium is required to be prepared, and the preparation of the methylbenzotriazole sodium requires multi-step synthesis, so that the cost is increased;
2. the acidic catalyst introduced in the reaction is easy to remain in the product, brings acidic impurities and is not easy to remove;
3. repeated washing can bring a large amount of industrial wastewater, and is not environment-friendly and economical. But also requires distillation of large amounts of solvent, increasing costs.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a metal deactivator, which has the advantages of simplified process, stable reaction, simple post-treatment, better metal corrosion inhibition, oxidation resistance, wear resistance and oil solubility.
The invention discloses a preparation method of a metal deactivator, which comprises the following steps:
carrying out Mannich reaction on methylbenzotriazole, formaldehyde and diisooctylamine to prepare a methylbenzotriazole metal deactivator; wherein the reaction process is as follows:
as a further improvement of the present invention, the preparation method specifically comprises:
mixing the methylbenzotriazole and the diisooctylamine in an organic solvent, heating, dissolving and preserving heat;
at a certain temperature, formaldehyde is added into the solution to carry out aminomethylation and electrophilic addition reaction.
As a further improvement of the invention, the molar ratio of the methylbenzotriazole to the formaldehyde to the diisooctylamine is (1.0-1.5): (0.9-1.2).
As a further improvement of the method, the reaction temperature of the Mannich reaction is 80-120 ℃, and the reaction time is 8-20 hours.
As a further improvement of the present invention, the preparation method further comprises:
and carrying out reduced pressure distillation on the product of the Mannich reaction to obtain the methylbenzotriazole metal deactivator.
As a further improvement of the present invention, the organic solvent is an ethanol solvent.
As a further improvement of the invention, the ratio of the addition amount of the organic solvent to the mass sum of the methylbenzotriazole and the diisooctylamine is 1 (0.6-0.9).
Compared with the prior art, the invention has the beneficial effects that:
the method adopts the Mannich reaction, does not introduce an acid catalyst and a water phase, has less side reaction, high yield, simple preparation process, stable reaction, simple post-treatment and no generation of three wastes, and is a green synthesis process; has better metal corrosion inhibition, oxidation resistance, abrasion resistance and oil solubility.
Drawings
FIG. 1 is an IR spectrum of a metal deactivator prepared in example 1 of the present invention;
FIG. 2 is a NMR H spectrum of a metal deactivator prepared in example 1 of the present invention;
FIG. 3 is a nuclear magnetic resonance C spectrum of the metal deactivator prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention is described in further detail below with reference to the attached drawing figures:
the invention provides a preparation method of a metal deactivator, which comprises the following steps:
under the condition of not introducing an acid catalyst and a water phase, carrying out Mannich reaction on methylbenzotriazole, formaldehyde and diisooctylamine to prepare a methylbenzotriazole metal deactivator;
wherein the reaction process is as follows:
the design principle of the preparation method is as follows:
the methylbenzotriazole has acidity, can provide catalytic action for Mannich reaction, does not need to introduce an additional acidic catalyst, and the final experimental result shows that the reaction is simple and feasible, no water phase is introduced, the post-treatment is not complex, no three wastes are generated, and the production process is greatly simplified.
Further, the preparation method of the metal deactivator specifically comprises the following steps:
mixing methylbenzotriazole and diisooctylamine in an organic solvent according to a certain proportion, heating, dissolving and preserving heat;
slowly adding formaldehyde into the solution at a certain temperature to carry out aminomethylation reaction, and finally carrying out Mannich electrophilic addition reaction under the reflux condition;
and carrying out reduced pressure distillation on the product of the Mannich reaction to obtain the methylbenzotriazole metal deactivator.
Furthermore, the preparation method of the metal deactivator specifically comprises the following steps:
adding methylbenzotriazole and diisooctylamine into a four-neck flask, and adding an organic solvent;
replacing air in the bottle with nitrogen, starting heating, starting stirring when the temperature reaches 30 ℃, wherein the stirring speed is preferably 280-350 rpm; continuously heating to 45 ℃, and keeping the temperature for 25-35 min;
after the heat preservation is finished, slowly dripping formaldehyde at the temperature, stirring for 1-2 hours at the temperature after finishing dripping, and carrying out aminomethylation reaction;
continuously increasing the temperature to the reflux temperature to carry out Mannich electrophilic addition reaction, wherein the reaction temperature of the Mannich reaction is 80-120 ℃, and the reaction time is 8-20 h;
carrying out reduced pressure distillation on a product of the Mannich reaction to obtain a methylbenzotriazole metal deactivator; the vacuum degree of the reduced pressure distillation is preferably 0.08MPa to 0.095 MPa.
The experimental results show that:
the appearance of the product is light yellow liquid; the residual amount of the methylbenzotriazole is 0.75 to 1.30 weight percent, and the comparative product is 1.42 to 2.41 weight percent; the residual content of diisooctylamine is 0.58-1.82 wt%, and the content of the comparable control product is 1.85-2.63 wt%. The corrosion of the copper sheet (150 ℃, 1h) is less than or equal to 1 b; the water content (m/m) is less than or equal to 0.15; kinematic viscosity at 40 ℃ of 80mm2About/s; the density (20 ℃) is about 0.950; the base number is 143.11-148.52mgKOH/g, the weight loss of the copper sheet in unit area is 0.15-0.30 when the copper sheet is put into a formula of the hydraulic oil complexing agent, and the weight loss of the copper sheet is 0.35-0.85 when compared with that of a control product.
Preferably, the first and second liquid crystal materials are,
in the preparation method, the molar ratio of the methylbenzotriazole to the formaldehyde to the diisooctylamine is (1.0-1.5): 0.9-1.2.
In the preparation method, the organic solvent is an ethanol solvent, and the ratio of the addition amount of the organic solvent to the mass sum of the methylbenzotriazole and the diisooctylamine is 1 (0.6-0.9).
The invention adopts the Mannich reaction to optimize the synthetic route, determines the optimal feeding ratio and the optimal feeding sequence of the reaction, does not introduce an acid catalyst and a water phase, has less side reactions, high yield (more than 98 percent), simple preparation process, stable reaction, simple post-treatment and no generation of three wastes, and is a green synthetic process; the obtained metal deactivator product is light yellow liquid, has better metal corrosion inhibition, oxidation resistance and oil solubility, and greatly improves the performance of the product.
In order to further illustrate the present invention, the following examples are provided to describe the preparation method of the new methylbenzotriazole metal deactivator of the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
A1000 ml four-necked flask equipped with a thermometer and a condenser was charged with 146.47g of methylbenzotriazole, 265.61g of diisooctylamine, and 247.25g of ethanol. Nitrogen gas was introduced into the reaction flask, and after the air in the flask was sufficiently replaced, heating was started. When the temperature reached about 30 ℃, the stirring was started at a rate of 350 rpm. Gradually heating to 45 ℃, keeping the temperature for 0.5h, adding 101.35g of formaldehyde solution into the dripping device, slowly dripping the formaldehyde solution at 45 ℃ to start reaction, reacting for 1.5h at the temperature after dripping is finished, then continuously heating to 82-85 ℃, reacting for 12h under a reflux state, and stopping reaction; cooling the reaction to normal temperature, reducing the vacuum degree to 0.08-0.095 Mpa and steaming to 140 ℃ to obtain light yellow liquid, cooling to normal temperature and carrying out vacuum filtration to obtain filtrate, namely the product. The collected distillate can be used as a recovered solvent for continuous recycling.
As shown in fig. 1 to 3, in the invention, the methyl benzotriazole derivative product prepared in example 1 is subjected to appearance visual inspection, infrared analysis, liquid chromatography analysis, oil solubility, copper corrosion and abrasion resistance experiment determination, and the content of diisooctylamine and the content of TTA in the methyl benzotriazole derivative product prepared in example 1 are 0.75 wt% and 0.58 wt%, respectively; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b;the water content% (m/m) is 0.08; the oil solubility is good; the potential base number is 144.56 mgKOH/g; the density (20 ℃ C.) was 0.9502g/cm3(ii) a A viscosity (40 ℃) of 80mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.15.
Example 2
A1000 ml four-necked flask equipped with a thermometer and a condenser was charged with 146.47g of methylbenzotriazole, 241.46g of diisooctylamine, and 232.76g of ethanol. Nitrogen gas was introduced into the reaction flask, and after the air in the flask was sufficiently replaced, heating was started. When the temperature reached about 30 ℃, the stirring was started at a rate of 350 rpm. Gradually heating to 45 ℃, keeping the temperature for 0.5h, adding 121.62g of formaldehyde solution into a dripping device, slowly dripping the formaldehyde solution at 45 ℃ to start reaction, reacting at the temperature for 1.5h after dripping is finished, then continuously heating to 82-85 ℃, reacting for 13h under a reflux state, and stopping reaction; cooling the reaction to normal temperature, reducing the vacuum degree to 0.08-0.095 Mpa and steaming to 140 ℃ to obtain light yellow liquid, cooling to normal temperature and carrying out vacuum filtration to obtain filtrate, namely the product. The collected distillate can be used as a recovered solvent for continuous recycling.
According to the invention, the methyl benzotriazole derivative product prepared in example 2 is subjected to appearance visual inspection, infrared analysis, liquid chromatography analysis, oil solubility, copper corrosion and abrasion resistance experiment determination, and the content of diisooctylamine and TTA in the methyl benzotriazole derivative product prepared in example 2 is 1.25 wt% and 1.11 wt%; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b; the water content% (m/m) was 0.09; the oil solubility is good; the potential base number is 146.25 mgKOH/g; the density (20 ℃) was 0.9478g/cm 3; a viscosity (40 ℃) of 88mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.30.
Example 3
A1000 ml four-necked flask equipped with a thermometer and a condenser was charged with 159.78g of methylbenzotriazole, 265.61g of diisooctylamine, and 255.23g of ethanol. Nitrogen gas was introduced into the reaction flask, and after the air in the flask was sufficiently replaced, heating was started. When the temperature reached about 30 ℃, the stirring was started at a rate of 350 rpm. Gradually heating to 45 ℃, keeping the temperature for 0.5h, adding 121.62g of formaldehyde solution into a dripping device, slowly dripping the formaldehyde solution at 45 ℃ to start reaction, reacting at the temperature for 1.5h after dripping is finished, then continuously heating to 70-72 ℃, reacting for 10h under a reflux state, and stopping reaction; cooling the reaction to normal temperature, reducing the vacuum degree to 0.08-0.095 Mpa and steaming to 140 ℃ to obtain light yellow liquid, cooling to normal temperature and carrying out vacuum filtration to obtain filtrate, namely the product. The collected distillate can be used as a recovered solvent for continuous recycling.
According to the invention, the methyl benzotriazole derivative product prepared in example 3 is subjected to appearance visual inspection, infrared analysis, liquid chromatography analysis, oil solubility, copper corrosion and abrasion resistance experiment determination, and the content of diisooctylamine and TTA in the methyl benzotriazole derivative product prepared in example 3 is 1.52 wt% and 1.48 wt%; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b; the water content% (m/m) is 0.08; the oil solubility is good; the potential base number is 144.25 mgKOH/g; the density (20 ℃ C.) was 0.9498g/cm3(ii) a A viscosity (40 ℃) of 89mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.25.
Example 4
A1000 ml four-necked flask equipped with a thermometer and a condenser was charged with 173.10g of methylbenzotriazole, 217.31g of diisooctylamine, and 234.25g of ethanol. Nitrogen gas was introduced into the reaction flask, and after the air in the flask was sufficiently replaced, heating was started. When the temperature reached about 30 ℃, the stirring was started at a rate of 350 rpm. Gradually heating to 45 ℃, keeping the temperature for 0.5h, adding 113.51g of formaldehyde solution into the dripping device, slowly dripping the formaldehyde solution at 45 ℃ to start reaction, reacting for 1.5h at the temperature after dripping is finished, then continuously heating to 70-72 ℃, reacting for 20h under a reflux state, and stopping reaction; cooling the reaction to normal temperature, reducing the vacuum degree to 0.08-0.095 Mpa and steaming to 140 ℃ to obtain light yellow liquid, cooling to normal temperature and carrying out vacuum filtration to obtain filtrate, namely the product. The collected distillate can be used as a recovered solvent for continuous recycling.
Preparation of the invention in example 4The prepared methyl benzotriazole derivative product is subjected to appearance visual inspection, infrared analysis, liquid chromatography analysis, oil solubility, copper corrosion and abrasion resistance experiment determination, and the content of diisooctylamine and TTA in the methyl benzotriazole derivative product prepared in example 4 is 1.72 wt% and 1.32 wt%; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b; the water content% (m/m) is 0.08; the oil solubility is good; the potential base number is 143.56 mgKOH/g; the density (20 ℃ C.) was 0.9522g/cm3(ii) a A viscosity (40 ℃) of 92mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.23.
Example 5
A1000 ml four-necked flask equipped with a thermometer and a condenser was charged with 130.48 methylbenzotriazole, 236.63g of diisooctylamine, and 220.27g of ethanol. Nitrogen gas was introduced into the reaction flask, and after the air in the flask was sufficiently replaced, heating was started. When the temperature reached about 30 ℃, the stirring was started at a rate of 350 rpm. Gradually heating to 45 ℃, keeping the temperature for 0.5h, adding 85.13g of formaldehyde solution into the dripping device, slowly dripping the formaldehyde solution at 45 ℃ to start reaction, reacting for 1.5h at the temperature after dripping is finished, then continuously heating to 70-72 ℃, reacting for 18h under a reflux state, and stopping reaction; cooling the reaction to normal temperature, reducing the vacuum degree to 0.08-0.095 Mpa and steaming to 140 ℃ to obtain light yellow liquid, cooling to normal temperature and carrying out vacuum filtration to obtain filtrate, namely the product. The collected distillate can be used as a recovered solvent for continuous recycling.
According to the invention, the methyl benzotriazole derivative product prepared in example 5 is subjected to appearance visual inspection, infrared analysis, liquid chromatography analysis, oil solubility, copper corrosion and abrasion resistance experiment determination, and the content of diisooctylamine and TTA in the methyl benzotriazole derivative product prepared in example 5 is 1.01 wt% and 1.05 wt%; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b; the water content% (m/m) is 0.08; the oil solubility is good; the potential base number is 145.58 mgKOH/g; the density (20 ℃ C.) was 0.9502g/cm3(ii) a A viscosity (40 ℃) of 81mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.19.
Example 6
A1000 ml four-necked flask equipped with a thermometer and a condenser was charged with 133.15g of methylbenzotriazole, 265.616g of diisooctylamine, and 239.25g of ethanol. Nitrogen gas was introduced into the reaction flask, and after the air in the flask was sufficiently replaced, heating was started. When the temperature reached about 30 ℃, the stirring was started at a rate of 350 rpm. Gradually heating to 45 ℃, keeping the temperature for 0.5h, adding 105.41g of formaldehyde solution into the dripping device, slowly dripping the formaldehyde solution at 45 ℃ to start reaction, reacting for 1.5h at the temperature after dripping is finished, then continuously heating to 70-72 ℃, reacting for 11h under a reflux state, and stopping reaction; cooling the reaction to normal temperature, reducing the vacuum degree to 0.08-0.095 Mpa and steaming to 140 ℃ to obtain light yellow liquid, cooling to normal temperature and carrying out vacuum filtration to obtain filtrate, namely the product. The collected distillate can be used as a recovered solvent for continuous recycling.
According to the invention, the methyl benzotriazole derivative product prepared in example 6 is subjected to appearance visual inspection, infrared analysis, liquid chromatography analysis, oil solubility, copper corrosion and abrasion resistance experiment determination, and the content of diisooctylamine and TTA in the methyl benzotriazole derivative product prepared in example 6 is 1.21 wt% and 1.32 wt%; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b; the water content% (m/m) is 0.08; the oil solubility is good; the potential base number is 147.25 mgKOH/g; the density (20 ℃ C.) was 0.9547g/cm3(ii) a A viscosity (40 ℃) of 87mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.22.
And (3) testing:
the obtained product is prepared into a hydraulic oil formula, and the hydraulic oil mainly comprises the following components: zinc dialkyldithiophosphate, metal detergents, antioxidants, rust inhibitors, metal deactivators, base oils and thickened oils. Wherein the addition amount of the metal deactivator is 0.03%. The additive is added into hydraulic oil according to the proportion to perform hydrolysis stability experiments, rotating oxygen bomb experiments and PDSC tests, and compared with a reference product, the better the performance is, and the better the oxygen resistance, the metal deactivation inhibition and the metal corrosion performance are. The results of the experiment are shown in table 1.
TABLE 1
The reference products 1 and 2 are commercial products of the metal deactivator methylbenzotriazole derivatives which can be obtained in the market, and as can be seen from the table 1, the methylbenzotriazole derivatives prepared according to the technical scheme provided by the invention have the advantages of good oil solubility, good abrasion resistance, strong copper corrosion inhibition performance and great improvement on product performance.
As can be seen from the above examples, the invention does not add any acidic catalyst, uses organic solvent to facilitate the reduced evaporation, and does not introduce a large amount of wastewater. Meanwhile, the product is cooled to normal temperature for suction filtration after reduced evaporation, and the product is purified. Optimizes the synthesis route, and determines the optimal feeding ratio and the optimal feeding sequence of the reaction. The appearance color of the obtained methylbenzotriazole metal deactivator product is light yellow, wherein the content of the diisooctylamine serving as a raw material is 0.75 wt%, and the content of TTA (TTA) is 0.58 wt%; the appearance of the product is light yellow liquid; the corrosion of the copper sheet (150 ℃, 1h) is 1 b; the water content% (m/m) is 0.08; the oil solubility is good; the potential base number is 144.561 mgKOH/g; the density (20 ℃ C.) was 0.9502g/cm3(ii) a A viscosity (40 ℃) of 80mm2And s. The copper powder is put into a hydraulic oil formula for hydrolysis stability test, and the weight loss of copper per unit area is 0.15.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for preparing a metal deactivator, which comprises:
carrying out Mannich reaction on methylbenzotriazole, formaldehyde and diisooctylamine to prepare a methylbenzotriazole metal deactivator; wherein the reaction process is as follows:
2. the preparation method according to claim 1, which specifically comprises:
mixing the methylbenzotriazole and the diisooctylamine in an organic solvent, heating, dissolving and preserving heat;
at a certain temperature, formaldehyde is added into the solution to carry out aminomethylation and electrophilic addition reaction.
3. The method according to claim 1 or 2, wherein the molar ratio of the methylbenzotriazole to the formaldehyde to the diisooctylamine is (1.0-1.5): (0.9-1.2).
4. The method of claim 1 or 2, wherein the mannich reaction is carried out at a reaction temperature of 80 to 120 ℃ for 8 to 20 hours.
5. The method of claim 2, further comprising:
and carrying out reduced pressure distillation on the product of the Mannich reaction to obtain the methylbenzotriazole metal deactivator.
6. The method according to claim 2, wherein the organic solvent is an ethanol solvent.
7. The preparation method according to claim 6, wherein the ratio of the addition amount of the organic solvent to the mass sum of the methylbenzotriazole and the diisooctylamine is 1 (0.6-0.9).
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| CN116715695A (en) * | 2023-06-12 | 2023-09-08 | 威海翔宇环保科技股份有限公司 | A kind of high temperature resistant metal deactivator and preparation method thereof |
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| CN113461626A (en) * | 2021-05-25 | 2021-10-01 | 深圳市广昌达石油添加剂有限公司 | Preparation method of benzotriazole derivative and metal passivator |
| CN116715695A (en) * | 2023-06-12 | 2023-09-08 | 威海翔宇环保科技股份有限公司 | A kind of high temperature resistant metal deactivator and preparation method thereof |
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