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A kind of epoxy dimer fatty acid methyl ester and its preparation method and application

A technology of epoxy dimerized fatty acid methyl ester and dimerized fatty acid methyl ester, which is applied in the direction of organic chemistry, can solve the problems of small molecular weight, poor compatibility, and single performance of plasticizers, and achieve stable product quality and plasticizing efficiency High, good thermal stability

Inactive Publication Date: 2016-09-28
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of preparation method of the epoxy dimer fatty acid methyl ester that is used as PVC plasticizer, aim at the shortcomings such as traditional plasticizer molecular weight is little, compatibility is poor, toxicity is bigger and performance is single, Provided is an epoxy dimer fatty acid methyl ester plasticizer with good heat resistance, good durability, high plasticizing efficiency, non-toxic and environment-friendly, and a preparation method thereof

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  • A kind of epoxy dimer fatty acid methyl ester and its preparation method and application
  • A kind of epoxy dimer fatty acid methyl ester and its preparation method and application
  • A kind of epoxy dimer fatty acid methyl ester and its preparation method and application

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preparation example Construction

[0023] A preparation method of epoxy dimerized fatty acid methyl ester, the steps are:

[0024] Step 1, blend fatty acid methyl ester with catalyst (accounting for 4-10% of the mass of fatty acid methyl ester) and heat to 160-230°C, react for 3-8 hours, the reaction mixture is washed with water and fractionated by vacuum distillation to obtain an intermediate product Dimerized fatty acid methyl ester; step 2, according to dimerized fatty acid methyl ester: peroxygen source carrier: peroxygen source: epoxidation catalyst (n / n / n / w) is 1:(0.5~0.8):(1~ 2): (0.01~0.04) proportional sampling. Mix and stir dimer fatty acid methyl ester, peroxyl group carrier and epoxidation catalyst and heat up to 50-70°C, then add the peroxygen source dropwise at a rate of 15-30ml / h, continue the heat preservation reaction for 2-4h, separate and The epoxidation catalyst is recovered to obtain the crude product of epoxy dimer acid methyl ester, and then the finished product of epoxy dimer acid methy...

Embodiment 1

[0035] Step 1: Add 50g of fatty acid methyl ester and 2g of anhydrous aluminum chloride into a 250mL four-necked flask respectively, pass in nitrogen gas to reduce the occurrence of side reactions in the reaction system, stir and heat to 180°C, react for 5h, and use 50°C for the reaction mixture ℃ mass concentration is 2% sodium carbonate solution washing and filtering to remove the catalyst, and carry out vacuum distillation at 190 ℃, 0.08MPa condition, obtain intermediate product dimerized fatty acid methyl ester;

[0036] Step 2: Weigh 20g of dimerized fatty acid methyl ester, 0.9g of formic acid and 0.4g of p-toluenesulfonic acid, add them into a three-necked flask equipped with a condenser, a stirring rod and a thermometer, stir and raise the temperature to 50°C at a speed of 15ml / h Add 4.3g of hydrogen peroxide (50%) dropwise. After the dropwise addition, the reaction temperature is raised to 65° C. to continue the reaction for 4 h; after the reaction, the crude product i...

Embodiment 2

[0038] Step 1: Add 50g of fatty acid methyl ester and 3g of anhydrous aluminum chloride into a 250mL four-necked flask respectively, pass in nitrogen gas to reduce the occurrence of side reactions in the reaction system, stir and heat to 210°C, react for 4h, and use the reaction mixture for 70 ℃ mass concentration is 2% sodium carbonate solution washing and filtering to remove the catalyst, and carry out vacuum distillation at 190 ℃, 0.08MPa condition, obtain intermediate product dimerized fatty acid methyl ester;

[0039]Step 2: Weigh 20g of dimerized fatty acid methyl ester, 0.95g of formic acid and 0.5g of p-toluenesulfonic acid, add them into a three-necked flask equipped with a condenser tube, a stirring rod and a thermometer, stir and heat up to 50°C, at a speed of 20ml / h Add 4.3g of hydrogen peroxide (50%) dropwise. After the dropwise addition, the reaction temperature is raised to 65° C. to continue the reaction for 3 h; after the reaction, the crude product is left to ...

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Abstract

The invention relates to an epoxy dimeric fatty acid methyl ester, a preparation method and applications thereof, and belongs to the technical field of chemical synthesis. The preparation steps comprise: adopting fatty acid methyl ester as a raw material, carrying out stirring heating in the presence of a catalyst to carry out a dimerization reaction to obtain an intermediate product dimeric fatty acid methyl ester, uniformly mixing the intermediate product, a peroxy source carrier and a catalyst, heating to a certain temperature, adding a peroxy source in a dropwise manner to carry out an epoxidation reaction so as to obtain an epoxy dimer acid methyl ester crude product, and carrying out standing layering, neutralization and dehydration to obtain the epoxy dimeric fatty acid methyl ester finished product. According to the present invention, the preparation method has characteristics of wide raw material source, raw material recycling, no dependence on petroleum, less byproduct during the preparation process, stable product quality, simple and reasonable process, and low energy consumption, and the obtained product has characteristics of no toxicity, environmental protection, heat resistance, good durability, excellent plasticizing performance, and good application prospects.

Description

technical field [0001] The invention relates to the development and preparation technology of a non-toxic and environment-friendly grease-based epoxy plasticizer, in particular to a preparation method of epoxy dimer fatty acid methyl ester used as a PVC plasticizer. Background technique [0002] In recent years, with the rapid development of the engineering plastics industry, the demand for plasticizers has grown at an annual rate of 7-10%, among which petroleum-based phthalate plasticizers occupy the vast majority of the market share. However, this type of plasticizer has persistent reproductive toxicity, and the United States, Japan and many European Union countries have strictly prohibited its use in industries such as electronics, food, daily necessities and toys. my country is a big consumer of plasticizers. The current annual consumption has exceeded 2.5 million tons. Phthalate plasticizers account for about 86% of the total consumption, which poses a potential threat ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/42C07D301/12C07D301/19C08L27/06C08K5/1515
CPCC07D301/12C07D301/19C07D303/42C08K5/1515C08L2201/08C08L27/06
Inventor 陈洁蒋剑春聂小安李科黄金瑞王义刚
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY