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Method for preparing (methyl)acrylic acid-3,4-epoxycyclohexyl methyl ester by microchannel reactor

A technology of microchannel reactor and cyclohexenyl methyl ester, which is applied in the direction of organic chemistry, can solve the problems of continuous production difficulty, low product yield, high raw material cost, etc., and achieve the improvement of conversion rate and product selectivity, The effect of high product purity and the improvement of production economic benefits

Active Publication Date: 2018-07-20
JIANGSU TETRA NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a method for preparing 3,4-epoxycyclohexylmethyl (meth)acrylate with a microchannel reactor, which has the advantages of cheap and easy-to-obtain raw materials, simple operation process, high product purity and yield, and The characteristics of continuous production overcome the disadvantages of high raw material cost, many by-products, low product yield and difficulty in continuous production in the traditional process.

Method used

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  • Method for preparing (methyl)acrylic acid-3,4-epoxycyclohexyl methyl ester by microchannel reactor
  • Method for preparing (methyl)acrylic acid-3,4-epoxycyclohexyl methyl ester by microchannel reactor
  • Method for preparing (methyl)acrylic acid-3,4-epoxycyclohexyl methyl ester by microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Esterification reaction: 58.8g of 3-cyclohexene-1-methanol, 0.05g of polymerization inhibitor p-hydroxyanisole, 50.6g of triethylamine and 300g of chloroform were sequentially added into a three-necked flask and stirred evenly to obtain solution 1. Solution 1 and 52.3g of methacryloyl chloride were pumped into the first mixer at a flow rate of 6.8mL / min: 1mL / min and mixed evenly, then entered the first microchannel reactor, and reacted for 22 minute. After the reaction is over, filter the salts generated by the reaction to obtain the intermediate methacrylate-3-cyclohexenyl methyl ester solution (solution two); this step solution can be directly used in the epoxidation reaction without vacuum distillation , simplifying the operation steps.

[0050] Epoxidation reaction: 10.7g of anhydrous sodium acetate was dissolved in 71.5g of 50% hydrogen peroxide (w / W) aqueous solution to obtain solution three; solution three and 75g of acetic anhydride were mixed at a flow rate of...

Embodiment 2

[0052] Esterification reaction: Add 58.8g of 3-cyclohexene-1-methanol, 0.05g of polymerization inhibitor p-hydroxyanisole, 50.6g of triethylamine and 300g of chloroform into a three-necked flask and stir evenly to obtain solution 1. Solution 1 and 45.2g of acryloyl chloride were pumped into the first mixer at a flow rate of 6.8mL / min: 1mL / min. After mixing, they entered the first microchannel reactor and reacted for 25 minutes at a temperature of 10°C. After the reaction, use a Buchner funnel to filter out the salt in the reaction solution to obtain a solution containing the intermediate 3-cyclohexenylmethyl acrylate (solution 2).

[0053] Epoxidation: 10.5g of anhydrous sodium acetate was dissolved in 72g of 50% hydrogen peroxide (w / w) aqueous solution to obtain solution three; solution three and 75g of acetic anhydride were respectively mixed at a flow rate of 1mL / min: 1mL / min After being pumped into the second mixer and mixed evenly, solution 4 was obtained; 367.5 g of solu...

Embodiment 3

[0056] The implementation conditions and steps are the same as in Example 1, except that the triethylamine in the esterification reaction is changed to 32% aqueous sodium hydroxide solution, the purity of methacrylic acid-3,4-epoxycyclohexylmethyl ester is 98.8%, and the molar yield 98.7%, 3-cyclohexenyl methyl methacrylate conversion rate 99.0%, product selectivity 99.7%.

[0057] The resulting product spectrogram is consistent with Example 1, so it is not provided repeatedly.

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Abstract

The invention discloses a method for preparing (methyl) acrylic acid-3,4-epoxycyclohexyl methyl ester by a microchannel reactor. The method is characterized in that firstly, 3-cyclohexene-1-methanol and (methyl)acryloyl chloride are used as raw materials; esterification reaction is performed in the microchannel reactor to prepare an intermediate of (methyl)acrylic acid-3-cyclohexenyl methyl ester;then, peroxyacetic acid is used as an oxidizing agent; chlorohydrocarbon is used as a reaction medium; selective epoxidation reaction is performed in the microchannel reactor to prepare a target product. The esterification reaction temperature is low; the side reactions are few; the efficiency is high; the aftertreatment is simple; an in-situ method is used; peroxyacetic acid is prepared; meanwhile, olefin epoxidation reaction is performed; the technological process is easy to operate; the reaction yield is high; the product purity is high; the operation of the product separation process is simple; the method is suitable for continuous production; when a curing resin composition prepared by the product is used, a good cured matter with high sealing performance and chemical resistant performance on a base material can be obtained, and can be suitable for being used in the field of electronic materials.

Description

technical field [0001] The invention relates to a method for preparing 3,4-epoxycyclohexylmethyl (meth)acrylate by using a microchannel reactor, and belongs to the field of preparation of acrylic epoxy resin. Background technique [0002] (Meth)acrylate-3,4-epoxycyclohexyl methyl ester is a new type of organic polyfunctional epoxy monomer, which is used in the synthesis of pesticides, pharmaceutical intermediates, plasticizers, adhesives, coating resins, etc. It is the main raw material of chemical substances and has been widely used in the field of chemical industry. In recent years, with the development of the printing industry and coating industry in various countries in the world, especially the development of adhesives and the enhancement of people's environmental protection awareness, it provides a good source for the development and application of functional (meth)acrylate-3,4-epoxycyclohexylmethyl ester a wide range of markets. [0003] Traditionally, it is prepare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/16C07D301/16
CPCC07D301/16C07D303/16
Inventor 韩建伟贾泉吴宏亮马培培
Owner JIANGSU TETRA NEW MATERIAL TECH
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