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Cycloaliphatic epoxy resin and preparation method thereof

An epoxy resin, cycloaliphatic technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult solvent recovery and reuse, complex system, etc.

Inactive Publication Date: 2010-03-17
AMICOGEN CHINA BIOPHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production of this cycloaliphatic epoxy resin uses peroxyacetic acid as an oxidizing agent, and there is a greater danger in the production process; -The study of methylene esters has always been the focus of research and attention of experts in this field
[0003] From the current worldwide research situation, the main production route of cycloaliphatic epoxy resin is to use bicycloalkenyl ester {α-(4' cyclohexenyl) 4' cyclohexene carboxylate methyl ester} as raw material, (1) produce oxygen cyclohexane-4-carboxylic acid, epoxy cyclohexane-4-methylene ester under the condition that peroxyacetic acid is made oxidant; Example is as the patent DE3723843 of Germany; (2) with the metal nickel Organic salt is used as catalyst, and oxygen is used as oxidizing agent, as Japanese patent JP05032647; (3) with propionic acid, 50% hydrogen peroxide and concentrated sulfuric acid are used as oxidizing agent in the mixed solvent of benzene, carry out epoxidation, such as German patent DE 3528002; The oxidants used in these designed cycloaliphatic oxygen resins all have different disadvantages, such as peracetic acid and oxygen are more dangerous, and the mixed solvent system of propionic acid, 50% hydrogen peroxide and concentrated sulfuric acid in benzene is very complicated, and it is not easy to recover the solvent. wait again

Method used

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  • Cycloaliphatic epoxy resin and preparation method thereof
  • Cycloaliphatic epoxy resin and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: a kind of preparation method of cycloaliphatic epoxy resin, the steps are as follows:

[0022] (1) Preparation of oxidant solution containing catalyst

[0023] Weigh 46.0 g of hydrogen peroxide (35%), 30.0 g of chloroform, and 2.2 g of catalyst heteropolyacid; add them to a 250 ml single-necked flask, install the stirrer, and adjust the pH value to 2.4- 3.0 range; stir for 90 minutes to mix the solution into a uniform milky solution; pour it into the dropping funnel for use.

[0024] (2) Weigh 44g of bicycloalkenyl ester and 80g of chloroform respectively, add them into a 500ml four-neck flask, install a stirrer, a thermometer, a dropping funnel, and a water separation condensing device. Stir, and when the temperature rises to 60-65°C, reflux occurs; start dropping the oxidant solution in the dropping funnel, maintain the system temperature at about 60-65°C, and complete the dropwise addition in 60-90 minutes; continue to react for 60 minutes. After stan...

Embodiment 2

[0028] Weigh 54.0 g of hydrogen peroxide (30% content) and 30.0 g of toluene, and 2.2 g of catalyst heteropolyacid respectively; 2 CH 2 PO 3 h 2 , adjust the pH value to the range of 2.0-2.7; stir for 120 minutes, mix the solution into a uniform milky solution; weigh 44g of bicycloalkenyl ester and 80g of toluene respectively, add them to a 500ml four-necked flask, install the stirrer, thermometer, Dropping funnel and water separator condenser. Stir and heat up to 70-80°C; start dropping the oxidant solution in the dropping funnel, maintain the system temperature at about 70-80°C, and complete the dropwise addition in 60-90 minutes; continue to react for 60 minutes. After standing still for 30 minutes, the lower organic phase was separated, and the upper aqueous layer was discarded.

[0029] The separated organic phase solution was added to a 250ml four-neck flask, and a stirrer, a thermometer, and a water condensing device were installed. Heating in an oil bath, the temp...

Embodiment 3

[0032] Take by weighing 80.0 g hydrogen peroxide (content is 15%) and 30.0g1,2 dichloroethanes, 2.5g catalyst heteropolyacid (composite heteropolyacid catalyst synthesized by 1mol tungstic acid and 9 molybdic acid); join in the single-necked flask, Install the stirrer, adjust the pH value to 2.4-3.0 with 0.5g-1.0 sodium hydrogen phosphate; stir for 60-90 minutes, and mix the solution into a uniform milky solution; weigh 44g of bicycloalkenyl ester, 1,2- Dichloroethane 80g, join in the 500ml four-necked flask, install stirrer, thermometer, dropping funnel and water separation condensing device. Stir and heat up to 60-70°C; start dropping the oxidant solution in the dropping funnel, maintain the system temperature at about 60-70°C, and complete the dropwise addition in 60-90 minutes; continue the reaction for 120 minutes. After standing still for 30 minutes, the lower organic phase was separated, and the upper aqueous layer was discarded.

[0033] The separated organic phase so...

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Abstract

The invention relates to cycloaliphatic epoxy resin and a preparation method thereof. The method comprises the following steps of: taking dicycloacrylate as a raw material, hydrogen peroxide solutionas an oxidizing agent and halocarbon or halogenated hydrocarbon as a catalyst and synthesizing the cycloaliphatic epoxy resin under the action of a heteropolyacid catalyst, wherein the main reaction product of the cycloaliphatic epoxy resin, namely epoxy cyclohexane-4-carboxylic epoxycyclohexane-4-methylene ester accounts for over 90 weight percent and the epoxy equivalent weight is between 120 and 140. Each quality index of the cycloaliphatic epoxy resin of the invention is the same as that of the cycloaliphatic epoxy resin prepared by using a peroxyacetic acid as the oxidizing agent. The cycloaliphatic epoxy resin of the invention can be used as an automobile paint, a metal surface paint and an insulative substrate resin in the field of electronic and electric appliances.

Description

technical field [0001] The invention relates to a cycloaliphatic epoxy resin and a preparation method thereof, belonging to the technical field of epoxy resins. Background technique [0002] Cycloaliphatic epoxy resin (the main component is epoxycyclohexane-4-carboxylic acid epoxycyclohexane-4-methylene ester) has good insulation, heat resistance, chemical corrosion resistance, mechanical performance, low volume shrinkage after curing and good adhesion to a variety of substrates. Therefore, as a resin with excellent comprehensive performance, it is widely used in the fields of automotive paint, metal surface paint, and electronic appliances. However, the production of this cycloaliphatic epoxy resin uses peroxyacetic acid as an oxidizing agent, and there is a greater danger in the production process; The study of -methylene esters has always been the focus of research and attention of experts in this field. [0003] From the current worldwide research situation, the main ...

Claims

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Application Information

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IPC IPC(8): C07D303/12C07D301/12C08G59/24
Inventor 张玉民庄儒田甄风雷
Owner AMICOGEN CHINA BIOPHARM CO LTD
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