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Preparation method for high softening point o-cresol formaldehyde epoxy resin

A technology of phenolic epoxy resin and phenolic resin, which is applied in ink, household utensils, applications, etc., can solve the problems of easy emulsification and high production cost, and achieve the effect of low epoxy equivalent, high softening point, and good electrical insulation performance

Inactive Publication Date: 2012-12-26
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, Japanese Patent JP6153317 provides a method for the etherification of a linear o-cresol novolac resin and epichlorohydrin with an alkali solution in the presence of a solvent and a PTC catalyst to prepare an o-cresol novolac epoxy resin, but in the reaction During the process, the system is easily emulsified under the action of PTC, and the high price of PTC results in high production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Under normal pressure, add 128g of o-cresol and 30g of paraformaldehyde in a four-neck flask equipped with stirring, thermometer, and condenser, raise the temperature to 98°C, add 10g of phosphoric acid, control the reaction temperature at 98°C, and react for 6 hours. Add 200mL of toluene to dissolve, add pure water to wash until neutral, and remove the solvent by steam distillation to obtain a high softening point o-cresol resin product; then add 60g of high softening point o-cresol resin and 370g epichlorohydrin to the belt Add 0.1g of ethylene glycol dimethyl ether to a 1L four-neck flask equipped with a stirring, thermometer, and condenser. Under the protection of high-purity nitrogen, add 1g of 30% sodium bicarbonate solution at 40°C for etherification reaction. After 2 hours, Add 30g of 50% sodium hydroxide solution under a vacuum of 0.03MPa to catalyze the ring-closure reaction, recover epichlorohydrin after 6 hours of reaction, then add 200g of toluene to dissolv...

Embodiment 2

[0025] Under normal pressure, add 118g of o-cresol and 30g of paraformaldehyde in a four-necked flask equipped with stirring, thermometer, and condenser, raise the temperature to 100°C, add 15g of acetic acid, control the reaction temperature at 100°C, and react for 10 hours, Add 200mL of xylene to dissolve, add pure water to wash until neutral, and remove the solvent by steam distillation to obtain a high softening point o-cresol resin product; then add 60g of high softening point o-cresol resin and 280g epichlorohydrin to the Add 0.2g of isopropanol to a 1L four-neck flask equipped with a stirring, thermometer, and condenser. Under the protection of high-purity nitrogen, add 2g of 30% sodium bicarbonate solution at 80°C for etherification reaction. Add 40g of 45% sodium hydroxide solution at 0.03MPa to catalyze the ring-closing reaction, recover epichlorohydrin after 4 hours of reaction, then add 200g of xylene to dissolve it, and add 2g of 20% potassium hydroxide solution to...

Embodiment 3

[0028] Under normal pressure, add 122g of o-cresol and 30g of paraformaldehyde in a four-neck flask equipped with stirring, thermometer, and condenser, raise the temperature to 110°C, add 5g of hydrochloric acid, control the reaction temperature at 110°C, and react for 4 hours. Add 200mL of xylene to dissolve, add pure water to wash until neutral, and remove the solvent by steam distillation to obtain a high softening point o-cresol resin product; then add 60g of high softening point o-cresol resin and 300g epichlorohydrin to the Add 0.05g of 1,4-dioxane to a 1L four-neck flask equipped with stirring, thermometer, and condenser. Under the protection of high-purity nitrogen, add 1g of 30% sodium bicarbonate solution at 55°C for etherification reaction. After 2 hours, 50g of 30% potassium hydroxide solution was added under a vacuum of 0.03MPa to catalyze the ring-closure reaction. After 5 hours of reaction, epichlorohydrin was recovered, and then 200g of cyclohexanone was added t...

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Abstract

The present invention provides a preparation method for a high softening point o-cresol formaldehyde epoxy resin. The preparation method comprises the following steps: adopting o-cresol and paraformaldehyde as raw materials, carrying out a reaction for 3-5 hours under a catalysis effect of a catalyst, and carrying out a post-treatment to obtain a high softening point o-cresol formaldehyde resin; mixing the synthesized linear high softening point o-cresol formaldehyde resin and epichlorohydrin according to a mass ratio of 1:3-1:10; adding an auxiliary agent; carrying out an etherification reaction at a temperature of 30-100 DEG C; adding an alkali to catalyze a ring closing reaction under a vacuum degree of 0.01-0.1 MPa; recovering the epichlorohydrin; and carrying out a refinement reaction and a post-treatment. The o-cresol formaldehyde epoxy resin prepared by adopting the preparation method of the present invention has the following characteristics that: high softening point of 80-95 DEG C can be achieved; epoxy equivalent is low; hydrolyzable chlorine content is low; and a high yield can be achieved. In addition, the o-cresol formaldehyde epoxy resin of the present invention is a special function type epoxy resin focused for green electronics encapsulation, IC packaging and circuit board (green oil), wherein the o-cresol formaldehyde epoxy resin has characteristics of high heat resistance, low moisture absorption, and low thermal expansion coefficient.

Description

technical field [0001] The invention relates to a preparation method of o-cresol novolac epoxy resin with high softening point. Background technique [0002] O-cresol novolac epoxy resin with high softening point is a special functional epoxy resin with high heat resistance, low moisture absorption and low thermal expansion coefficient, which is mainly used in green electronic packaging, IC packaging and circuit board (green oil). It is different from low-viscosity o-cresol novolac epoxy resin, because of its large molecular weight, long chain is easy to curl, and the steric hindrance effect of the ortho-methyl group increases, which makes it difficult to graft epoxy groups to phenolic hydroxyl groups. Equivalent increases accordingly. The present invention strives to increase the softening point of EOCN while maintaining a low epoxy equivalent and hydrolyzable chlorine. [0003] In the prior art, Japanese Patent JP6153317 provides a method for the etherification of a line...

Claims

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Application Information

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IPC IPC(8): C08G59/08C08G8/12C09D11/10C09D11/102
Inventor 张晖唐光斌任六波江玲袁健
Owner CHINA PETROCHEMICAL CORP
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