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O-cresol formaldehyde epoxy resin, preparation method and application thereof

A technology of phenolic epoxy resin and phenolic resin, which is applied in the direction of electrical components, electrical solid devices, circuits, etc., can solve the problem of high content of non-hydrolyzable chlorine and achieve the effect of low content of non-hydrolyzable chlorine

Active Publication Date: 2019-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the technical problem of high non-hydrolyzable chlorine content in the product of the existing o-cresol novolac epoxy resin preparation method, the invention provides a preparation method that can reduce the non-hydrolyzable chlorine content of the o-cresol novolac epoxy resin product

Method used

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  • O-cresol formaldehyde epoxy resin, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0091] Add 323g of epichlorohydrin to a 1L four-neck flask with a stirring, thermometer, and reflux condenser, then add 75g of o-cresol novolac resin, protect it with industrial nitrogen, heat up to 60°C, and add 5.6g of 30% sodium hydroxide solution ether cyclization reaction for 2 hours; at 30kPa, mix 42.5g of 50% sodium hydroxide solution with 0.2g of 15-crown-5, slowly add to the reaction system at 62°C, cyclization reaction for 4 hours; filter to remove salt; at pressure less than 20kPa, 150°C Add 320g of methyl isobutyl ketone to dissolve; add 15g of 15% sodium hydroxide solution at 85°C for refining for 1 hour; wash with water (50-100°C) until the pH is 7, and then set at 5kPa, Solvent removal at 150°C to obtain o-cresol novolac epoxy resin product.

[0092] The obtained product index is as follows: epoxy equivalent: 202.6g / eq, hydrolyzable chlorine 65ppm, total chlorine 623ppm, inorganic chlorine 1ppm. Non-hydrolyzable chlorine content = 623-65-1 = 557ppm.

Embodiment 2

[0094] Add 323g of epichlorohydrin to a 1L four-neck flask with a stirring, thermometer, and reflux condenser, then add 75g of o-cresol novolac resin, protect it with industrial nitrogen, heat up to 60°C, and add 7.84g of 30% potassium hydroxide solution ether cyclization reaction for 2 hours; at 30kPa, take 59.5g of 50% potassium hydroxide solution and 0.3g of 18-crown-6 and mix evenly, slowly add to the reaction system at 62°C, cyclization reaction for 4 hours; filter to remove salt; desalt at 20kPa, 150°C Remove epoxy ECH; add 320g of methyl isobutyl ketone to dissolve; add 21g of 15% potassium hydroxide solution at 85°C for refining for 1 hour; wash with water (50-100°C) until the pH is 7, then place it at 5kPa, 150°C The following solvent removal obtains the o-cresol novolac epoxy resin product.

[0095] The obtained product index is as follows: epoxy equivalent: 200.4g / eq, hydrolyzable chlorine 76ppm, total chlorine 566ppm, inorganic chlorine 1ppm. Non-hydrolyzable chlo...

Embodiment 3

[0096] Embodiment 3 (pre-reaction alkali concentration improves, and the reaction time reduces)

[0097]Add 349g of epichlorohydrin to a 1L four-neck flask with a stirring, thermometer, and reflux condenser, then add 75g of o-cresol novolac resin, protect it with industrial nitrogen, heat up to 60°C, and add 2.16g of 50% sodium hydroxide solution ether cyclization reaction for 2 hours; at 30kPa, take 42.5g of 50% sodium hydroxide solution and mix evenly with 0.2g of 15-crown-5, slowly add to the reaction system at 60°C, cyclization reaction for 1.5 hours; filter to remove salt; Add 350g of methyl isobutyl ketone to dissolve; add 15g of 15% sodium hydroxide solution at 85°C for refining for 1 hour; wash with water (50-100°C) until the pH is 7, then in 5kPa, Solvent removal at 150°C to obtain o-cresol novolac epoxy resin product.

[0098] The obtained product index is as follows: epoxy equivalent: 205.8g / eq, hydrolyzable chlorine 55ppm, total chlorine 589ppm, inorganic chlorine...

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Abstract

The invention discloses a preparation method of an o-cresol formaldehyde epoxy resin. The preparation method is characterized by comprising the steps of pre-reacting an o-cresol-formaldehyde resin, epichlorohydrin and an alkali A to obtain a pre-reaction liquid; mixing a crown ether and an alkali B to obtain a mixed liquid; then adding the mixed liquid to the pre-reaction liquid to carry out a catalytic ring-closing reaction; after the ring-closing reaction is completed, removing the epichlorohydrin first, then performing a refining reaction, washing, and removing a solvent to obtain the product. The o-cresol formaldehyde epoxy resin synthesized by the method is low in non-hydrolyzable chlorine content and meets the requirement of high-end products of the electronic molding compound industry for the o-cresol formaldehyde epoxy resin.

Description

technical field [0001] The invention relates to a preparation method of o-cresol novolac epoxy resin, which belongs to the technical field of epoxy resin synthesis. Background technique [0002] O-cresol novolac epoxy resin has the characteristics of excellent thermal stability, mechanical strength, electrical insulation performance, water resistance, chemical resistance and high glass transition temperature. It is mainly used in laminated products, civilian weak current products, packaging of electronic components in semiconductor integrated circuits and large-scale integrated circuits (electronic molding compound), synthesis of circuit board ink photosensitive resin, etc. As one of the raw materials, epichlorohydrin can not only undergo etherification and epoxidation reactions with o-cresol aldehyde resins, but also undergo hydrolysis reactions by itself under the action of alkali. The epoxidation ring-closing reaction of epoxy resin is a reversible reaction, and the form...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/08H01L23/29
Inventor 肖雄任六波周江明杨鑫
Owner CHINA PETROLEUM & CHEM CORP
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