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Production method of high-purity o-cresol formaldehyde epoxy resin

A novolac epoxy resin and a production method technology, applied in the production field of high-purity o-cresol novolac epoxy resin, can solve the problems of residue, influence on the electrical properties of resin cured products, easy emulsification, etc., and achieve the effect of low epoxy equivalent

Active Publication Date: 2014-11-12
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 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
Chinese patent CN101220135A provides a method for synthesizing o-cresol novolac epoxy resin. This method uses a quaternary salt catalyst, which will remain in the resin. Due to the presence of chlorine and bromine, the electrical properties of the cured resin will be affected.
[0006] At present, there is no report on the recovery of co-solvent in the preparation of o-cresol novolac epoxy resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a four-neck flask equipped with stirring, thermometer, and condenser, add 60g of o-cresol novolac resin, 200g of epichlorohydrin and 60g of ethylene glycol dimethyl ether. At 52°C, add 5g of 30% under the protection of high-purity nitrogen. Sodium bicarbonate solution for pre-reaction, after maintaining for 4 hours, add 30g of 50% sodium bicarbonate solution under vacuum of 0.03MPa to catalyze the ring-closure reaction, recover epichlorohydrin and co-solvent after reaction for 6 hours, then add 200g of toluene to dissolve, at 65℃ , Add 11g45% sodium bicarbonate solution and refine for 3h. After the refining reaction is completed, add pure water to wash until neutral, and remove the solvent to obtain the product.

[0018] The product indicators are as follows: epoxy equivalent: 198.5g / ep, total chlorine: 951ppm, hydrolyzable chlorine: 85ppm, inorganic chlorine: not detected.

Embodiment 2

[0020] In a four-neck flask equipped with stirring, thermometer, and condenser, add 60g of o-cresol novolac resin, 277.5g of epichlorohydrin and 40g of propylene glycol methyl ether. At 58°C, add 1g of 60% bicarbonate under the protection of high-purity nitrogen. Potassium solution is carried out pre-reaction, after 2.5h, under vacuum 0.08MPa, add 30g50% potassium bicarbonate solution catalytic ring closure reaction, reclaim epichlorohydrin and cosolvent after reaction 8h, then add 250g methyl isobutyl ketone to dissolve, in At a temperature of 65°C, add 10g of 20% potassium bicarbonate solution and refine for 5 hours. After the refining reaction is completed, add pure water to wash until neutral, and remove the solvent to obtain the product.

[0021] The product indicators are as follows: epoxy equivalent: 199.7g / ep, total chlorine: 1006ppm, hydrolyzable chlorine: 92ppm, inorganic chlorine: not detected.

Embodiment 3

[0023] In a four-neck flask with stirring, thermometer, and condenser, add 60g of o-cresol novolac resin, 370g of epichlorohydrin and 6g of diethylene glycol dimethyl ether. At 65°C, add 6g of 45 under the protection of high-purity nitrogen. % sodium hydroxide solution for pre-reaction, after 1h, add 30g50% sodium hydroxide solution to catalyze the ring-closing reaction under a vacuum of 0.1MPa, recycle epichlorohydrin and co-solvent after reaction for 3h, then add 300g xylene to dissolve, at a temperature of 65 ℃, adding 4g of 5% sodium hydroxide solution for refining for 3h. After the refining reaction is completed, add pure water to wash until neutral, and remove the solvent to obtain the product.

[0024] The product indicators are as follows: epoxy equivalent: 197.9 g / ep, total chlorine: 974ppm, hydrolyzable chlorine: 69ppm, inorganic chlorine: not detected.

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Abstract

The invention provides a production method of high-purity o-cresol formaldehyde epoxy resin, comprising the following steps of: mixing o-cresol formaldehyde resin and chloropropylene oxide according to the mass ratio of 1:3-1:10, adding a cosolvent, adding an alkaline catalyst under the protection of high-purity nitrogen, pre-reacting for 0.5-5 hours, adding alkali to catalyze a cyclization reaction for 2-8 h at the temperature of 50-120 DEG C and at the degree of vacuum of 0.01-0.1 MPa, recovering chloropropylene oxide and the cosolvent, carrying out refining reaction and post-treatment to obtain the product. The cosolvent used in the invention can be recovered and repeatedly used, thus mainly solving the problem that a quaternary salt catalyst remains in a product by the adoption of a present two-step synthesis technology. Epoxy equivalent of the obtained o-cresol formaldehyde epoxy resin is low, total nitrogen content can reach less than 1200 ppm, the content of hydrolyzable chlorine can reach less than 100 ppm, and there is no catalyst residues. The production method provided by the invention can be applied in the industrial production of the high-purity o-cresol formaldehyde epoxy resin.

Description

technical field [0001] The invention relates to a production method of high-purity o-cresol novolac epoxy resin. Background technique [0002] O-cresol novolac epoxy resin has excellent thermal and chemical stability, excellent moisture resistance, and has become the most widely used matrix resin for epoxy molding compounds. [0003] When the epoxy equivalent of o-cresol novolac epoxy resin is low, the molding compound has high bending strength, good heat resistance and dielectric properties. The side reactions during resin synthesis lead to side reaction products (ie, impurities) in the product. The presence of these impurities will degrade the performance of epoxy molding compounds and affect the reliability of plastic-encapsulated semiconductor devices. The less chlorine ions and sodium ions the epoxy molding compound contains, the smaller the corrosion of the aluminum wiring on the semiconductor device chip will be. The catalyst residue will shorten the storage time of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/08
Inventor 唐光斌张立新潘卫章江玲
Owner CHINA PETROCHEMICAL CORP
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