Method for synthesizing ultra-pure o-cresol formaldehyde epoxy resin

A novolak epoxy resin and a synthesis method technology, which is applied in the synthesis field of o-cresol novolac epoxy resin, can solve the problems that do not meet the ultra-high purity requirements of the resin, achieve low chlorine content, high purity, and avoid chlorine-based residues Effect

Inactive Publication Date: 2016-12-14
JIANGSU SANJILI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the main method of preparing o-cresol novolac epoxy resin is the first condensation and then epoxidation process. In this process, due to the use of hydrochloric acid as a catalyst, especially the polymerization of the raw material epichlorohydrin itself, the content of chloride ions, especially hydrolyzable chlorine, in the product Higher, as Chinese patent CN101220135A provides a kind of synthetic method of o-cresol novolac epoxy resin, the hydrolyzable chlorine of the o-cresol novolac epoxy resin synthesized by this method is 400~600ppm, does not meet the requirement of resin ultra-high purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under normal pressure, 108.0g of o-cresol and 382.5g of allyl chloride were added to the reactor, nitrogen gas was introduced, after stirring evenly, 80g of 50% sodium hydroxide aqueous solution was added, and the reaction was carried out at 60°C, wherein The molar ratio of o-cresol: allyl chloride: sodium hydroxide=1:5:1, allyl chloride is recovered under reduced pressure after the reaction, washed with water to neutrality, and enol ether monomer is obtained; the obtained enol ether Mix the monomer with 63.8g of 40% formaldehyde aqueous solution, add 1.5g of concentrated hydrochloric acid, heat up the reaction, the temperature is 90°C, and the molar ratio of enol ether monomer: formaldehyde: hydrochloric acid = 1: 0.85: 0.015, add 300g after the reaction Methyl isobutyl ketone is dissolved and separated, and the oil layer is washed to neutrality to obtain a solution of o-cresol aldehyde allyl ether resin; add 16.4g of sodium acetate to the above solution, and then raise...

Embodiment 2

[0022] Under normal pressure, 108.0g of o-cresol and 612.0g of allyl chloride were added to the reactor, nitrogen gas was introduced, after stirring evenly, 120g of 50% sodium hydroxide aqueous solution was added, and the reaction was carried out at 90°C, wherein The molar ratio of o-cresol: allyl chloride: sodium hydroxide=1:8:1.5, allyl chloride is recovered under reduced pressure after the reaction is completed, washed with water until neutral, and enol ether monomer is obtained; the obtained enol ether Mix the monomer with 37.5g of 40% formaldehyde aqueous solution, add 3.0g of concentrated hydrochloric acid, heat up the reaction, the temperature is 90°C, in which the molar ratio of enol ether monomer: formaldehyde: hydrochloric acid = 1:0.5:0.03, add 300g after the reaction Toluene was dissolved and separated, and the oil layer was washed to neutrality to obtain a solution of o-cresol aldehyde allyl ether resin; 8.2g of sodium acetate was added to the above solution, and t...

Embodiment 3

[0024] Under normal pressure, 108.0g of o-cresol and 765.0g of allyl chloride were added to the reactor, nitrogen gas was passed into it, after stirring evenly, 44.5g of 45% sodium hydroxide aqueous solution was added, and the reaction was carried out at 60°C. Among them, the molar ratio of o-cresol: allyl chloride: sodium hydroxide=1:10:0.5, allyl chloride is recovered under reduced pressure after the reaction is completed, washed with water to neutrality, and enol ether monomer is obtained; the obtained enol Mix the ether monomer and 90g of 40% formaldehyde aqueous solution, add 0.9g of oxalic acid, heat up the reaction, the temperature is 90°C, the molar ratio of enol ether monomer: formaldehyde: oxalic acid = 1:1.2:0.01, add 300g of chloroform after the reaction Dissolve and separate layers, wash the oil layer with water to neutrality, and obtain a solution of o-cresol aldehyde allyl ether resin; add 4.1 g of sodium acetate to the above solution, then raise the temperature ...

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Abstract

The invention discloses a method for synthesizing an ultra-pure o-cresol formaldehyde epoxy resin. The method comprises the following steps: preparing an enol ether monomer by taking o-cresol and allyl chloride as raw materials; adding formaldehyde and acid catalysts for reaction to obtain a solution of o-cresol formaldehyde allyl ether resins; finally, oxidizing by using peroxyacetic acid to obtain the o-cresol formaldehyde epoxy resin. According to the invention, a process of synthesizing the o-cresol formaldehyde epoxy resin is optimized, the product purity is high, the content of hydrolyzable chlorides is low, and the method has the obvious advantages that residual chlorine groups are avoided in the synthetic process, chlorine exists in an inorganic chlorine form, and the content of the hydrolyzable chlorides in the o-cresol formaldehyde epoxy resin is greatly reduced and is generally 20ppm or lower.

Description

technical field [0001] The invention relates to a method for synthesizing a polymer compound, in particular to a method for synthesizing a high-purity and low-chlorine content o-cresol novolac epoxy resin. Background technique [0002] O-cresol novolac epoxy resin is a polyfunctional glycidyl ether type epoxy resin developed in the 1970s to adapt to the rapid development of the semiconductor industry and electronics industry. The epoxy value of o-cresol novolac epoxy resin is as high as 0.5 eq / 100g Above, the resin can provide 2.5 times more cross-linking points when curing, and it is easy to form a three-dimensional structure with high cross-linking density. In addition, the cured product is rich in phenolic skeleton, showing excellent thermal stability, mechanical strength, electrical insulation performance, and water resistance. , Higher glass transition temperature of chemical resistance. Electronic components encapsulated with high-purity resin can maintain their good ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G16/04C08G16/02
CPCC08G16/04C08G16/0225
Inventor 杨世刚江保卫刘德标王恒启徐廷芒
Owner JIANGSU SANJILI CHEM
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