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Synthesis process for bisphenol acid type epoxy resin with medium molecular mass

A technology of epoxy resin and molecular weight, applied in the field of synthesis technology of bisphenolic acid type epoxy resin with medium molecular weight, can solve the problems of alkali dosage and usage without specific reports, dark product color, etc.

Inactive Publication Date: 2009-02-18
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Japan Sanyuan Kazuko et al condensed bisphenolic acid and epichlorohydrin in an alkaline medium to make a bisphenolic acid epoxy resin, and further synthesized it into a coating, but there is no specific report on the amount and usage of the alkali
In the 1970s, my country's Jinan Paint Factory improved the Japanese Sanyuan Kazuko process and independently synthesized bisphenolic acid epoxy resin, but only produced epoxy resin with a minimum epoxy value of 0.18, and the product was darker in color

Method used

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  • Synthesis process for bisphenol acid type epoxy resin with medium molecular mass
  • Synthesis process for bisphenol acid type epoxy resin with medium molecular mass

Examples

Experimental program
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Embodiment 1

[0021] In a 500mL three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, add 14.3g of bisphenolic acid and 9.3% of epichlorohydrin, then add 0.1g of phase transfer catalyst tetramethylammonium chloride, heat up to 80°C and keep the temperature To react, dissolve the bisphenolic acid, then lower the temperature to 60° C., slowly add 10 mL of 30% liquid caustic soda NaOH dropwise, and finish the reaction after reflux for 3 hours. Recover the unreacted epichlorohydrin under reduced pressure, add organic solvent benzene to dissolve the crude product, then add water to wash until neutral, stand to separate the water layer, and finally distill to remove benzene, which is the bisphenol with molecular weight in the product of the method of the present invention. Acid type epoxy resin, yield 92.5%.

Embodiment 2

[0023] Add 14.3g of bisphenolic acid and 18.6g of epichlorohydrin to a 500mL three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, then add 0.2g of a phase transfer catalyst tetramethylammonium chloride, and heat up to 70°C Insulate the reaction to dissolve the bisphenolic acid, then lower the temperature to 50° C., slowly add 10 mL of 30% liquid caustic soda NaOH dropwise, and stop the reaction after reflux for 4 hours. Recover the unreacted epichlorohydrin under reduced pressure, add organic solvent benzene to dissolve the crude product, then add water to wash until neutral, stand to separate the water layer, and finally distill to remove benzene, which is the bisphenol with molecular weight in the product of the method of the present invention. Acid type epoxy resin, yield 94.8%.

Embodiment 3

[0025] In a 500mL three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 14.3g of bisphenolic acid and 46.4% of epichlorohydrin, then add 0.2g of a phase transfer catalyst tetramethylammonium chloride, heat up to 70°C and keep the temperature To react, dissolve the bisphenolic acid, then lower the temperature to 60°C, slowly add 30mL of 30% liquid caustic soda NaOH dropwise, and finish the reaction after reflux for 5 hours. Recover the unreacted epichlorohydrin under reduced pressure, add organic solvent benzene to dissolve the crude product, then add water to wash until neutral, stand to separate the water layer, and finally distill to remove benzene, which is the bisphenol with molecular weight in the product of the method of the present invention. Acid type epoxy resin, yield 93.2%.

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Abstract

The invention relates to a synthesis technology of diphenolic acid epoxy resin with moderate molecular weight, comprising the steps of using diphenolic acid and epoxy chloropropane as rawsource materials and condensing and catalyzing with alkaline catalyst to obtain diphenolic acid epoxy resin with moderate molecular weight through catalyzing by basic catalyst in the presence existence of phase transfer catalyst. The mole ratio of diphenolic acid to epoxy chloropropane is 1:2 to 10. The usage of the phase transfer catalyst is 1 to 4 percent of the mole number of diphenolic acid. The mole ratio of the usage of basic catalyst and diphenolic acid is 1:0.2 to 0.6. The reaction temperature is 60 to 80 degrees centigrade DEG C. , and The the reaction time is 2 to 6 hours. The synthesis technology of diphenolic acid epoxy resin with moderate molecular weight is characterized in by simple technique and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis process of a middle molecular mass bisphenolic acid type epoxy resin. Background technique [0002] Medium molecular mass epoxy resins are widely used in coatings, adhesives, laminated materials, electrical casting, electronic packaging and other fields. With the rapid development of the coatings industry and the electronics industry, the performance and synthesis methods of such resins have attracted increasing attention. . Bisphenol A type epoxy resin has the largest output due to the easy availability of raw materials and low cost, accounting for about 90% of the total output of epoxy resin in my country. However, studies have found that low levels of bisphenol A can cause diseases such as increased prostate cancer and breast cancer, reproductive abnormalities, decreased sperm count, precocious females, obesity and diabetes. Therefore, new materials to replace bisphenol A are used to synthesize resins. It is on...

Claims

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Application Information

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IPC IPC(8): C08G59/06
Inventor 李洪亮常春陈俊英方书起马晓建韩秀丽
Owner ZHENGZHOU UNIV
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