Method for synthetizing hydrogenated bisphenol A epoxy resin under catalysis of ammonium salt

A technology for hydrogenating bisphenol and epoxy resin, applied in the field of epoxy resin preparation, can solve problems such as inability to control product color well, and achieve the effects of easy industrial production and simple process flow

Inactive Publication Date: 2013-09-04
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are literature reports using unpublished self-made quaternary ammonium salt as a catalyst to synthesize hydrogenated bisphenol A e

Method used

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  • Method for synthetizing hydrogenated bisphenol A epoxy resin under catalysis of ammonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0041] In a 1000ml four-neck flask equipped with an electric heating pack heating device, a stirrer, a condenser, a thermometer, and a dropping funnel, use dry air to purge the entire system, add 100g of hydrogenated bisphenol A and 50g of solvent toluene, and start stirring , heated to 30°C with an electric heating pack, and added 0.32g of ammonium acetate and 16.7g of sodium hydroxide. Add 115g of epichlorohydrin dropwise through the dropping funnel to carry out etherification reaction, fully react for 15 hours, and the reaction temperature is 30°C. During the dropping process, observe the temperature and color changes of the system, adjust the dropping speed, and control the dropping time to 2-5 hours. Then 11.2 g of 30% sodium hydroxide aqueous solution was added dropwise through the dropping funnel, the reaction time was 2 h, and the reaction temperature was 100°C. In order to reduce the viscosity of the system, add 200g of toluene after the reaction reaches the process ...

Embodiment 2

[0049] In a 1000ml four-necked flask equipped with an electric heating pack heating device, a stirrer, a condenser, a thermometer, and a dropping funnel, use dry air to purge the entire system, add 100g of hydrogenated bisphenol A and 80g of solvent xylene, and start Stir, heat the electric heating pack to 100°C, add 2.3g of phenyltrimethylammonium formate, and 30g of sodium ethoxide. Add 150 g of methyl epichlorohydrin dropwise through the dropping funnel to carry out etherification reaction, fully react for 2 hours, and the reaction temperature is 100°C. During the dropping process, observe the temperature and color changes of the system, adjust the dropping speed, and control the dropping time to 2-5 hours. Then, 140 g of calcium hydroxide aqueous solution with a mass fraction of 11% was added dropwise through the dropping funnel, the reaction time was 8 hours, and the reaction temperature was 100°C. In order to reduce the viscosity of the system, add 400g of xylene after ...

Embodiment 3

[0057] In a 1000ml four-neck flask equipped with an electric heating pack heating device, a stirrer, a condenser tube, a thermometer, and a dropping funnel, use dry air to purge the entire system, add 100g of hydrogenated bisphenol A and 60g of solvent methyl isobutyl Base ketone, start stirring, heat the electric heating pack to 70°C, add 2.5g octadecyltrimethylammonium bromide, and 25g sodium methoxide. Add 120 g of epibromohydrin dropwise through the dropping funnel to carry out etherification reaction, fully react for 8 hours, and the reaction temperature is 60°C. During the dropping process, observe the temperature and color changes of the system, adjust the dropping speed, and control the dropping time to 2-5 hours. Then 20 g of 15% sodium ethoxide ethanol solution was added dropwise through the dropping funnel, the reaction time was 4 hours, and the reaction temperature was 70°C. In order to reduce the viscosity of the system, add 208g of methyl isobutyl ketone after t...

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Abstract

The invention discloses a method for synthetizing a hydrogenated bisphenol A epoxy resin under the catalysis of ammonium salt. According to the method, epihalohydrin such as hydrogenated bisphenol A, epichlorohydrin and the like are taken as raw materials, simultaneously, an ammonium salt catalyst and alkali are added, a ring-opening etherification reaction is performed at the temperature of 30 DEG C-100DEG C, and halogen alcohol ether is obtained; then, the alkali is continuously added in the same reaction system, and a ring-closing epoxidation reaction is performed at the temperature of 20 DEG C-80 DEG C; and the hydrogenated bisphenol A epoxy resin is obtained through posttreatment processes such as filtering, washing, separation, reduced pressure distillation and the like. A product is measured to be superior to number one with a GB-T12007.1-1989 epoxy resin color measuring method-Gardner colorimetric method.

Description

technical field [0001] The invention relates to the technical field of epoxy resin preparation. Background technique [0002] Hydrogenated bisphenol A epoxy resin not only has the performance of bisphenol A epoxy resin, but also overcomes the defect that unsaturated double bonds are easy to break because the benzene ring is transformed into a saturated six-membered ring without double bonds. With proper curing agent selected, the prepared epoxy resin material has the characteristics of good weather resistance and high dielectric strength, and can be used in outdoor electric power and other industries. Hydrogenated bisphenol A epoxy resin instead of bisphenol A epoxy resin is used in daily production and life, which can also reduce the damage to people's health. With the development of LED lighting technology in recent years, the outer packaging material requires epoxy resin with good color and high transparency in the visible light region. [0003] At present, Zhongwu Chen...

Claims

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Application Information

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IPC IPC(8): C08G59/06C08G59/68
Inventor 周东山薛奇单美娟王晓亮朱青陈葳江伟车波
Owner NANJING UNIV
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