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Low-viscosity and high-quality liquid bisphenol A type epoxy resin synthesis method

A technology of epoxy resin and synthesis method, which is applied in the field of epoxy resin synthesis, and can solve the problems of high viscosity, high hydrolyzable chlorine content, and low hydrolyzable chlorine content of liquid bisphenol A epoxy resin

Inactive Publication Date: 2016-01-20
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on this, it is necessary to address the problems of high viscosity, high content of hydrolyzable chlorine and low purity in the liquid bisphenol A type epoxy resin synthesized by traditional synthesis methods, and provide a low viscosity, low content of hydrolyzable chlorine and high purity Synthetic method of high low viscosity, high quality liquid bisphenol A type epoxy resin

Method used

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  • Low-viscosity and high-quality liquid bisphenol A type epoxy resin synthesis method

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preparation example Construction

[0025] see figure 1 , the synthetic method of the low viscosity of one embodiment, high-quality liquid bisphenol A type epoxy resin, comprises the following steps:

[0026] Step S110, in a protective gas atmosphere, mix epichlorohydrin, bisphenol A and additives with a mass ratio of 0.81~4.1:1:0.005~0.1, heat to 30°C~80°C, and wait until the bisphenol A is completely After dissolving, add alkali 0.03-0.29 times the amount of bisphenol A substance, and react for 1-5 hours to obtain a reaction solution.

[0027] Wherein, the protective gas is nitrogen, argon, helium or neon.

[0028] Additives are water, ethylene glycol, glycerol, butanone, cyclohexane, cyclohexanone, propylene glycol methyl ether, methyl isobutyl ketone, polyethylene glycol, 18-crown-6 or benzyl trimethyl ammonium chloride.

[0029] The above-mentioned additives are cheap and easy to obtain, can be produced without modifying the production equipment, and are simple and easy to operate.

[0030] Wherein, the...

Embodiment 1

[0052] In a nitrogen atmosphere, mix 228g of epichlorohydrin, 114g of bisphenol A and 3g of glycerol, heat to 50°C, and after the bisphenol A is completely dissolved, add 15g of 20% by mass sodium hydroxide aqueous solution , and reacted for 2 hours to obtain a reaction solution.

[0053] At 55°C, 50kPa, 165g of 20% sodium hydroxide aqueous solution was added dropwise at a constant speed by a peristaltic pump to the above reaction solution, and after 10 hours of reaction, at 200°C, 10kPa, excess epichlorohydrin was removed, to get the mixture.

[0054] Dissolve the above mixture in 200g of toluene, wash with water, separate the liquids, take the organic layer, add 9.5g of 20% sodium hydroxide aqueous solution to the above organic layer at 65°C, react for 2 hours, and then add 1g Cyclohexanone and 23 g of 20% aqueous sodium hydroxide solution were reacted for 4 hours to obtain a reaction mixture.

[0055] At 50°C, the above reaction mixture was washed with water until neutral...

Embodiment 2

[0058] In an argon atmosphere, mix 300g of epichlorohydrin, 114g of bisphenol A and 4g of cyclohexane, heat to 56°C, and after the bisphenol A is completely dissolved, add 9.1g of 35% by mass hydrogen hydroxide Sodium aqueous solution was reacted for 4 hours to obtain a reaction solution.

[0059] At 63°C and 30kPa, 100g of 35% sodium hydroxide aqueous solution was added dropwise through the peristaltic pump at a constant speed in the above reaction solution, and after 7 hours of reaction, at 150°C and 10kPa, excess epichlorohydrin was removed. to get the mixture.

[0060] Dissolve the above mixture in 300g of toluene, wash with water, separate the liquids, take the organic layer, add 9.8g of 35% sodium hydroxide aqueous solution to the above organic layer at 75°C, react for 2 hours, and then add 1g Cyclohexane and 16.5 g of 35% aqueous sodium hydroxide solution were reacted for 4 hours to obtain a reaction mixture.

[0061] At 70°C, the above reaction mixture was washed wit...

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Abstract

The present invention provides a low-viscosity and high-quality liquid bisphenol A type epoxy resin synthesis method, which comprises: in a protection gas atmosphere, mixing epichlorohydrin, bisphenol A and an auxiliary agent, heating to a temperature of 30-80 DEG C, adding an alkali after completely dissolving the bisphenol A, and carrying out a reaction for 1-5 h to obtain a reaction solution; at a temperature of 40-70 DEG C under a pressure of 10-100 kPa, adding an alkali to the reaction solution, carrying out a reaction for 2-10 h, and removing the excess epichlorohydrin to obtain a mixture; dissolving the mixture in a solvent, carrying out water washing, carrying out liquid separation, taking the organic layer, adding an alkali to the organic layer at a temperature of 50-100 DEG C, carrying out a reaction for 0.5-5 h, adding an auxiliary agent and an alkali, and carrying out a reaction for 0.5-5 h to obtain a reaction mixing solution; and carrying out separation purification on the reaction mixing solution to obtain the liquid bisphenol A type epoxy resin. According to the presentinvention, the liquid bisphenol A type epoxy resin prepared through the synthesis method has characteristics of low viscosity, low hydrolyzable chlorine content, and high purity.

Description

technical field [0001] The invention relates to the field of epoxy resin synthesis, in particular to a method for synthesizing low-viscosity, high-quality liquid bisphenol A epoxy resin. Background technique [0002] Liquid bisphenol A type epoxy resin is a low toxicity, colorless or light yellow viscous fluid, which has the advantages of high epoxy value, light color, high purity and low chlorine content. Compared with most resins, liquid bisphenol A type epoxy resin cured product has higher bonding strength and lower shrinkage rate, especially in mechanical strength, electrical insulation and chemical resistance. At present, bisphenol A epoxy resin is one of the most produced and consumed resins, of which liquid bisphenol A epoxy resin accounts for 58%. [0003] Liquid bisphenol A epoxy resin has excellent physical and mechanical properties, electrical insulation properties, chemical resistance and bonding properties, and can be used directly or indirectly as coatings, ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06
Inventor 潘卫章王新龙傅江福周江明江玲肖雄杨鑫
Owner CHINA PETROLEUM & CHEM CORP