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Low-viscosity bisphenol A epoxide resin and production method thereof

A technology of epoxy resin and production method, which is applied in the field of bisphenol A epoxy resin and its production, can solve the problems of unrecorded product specific parameters and insurmountable problems, achieve excellent storage stability, reduce failure maintenance rate, good Effect of molding performance

Inactive Publication Date: 2008-02-06
DALIAN QIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the specific parameters of its products are not described in detail in the present invention, and this method cannot overcome the problems referred to above

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] ①Pre-reaction: bisphenol A, epichlorohydrin and Na 2 CO 3 Mix at a molar ratio of 1:6 to 8:0.12, and react at a temperature of 60 to 65°C for 1 hour;

[0027] ②Reaction: Step ① The reaction product enters the reaction kettle, under the condition of inert gas protection, the absolute pressure is 15 ~ 20kPa under vacuum, and the concentration is 40 ± 0.5% sodium hydroxide solution is added dropwise at 50 ~ 55 ° C, hydrogen The amount of sodium oxide is 1. times (molar ratio) of the amount of bisphenol A in the step 1. During the reaction, keep epichlorohydrin reflux dehydration, and the reaction time is 2h;

[0028] ③Removal of solvent epichlorohydrin: After the reaction in step ② is completed, the epichlorohydrin is recovered by distillation at a temperature of 120°C and a vacuum of 10kPa; the remaining small amount of epichlorohydrin is removed by kettle evaporation , operating pressure 0.2 ~ 0.5Kpa (absolute pressure), operating temperature 120 ~ 130 ℃;

[0029] ④ R...

Embodiment 2

[0033] ①Pre-reaction: bisphenol A, epichlorohydrin and Na 2 CO 3 Mix at a molar ratio of 1:6 to 8:0.12, and react at a temperature of 60 to 65°C for 1 hour;

[0034] ②Reaction: Step ①The reaction product enters the reaction kettle, under the condition of inert gas protection, the absolute pressure is 15~20kPa under vacuum, and the concentration is 55±0.5% sodium hydroxide solution is added dropwise at the temperature of 50~55℃, hydrogen The amount of sodium oxide is 3 times (molar ratio) of the amount of bisphenol A in the step 1. During the reaction, keep epichlorohydrin reflux dehydration, and the reaction time is 2h;

[0035] ③Removal of solvent epichlorohydrin: After the reaction in step ② is completed, the epichlorohydrin is recovered by distillation at a temperature of 120°C and a vacuum of 10kPa; the remaining small amount of epichlorohydrin is removed by kettle evaporation , operating pressure 0.2 ~ 0.5Kpa (absolute pressure), operating temperature 120 ~ 130 ℃;

[0...

Embodiment 3

[0040] ①Pre-reaction: bisphenol A, epichlorohydrin and Na 2 CO 3 Mix at a molar ratio of 1:6 to 8:0.12, and react at a temperature of 60 to 65°C for 1.5 hours;

[0041] ②Reaction: Step ①The reaction product enters the reaction kettle, and under the protection of inert gas, the absolute pressure is 15-20kPa under vacuum, and the sodium hydroxide solution with a concentration of 45±0.5% is added dropwise at a temperature of 50-55°C. The sodium oxide consumption is step 1. 1.7 times (mol ratio) of bisphenol A consumption, keeps epichlorohydrin reflux dehydration during reaction, reaction time 4h;

[0042] ③Removal of solvent epichlorohydrin: After the reaction in step ② is completed, the epichlorohydrin is recovered by distillation at a temperature of 120°C and a vacuum of 10kPa; the remaining small amount of epichlorohydrin is removed by kettle evaporation , operating pressure 0.2 ~ 0.5Kpa (absolute pressure), operating temperature 120 ~ 130 ℃;

[0043] ④ Refining reaction: A...

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Abstract

The present invention discloses a low-viscosity bisphenol-A epoxy resin which has such properties as epoxy equivalent is 180-184g / eq, viscosity is 11,000-12,000cps, hydrolytic chlorine is 150-300ppm, chlorine ion is less than 2ppm, sodium ion is 2ppm, chroma is less than 0.5, and alpha-Morindadiol content is less than 2mmol / 100g resin. The present invention also provides the method of producing the low-viscosity bisphenol-A epoxy resin. The low-viscosity bisphenol-A epoxy resin is featured by narrow distribution of molecular weight, high purity, low viscosity and good chroma; and has good storage stability and good shape-forming processing performance. The production method comprises a pre-reaction step catalyzed by Na2CO3, which effectively increases the conversion rate of BPA from 82 percent to 86.6 percent. Besides; the present invention adopts a kettle-type evaporator and an in-series static thin-film evaporator to remove the solvent in the reaction; thereby reducing the consumption, realizing the reduction of production cost, and improving the quality of products.

Description

technical field [0001] The invention relates to a bisphenol A epoxy resin and a production method thereof. Background technique [0002] Bisphenol A epoxy resin exhibits different forms according to different degrees of polymerization. When the content of bisphenol A diglycidyl ether is extremely high, it exhibits low viscosity characteristics. Due to the low content of hydroxyl groups in its molecule, low content of hydrolyzable chlorine and other impurities, it has excellent storage stability after being mixed with a curing agent, and its heat resistance and electrical insulation are superior to ordinary epoxy resins. Especially suitable for applications in electronics, composite materials, etc. Most of the existing bisphenol A epoxy resin synthesis processes are based on the reaction of bisphenol A, epichlorohydrin (ECH) and sodium hydroxide (NaOH) under certain conditions. [0003] The reaction between bisphenol A and ECH is very complicated. In the basic reaction pro...

Claims

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Application Information

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IPC IPC(8): C08G59/06
Inventor 刘广宇马树君叶玉波梁景奎邱鹏李程郭树志关宏宇李福迟景丰
Owner DALIAN QIHUA CHEM