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Method for purifying bisphenol A diglycidyl ether

A technology of diglycidyl ether and purification method, which is applied in the direction of organic chemistry, can solve the problems of difficult recycling of mixed solvents, large temperature influence, and low selection efficiency, and achieve excellent selection effect, good selectivity, and good selectivity Effect

Active Publication Date: 2014-07-16
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, methods for preparing high-purity and low-viscosity epoxy resins (referring to bisphenol A epoxy resins with a mass percentage of bisphenol A diglycidyl ether in bisphenol A epoxy resins ≥ 90%) exist. Many deficiencies: the research methods reported in the literature include: (1) solvent extraction method: generally, mixed solvents are not easy to recycle and are greatly affected by temperature, and the selection efficiency is low; (2) recrystallization method: there is a shortage of low temperature required for a long crystallization process; (3) Short-path distillation technology: Although the industrial production of purified bisphenol A diglycidyl ether has been realized, due to the need for high temperature of about 200 ° C and high vacuum (close to the pressure of 0 to 10 -5 Pa), equipment investment is high

Method used

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  • Method for purifying bisphenol A diglycidyl ether
  • Method for purifying bisphenol A diglycidyl ether
  • Method for purifying bisphenol A diglycidyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Step 1: Add 3000g of epoxy resin (epoxy value 0.54) and 450g of ethylene glycol to the 30L reaction kettle ① in turn, raise the temperature of the material to 80°C under stirring, keep it warm for 60 minutes, and then add 20000g of cyclohexane , the material was gradually heated up to 60°C within 50 minutes, and then kept at 60°C for 60 minutes.

[0032] The second step: transfer the upper layer liquid A in the first step to a clean reactor ②, first distill 14000g of cyclohexane solvent at a temperature of 80-90°C and normal pressure, and then the upper layer liquid A The remaining part is distilled under reduced pressure step by step, the final distillation temperature is 70°C, and the highest vacuum degree reaches 50 Pa. After the distillation, high-purity bisphenol A diglycidyl ether is obtained.

Embodiment 2

[0034]Step 1: Add 3000g epoxy resin (epoxy value 0.51) and 300g chromatographic silica gel (particle size 400-500 mesh) to the 30L reactor ① in turn, raise the temperature of the material to 85°C under stirring, and keep it warm for 30 minutes , and then add 17000g of petroleum ether to make the temperature of the material gradually rise to 75°C within 60 minutes, and then keep it at 75°C for 80 minutes. b.

[0035] The second step: transfer the upper layer material liquid A in the first step to a clean reactor ②, first distill 15300g of petroleum ether solvent at a temperature of 85-95°C and normal pressure, and then the upper layer material liquid A The remaining part is distilled under reduced pressure step by step. The final distillation temperature is 90°C and the maximum vacuum reaches 80 Pa. After the distillation, high-purity bisphenol A diglycidyl ether is obtained.

Embodiment 3

[0037] Step 1: Add 3000g of epoxy resin (epoxy value 0.53) and 360g of polyethylene glycol 400 to the 30L reactor ① in sequence, raise the temperature of the material to 90°C under stirring, keep it warm for 50 minutes, then add 17000g of n-hexane alkane, the temperature of the material was gradually raised to 65°C within 40 minutes, and then kept at 65°C for 70 minutes.

[0038] The second step: transfer the upper layer material liquid A in the first step to a clean reactor ②, first distill 14500g of n-hexane solvent at a temperature of 85-95°C and normal pressure, and then remove the upper layer material liquid A The remaining part is distilled under reduced pressure step by step. The final distillation temperature is 100°C and the maximum vacuum reaches 90 Pa. After the distillation, high-purity bisphenol A diglycidyl ether is obtained.

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Abstract

The invention discloses a method for purifying bisphenol A diglycidyl ether, which is characterized in that it comprises: adding 100 parts by mass of liquid bisphenol A type epoxy resin and 6-16 parts by mass of a selection aid in reactor ①, Stir and heat to 80-90°C, keep warm for 30-60 minutes, then add 500-950 parts by mass of solvent I, make the material heat up to 45-75°C within 30-80 minutes, keep the temperature for 60-80 minutes, Separate the upper layer feed liquid A and the lower layer feed liquid B in the reactor ① and put them into the reactor ② and the reactor ③ respectively; distill the upper layer feed liquid A of the reactor ② at 65~95°C to distill 70%~90% % solvent I, and then carry out vacuum distillation, the residue in the reactor ② is the obtained bisphenol A diglycidyl ether; further includes the recovery of selection aids. The invention is easy to operate, the solvent, the selection aid and the like in the system can be recovered and recycled, and the product yield and purity are high.

Description

Technical field [0001] The present invention is a separation of organic epoxy compounds, involving a method that is separated from the principle of similarity and similarities.It is particularly suitable for separating bisphenols A two -shrimply gly gly gly glyceral ether from a bisphenol -A -type epoxy resin. Background technique [0002] Bisphenol -A -type epoxy resin is generally a collection of different aggregate "N" values. The different degree of polymerization "N" value causes different forms and characteristics of epoxy resin.High -purity and low viscosity bisphenol A -type epoxy resin has the characteristics of ordinary bisphenol -A -type epoxy resin. Its mainly divided into bisphenol A two -shrinking gly glycerin ether in "n = 0".When the content is very high (mass percentage content ≥90%, that is, high purity) shows the low viscosity characteristics, the viscosity at 25 ° C is only 4000 to 7000MPa.s, and only 1 / only the viscosity of ordinary epoxy resin (E-51)3 ~ 1 / 2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/27C07D301/32
Inventor 吴学明杨波唐安斌韩勇叶伦学
Owner SICHUAN DONGFANG INSULATING MATERIAL
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