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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: 2012-10-10
SICHUAN DONGFANG INSULATING MATERIAL
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  • Abstract
  • Description
  • Claims
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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

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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, and the method is characterized by comprising the following steps of: adding 100 parts by weight of liquid bisphenol A type epoxy resin and 6-16 parts by weight of selective auxiliary agent into a reactor (1), heating up to 80-90 DEG C while stirring, carrying out heat preservation for 30-60 minutes, adding 500-950 parts by weight of solvent I, heating the material up to 45-75 DEG C within 30-80 minutes, carrying out heat preservation for 60-80 minutes and standing still; separating upper-layer liquid A and lower-layer liquid B in the reactor (1) and respectively putting the upper-layer liquid A and the lower-layer liquid B into a reactor (2) and a reactor (3); distilling the upper-layer liquid A in the reactor (2) at 65-95 DEG C to obtain 70-90% of solvent I, and then carrying out reduced pressure distillation, wherein the residue in the reactor (2) is the prepared bisphenol A diglycidyl ether; and finally, further recovering the selective auxiliary agent. The method is easy to operate, the solvent, the selective auxiliary agent and the like in the system can be recycled, and the yield and purity of the product are high.

Description

technical field [0001] The invention belongs to the separation of organic epoxy compounds, and relates to a method for separating and purifying bisphenol A diglycidyl ether by utilizing the principle of similarity and similarity. It is especially suitable for separating and purifying bisphenol A diglycidyl ether from bisphenol A type epoxy resin. Background technique [0002] Bisphenol A type epoxy resin is generally an aggregate composed of different polymerization degree "n" values. Different polymerization degree "n" values ​​lead to different shapes and characteristics of epoxy resins. High-purity and low-viscosity bisphenol-A epoxy resin has the characteristics that ordinary bisphenol-A epoxy resin does not have. Its main component is bisphenol-A diglycidyl ether with "n=0". When the content of epoxy resin is very high (mass percentage content ≥ 90%, that is, high purity), it shows low viscosity characteristics, and the viscosity at 25°C is only 4000-7000mPa.s, which i...

Claims

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Application Information

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Patent Type & Authority Applications(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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