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Preparation method of epoxy resins with low total chlorine content

A technology of total chlorine content and epoxy resin, which is applied in the field of preparation of epoxy resin with low total chlorine content, can solve problems such as epoxy resin anionic polymerization gel, purified epoxy resin viscosity, epoxy value change, etc., to meet the conditions Mildness, reduced by-product content, stable viscosity and yield effects

Active Publication Date: 2021-06-25
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent application (CN200480000133.3) discloses a refining method for treating epoxy resin with a high-concentration alkali metal hydroxide aqueous solution (concentration ≥ 80%), which can obtain high-purity epoxy resin with a total chlorine content of 500ppm or lower ; Chinese patent application (CN201711442464.8) discloses the refining method of utilizing alkali metal / alkaline earth metal catalyst A and salt-based catalyst B to treat epoxy resin, and can also obtain ultra-high-purity ring with total chlorine content below 500ppm Oxygen resin; however, due to the use of high-concentration alkali treatment in the above two methods, it is easy to cause anionic polymerization of epoxy resin to produce gel during the purification process, which changes the viscosity, epoxy value and other parameters of purified epoxy resin

Method used

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Examples

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Embodiment 1

[0039] Embodiment 1, the synthesis of bisphenol A diglycidyl ether

[0040]Add 228g of bisphenol A, 555g of epichlorohydrin and 88g of dioxane into a 2000ml three-necked flask equipped with a mechanical stirrer, an azeotropic reflux dehydrator and a thermometer, stir and heat to 40°C. After the reaction solution was dissolved until transparent, 120 g of solid sodium hydroxide with an average particle diameter of 1.0 mm was added, and then the pressure was reduced (the vacuum degree in the reaction vessel was adjusted to 20 kPa), and the reaction was continued at 40° C. for 2.5 hours. After the reaction was completed, it was filtered while it was hot, and then subjected to vacuum distillation (distillation temperature 110° C., vacuum degree 0.5 kPa) to obtain 320.5 g of crude product.

[0041] The crude product was uniformly dissolved in 330 g of toluene, then 150 g of 10% sodium hydroxide aqueous solution was added, and the temperature was raised to 50° C. while stirring, and ...

Embodiment 2

[0043] Embodiment 2, the synthesis of bisphenol A diglycidyl ether

[0044] Add 228g of bisphenol A, 925.2g of epichlorohydrin and 156g of dimethyl sulfoxide into a 3000ml three-necked flask equipped with a mechanical stirrer, an azeotropic reflux dehydrator and a thermometer, stir and heat to 55°C. After the reaction solution was dissolved until transparent, 96 g of solid sodium hydroxide with an average particle diameter of 1.5 mm was added, and then the pressure was reduced (the vacuum degree in the reaction vessel was adjusted to 30 kPa), and the reaction was continued at 55° C. for 2 hours. After the reaction was completed, it was filtered while it was hot, and then subjected to vacuum distillation (distillation temperature 130° C., vacuum degree 0.5 kPa) to obtain 316 g of crude product.

[0045] The crude product was uniformly dissolved in 300 g of xylene, then 100 g of 5% sodium hydroxide aqueous solution was added, and the temperature was raised to 60° C. while stirri...

Embodiment 3

[0047] Embodiment 3, the synthesis of bisphenol F diglycidyl ether

[0048] Add 200g of bisphenol F, 740.2g of epichlorohydrin and 88g of dioxane into a 2000ml three-necked flask equipped with a mechanical stirrer, an azeotropic reflux dehydrator and a thermometer, stir and heat to 45°C. After the reaction solution was dissolved until transparent, 112 g of solid sodium hydroxide with an average particle diameter of 1.2 mm was added, and then the pressure was reduced (the vacuum degree in the reaction vessel was adjusted to 26 kPa), and the reaction was continued at 45° C. for 2.5 hours. After the reaction was completed, it was filtered while it was hot, and then subjected to vacuum distillation (distillation temperature 110° C., vacuum degree 0.5 kPa) to obtain 296.9 g of crude product.

[0049] The crude product was uniformly dissolved in 300 g of xylene, then 120 g of 10% sodium hydroxide aqueous solution was added, and the temperature was raised to 60° C. while stirring, an...

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Abstract

The invention discloses a preparation method of glycidyl ether epoxy resins with low total chlorine content. The preparation method comprises two steps of synthesis and refining treatment, wherein in the synthesis step, a phenol or alcohol raw material, epoxy chloropropane, an aprotic polar solvent and a granular alkali metal hydroxide with a specific particle size are subjected to a one-step reaction; and in the refining step, the resin product is treated by adopting an alkaline aqueous solution with the concentration of 2-10%. According to the preparation method disclosed by the invention, the ultra-high-purity epoxy resin with the total chlorine content lower than 200 ppm can be obtained. The preparation method provided by the invention is suitable for preparing various glycidyl ether epoxy resins, and has the advantages of low total chlorine content of the product, high epoxy value and yield, mild reaction conditions and the like.

Description

technical field [0001] The invention relates to a preparation method of epoxy resin with low total chlorine content, belonging to the technical field of epoxy resin. Background technique [0002] Since the molecular structure of epoxy resin contains two or more epoxy groups, it can react with amines, acid anhydrides, etc. to form a stable three-dimensional cross-linked structure, so it has excellent mechanical strength, dimensional stability, chemical resistance and heat resistance. It is widely used in fiber reinforced composite materials, electronic and electrical packaging materials and adhesives and other fields. According to the different chemical groups connected to epoxy groups, epoxy resins can be divided into glycidyl ether epoxy resins, glycidyl ester epoxy resins, glycidyl amine epoxy resins, etc., which are composed of hydroxyl, carboxyl and amino groups and epoxy resins. Chloropropane is prepared by reaction. [0003] The synthesis of epoxy resin is generally ...

Claims

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Application Information

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IPC IPC(8): C08G59/06C08G59/04C08G59/08
CPCC08G59/063C08G59/04C08G59/08
Inventor 杨欣黄伟刘盛祁志强赵晓娟于然张瑛
Owner INST OF CHEM CHINESE ACAD OF SCI
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