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A kind of epoxide with low total chlorine content and no heavy metal residue and its synthesis process

一种环氧化物、合成工艺的技术，应用在有机化学、化学仪器和方法、分离方法等方向，能够解决残留、交联影响、影响产品固化速度等问题

Active Publication Date: 2021-05-18
JIANGSU TETRA NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Because prior art method adopts the cycloaliphatic epoxy resin prepared by the method of traditional catalyst more, usually contains heavy metal ion (such as tungsten W) in this type of catalyst, so reaction product also contains certain heavy metal ion residue correspondingly; Due to the influence of the catalyst, the final product also has heavy metal ions remaining. This trace amount of heavy metal ions also affects the curing speed of the product (ie gel time); the crosslinking in the molecule is affected during curing, resulting in prolonged gel time of the product. Thus affecting production efficiency and product quality

Method used

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  • A kind of epoxide with low total chlorine content and no heavy metal residue and its synthesis process
  • A kind of epoxide with low total chlorine content and no heavy metal residue and its synthesis process
  • A kind of epoxide with low total chlorine content and no heavy metal residue and its synthesis process

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Effect test

Embodiment 1

[0088] Embodiment 1 of the present invention provides an epoxide, and the preparation raw materials of the epoxide include an unsaturated alicyclic compound containing a double bond, hydrogen peroxide, an organic acid compound, a solvent, and a basic salt.

[0089] The unsaturated alicyclic compound containing a double bond is methacrylic acid-3-cyclohexenyl methyl ester; the organic acid compound is acetic anhydride, and the purity of the acetic anhydride is 98wt%, and the acetic anhydride The molar ratio of methacrylic acid-3-cyclohexenyl methyl ester is 1.2:1; the concentration of the hydrogen peroxide solution is 35wt%, and the hydrogen peroxide and methacrylic acid-3-cyclohexenyl methyl The molar ratio of double bonds in the ring in the ester is 1.5:1; the solvent is toluene, and the weight ratio of toluene to 3-cyclohexenylmethyl methacrylate is 3:1; the basic salt is acetic acid sodium.

[0090] The synthetic technique of described epoxide comprises the following steps...

Embodiment 2

[0097] Embodiment 2 of the present invention provides an epoxide, and the preparation raw materials of the epoxide include an unsaturated alicyclic compound containing a double bond, hydrogen peroxide, an organic acid compound, a solvent, and a basic salt.

[0098] The unsaturated alicyclic compound containing a double bond is acrylate-3-cyclohexenyl methyl ester; the organic acid compound is acetic anhydride, and the purity of the acetic anhydride is 98wt%, and the acetic anhydride and acrylic acid The molar ratio of -3-cyclohexenyl methyl ester is 1.25:1; the concentration of the hydrogen peroxide solution is 35wt%, the hydrogen peroxide and the double bond The molar ratio is 1.5:1; the solvent is toluene, and the weight ratio of the toluene to 3-cyclohexenylmethyl acrylate is 3:1; the basic salt is sodium acetate.

[0099] The synthetic technique of described epoxide comprises the following steps:

[0100] (1) Mix unsaturated alicyclic compound, organic acid compound, basi...

Embodiment 3

[0106] Embodiment 3 of the present invention provides an epoxide. The raw materials for the preparation of the epoxide include unsaturated alicyclic compounds containing double bonds, hydrogen peroxide, organic acid compounds, solvents, and basic salts.

[0107] The unsaturated alicyclic compound containing double bonds is diglycidyl tetrahydrophthalate; the organic acid compound is acetic anhydride, and the purity of the acetic anhydride is 98wt%. The molar ratio of bisglycidyl hydrogen phthalate is 1.4:1; The molar ratio is 1.7:1; the solvent is toluene, and the weight ratio of the toluene to diglycidyl tetrahydrophthalate is 3:1; the basic salt is sodium acetate.

[0108] The synthetic technique of described epoxide comprises the following steps:

[0109] (1) Mix unsaturated alicyclic compound, organic acid compound, basic salt and solvent, and cool to 13°C;

[0110] (2) Add hydrogen peroxide solution dropwise for 2 hours, and then continue to react for 2 hours. The tempe...

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Abstract

The invention relates to the field of epoxy resins, more specifically, the invention relates to an epoxy with low total chlorine content and no heavy metal residue and a synthesis process. The first aspect of the present invention provides an epoxide, the preparation raw material of the epoxide includes an unsaturated alicyclic compound containing a double bond, hydrogen peroxide, an organic acid compound, a solvent, and a basic salt; The molar ratio of the organic acid compound to the unsaturated alicyclic compound containing double bonds is (1-1.5):1. The epoxide obtained by the present invention has high yield, low solvent content, low chroma, low chlorine content and low metal ion content; meanwhile, the epoxide has a simple reaction system, is environmentally friendly, safe and controllable, and has low production cost. It can meet the requirements of technical economy and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of epoxy resins, more specifically, the invention relates to an epoxy with low total chlorine content and no heavy metal residue and a synthesis process. Background technique [0002] Cycloaliphatic epoxy resins and their cured products have excellent comprehensive properties such as processability, thermal stability, electrical insulation, and ultraviolet radiation resistance, and have been widely used in important industrial fields such as aerospace, microelectronic packaging, and motor insulation. In response to the increasing performance and functional requirements of modern industry for polymer materials, the synthesis and performance research of alicyclic epoxy resins has been very active in recent years. [0003] Compared with glycidyl ether type epoxy resin, cycloaliphatic epoxy resin has definite molecular weight and molecular structure, various synthesis methods, strong structural designability, easy to chan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02
CPCC08G59/027C07D301/16C07D303/16C07D303/44C07D303/00
Inventor 韩建伟贾泉常杨军曹祥明
Owner JIANGSU TETRA NEW MATERIAL TECH
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