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A kind of preparation method of tetrabromobisphenol A type epoxy resin

A technology of tetrabromobisphenol and epoxy resin, which is applied in the direction of organic chemistry, can solve the problems of inflexible control of bromine content in resin, energy and material consumption, and inability to provide production, etc., to achieve high bromine content, reduce steps, and reduce hydrolysis Effect

Active Publication Date: 2018-03-20
建滔(广州)电子材料制造有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, there are certain defects in the synthesis of existing brominated epoxy resins, such as the bromine content of the resin cannot be flexibly regulated, and production cannot be provided according to downstream product requirements. Tribromophenol is used as the end-capping agent. It is easy to sublimate and decompose at high temperature, which is not conducive to the reaction
In addition, in the prior art, after the ring-closing reaction is completed, the re-refining process is often used to reduce the hydrolyzable chlorine, which will complicate the reaction process and cause unnecessary energy and material consumption.

Method used

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  • A kind of preparation method of tetrabromobisphenol A type epoxy resin
  • A kind of preparation method of tetrabromobisphenol A type epoxy resin
  • A kind of preparation method of tetrabromobisphenol A type epoxy resin

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Effect test

Embodiment 1

[0036] Embodiment 1, the preparation of a kind of tetrabromobisphenol A type epoxy resin

[0037] S1 Add tetrabromobisphenol A and epichlorohydrin to the reaction kettle first, and the tetrabromobisphenol A and epichlorohydrin are added to the reaction kettle with a molar ratio of 1:1.6, and then add isopropanol aqueous solution , the isopropanol aqueous solution is composed of isopropanol and water in a volume ratio of 7:1, under nitrogen protection, stirred until completely dissolved, the mixture of tetrabromobisphenol A and epichlorohydrin and isopropanol The aqueous solution is added to the reactor in a ratio of 3:1 by weight;

[0038] S2 is that the aqueous solution of 50% sodium hydroxide is added dropwise in the reactor in the mass percent, and the addition amount of the aqueous solution of sodium hydroxide is 1.5% of the addition amount of tetrabromobisphenol A, and at the condition that temperature is 55 ℃ Under reaction 40min, the rate of addition of the aqueous sol...

Embodiment 2

[0044] Embodiment 2, the preparation of a kind of tetrabromobisphenol A type epoxy resin

[0045] S1 Add tetrabromobisphenol A and epichlorohydrin to the reaction kettle first, the tetrabromobisphenol A and epichlorohydrin are added to the reaction kettle with a molar ratio of 1:1.8, and then add isopropanol aqueous solution , the isopropanol aqueous solution is composed of isopropanol and water in a volume ratio of 7:1, under nitrogen protection, stirred until completely dissolved, the mixture of tetrabromobisphenol A and epichlorohydrin and isopropanol The aqueous solution is added in the reactor in a ratio of 3.5:1 by weight;

[0046] S2 is that the aqueous solution of sodium hydroxide of 50% mass percent is added dropwise in the reaction kettle, the addition amount of the aqueous solution of sodium hydroxide is 2% of the addition amount of tetrabromobisphenol A, and at the condition that temperature is 60 ℃ Under reaction 50min, the rate of addition of the aqueous solutio...

Embodiment 3

[0052] Embodiment 3, the preparation of a kind of tetrabromobisphenol A type epoxy resin

[0053] S1 Add tetrabromobisphenol A and epichlorohydrin to the reaction kettle first, the tetrabromobisphenol A and epichlorohydrin are added to the reaction kettle with a molar ratio of 1:2, and then add isopropanol aqueous solution , the isopropanol aqueous solution is composed of isopropanol and water in a volume ratio of 7:1, under nitrogen protection, stirred until completely dissolved, the mixture of tetrabromobisphenol A and epichlorohydrin and isopropanol The aqueous solution is added to the reactor in a ratio of 4:1 by weight;

[0054] S2 is that the aqueous solution of sodium hydroxide of 50% by mass percent is added dropwise in the reaction kettle, the addition amount of the aqueous solution of sodium hydroxide is 2.5% of the addition amount of tetrabromobisphenol A, and at the condition that temperature is 65 ℃ Under reaction 60min, the rate of addition of the aqueous soluti...

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Abstract

The invention belongs to the field of high polymer materials and particularly relates to a preparation method of tetrabromobisphenol A epoxy resin. According to the preparation method of the tetrabromobisphenol A epoxy resin, tetrabromobisphenol A and epoxy chloropropane are used as reaction materials to react in an isopropanol water solution in a specific ratio with a three-step alkali adding method to produce the tetrabromobisphenol A epoxy resin. The prepared tetrabromobisphenol A epoxy resin has the advantages of low chromaticity, high transparency, moderate epoxy value, low tetrabromobisphenol A residue amount, low hydrolysable chloride content, low inogrnaic chlorine content and high tetrabromobisphenol A bis-glycidyl ether in the tetrabromobisphenol A epoxy resin. Meanwhile, the prepared tetrabromobisphenol A epoxy resin has the advantages of high dielectric constant and high voltage resistance value and is relatively ideal tetrabromobisphenol A epoxy resin.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of tetrabromobisphenol A epoxy resin. Background technique [0002] Bisphenol A type epoxy resin has good physical and chemical properties. It has excellent bonding strength to the surface of metal and non-metal materials, and has good dielectric properties, small set shrinkage, good dimensional stability of products, and high hardness. It is widely used in pouring, impregnation, lamination, adhesives, coatings and other fields due to its advantages of high strength, good flexibility, and stability to alkali and most solvents. In recent years, with the gradual expansion of the application of epoxy resin in high technology, the requirements for the performance of epoxy resin, such as heat resistance, weather resistance, high adhesion, corrosion resistance, etc., have been continuously improved. Purity requirements are also increasing. [0003] Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/27C07D301/28C07D301/32C08G59/06
CPCC07D301/28C07D301/32C07D303/27C08G59/063
Inventor 张广军
Owner 建滔(广州)电子材料制造有限公司