The synthetic method of brominated epoxy resin

A technology of brominated epoxy resin and synthesis method, which is applied in the field of epoxy resin, and can solve problems such as high organic chlorine content, deep product color, and light product color

Active Publication Date: 2018-02-27
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on this, it is necessary to solve the problems of low reaction yield, more by-products, high organic chlorine content and dark product color of traditional brominated epoxy resins, and provide a high reaction yield, less by-products, low organic chlorine content Synthesis method of brominated epoxy resin with low and light product color

Method used

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  • The synthetic method of brominated epoxy resin

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preparation example Construction

[0024] see figure 1 , the synthetic method of the brominated epoxy resin of an embodiment, comprises the following steps:

[0025] Step S110, in a protective gas atmosphere, mix and stir tetrabromobisphenol A, epichlorohydrin, solvent, the first auxiliary agent and the second auxiliary agent, and dissolve at 70°C~90°C for 1~2 hours to obtain The reaction solution.

[0026] Wherein, the protective gas is nitrogen.

[0027] The first auxiliary agent is selected from at least one of phosphite, pentaerythritol diphosphate, pentaerythritol diphosphite and thioester.

[0028] The second additive is selected from at least one of ethylene glycol, propylene glycol, n-butanol, isobutanol and neopentyl alcohol.

[0029] The solvent is at least one selected from toluene, benzene, xylene, methyl isobutyl ketone and n-butanol.

[0030] In this embodiment, in parts by mass, tetrabromobisphenol A is 272 parts, epichlorohydrin is 70-100 parts, solvent is 70-140 parts, the first auxiliary a...

Embodiment 1

[0046] In a nitrogen atmosphere, 272g of tetrabromobisphenol A, 70g of epichlorohydrin, 70g of methyl isobutyl ketone, 1g of phospholipid and 5g of ethylene glycol were mixed and stirred, and dissolved at 70°C for 1 hour to obtain a reaction solution. At 80° C., 10 g of 30% NaOH aqueous solution was added dropwise to the above reaction solution for 1 hour, then the reaction was maintained for 2 hours, 150 g of 30% NaOH aqueous solution was added, and the mixture was obtained for 3 hours. The above mixture was dissolved in 300 g of methyl isobutyl ketone, 10 g of 10% NaOH aqueous solution was added, and the mixture was reacted at 85° C. for 1 hour to obtain a reaction mixture. Dissolve the above reaction mixture in methyl isobutyl ketone again, add 10g of phosphoric acid and 80g of water, wash with water several times until neutral, separate the liquids, take the organic layer, and distill under reduced pressure to separate the solvent to obtain brominated epoxy resin .

[004...

Embodiment 2

[0059] In a nitrogen atmosphere, 272g of tetrabromobisphenol A, 100g of epichlorohydrin, 140g of toluene, 10g of pentaerythritol diphosphate and 15g of propylene glycol were mixed and stirred, and dissolved at 90° C. for 2 hours to obtain a reaction solution. At 95° C., 25 g of 28% NaOH aqueous solution was added dropwise to the above reaction solution for 3 hours, and the reaction was maintained for 4 hours. 250 g of 28% NaOH aqueous solution was added and reacted for 5 hours to obtain a mixture. The above mixture was dissolved in 500 g of toluene, 30 g of 20% NaOH aqueous solution was added, and the mixture was reacted at 100° C. for 3 hours to obtain a reaction mixture. The above reaction mixture was dissolved in toluene again, 110 g of water was added, washed with water several times until neutral, separated, the organic layer was taken, and the solvent was separated by distillation under reduced pressure to obtain a brominated epoxy resin.

[0060] After measurement, the ...

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Abstract

The invention provides a synthesis method of brominated epoxy resin, comprising the following steps: in a protective gas atmosphere, mixing and stirring tetrabromobisphenol A, epichlorohydrin, a solvent, a first auxiliary agent and a second auxiliary agent , to obtain a reaction solution; then dropwise add 28% to 32% NaOH aqueous solution to the reaction solution for 1 to 3 hours, maintain the reaction for 2 to 4 hours after the dropwise addition, then add 28% to 32% NaOH aqueous solution, and react for 3 to 3 hours 5 hours to obtain a mixture; dissolve the mixture in a solvent, add 10% to 20% NaOH aqueous solution, and react at 85°C to 100°C for 1 to 3 hours to obtain a reaction mixture; and dissolve the reaction mixture in a solvent again In, separated and purified to obtain brominated epoxy resin. The synthesis method of the above-mentioned brominated epoxy resin effectively controls the occurrence of side reactions in the reaction process, and effectively controls the dissolution and oxidation phenomena in the reaction process.

Description

technical field [0001] The invention relates to the field of epoxy resins, in particular to a synthesis method of brominated epoxy resins. Background technique [0002] With the gradual popularity of plastics, rubber, resins, etc. in daily life, the demand for flame retardants is also increasing, and it has become the second largest additive in plastics, rubber, resins, etc. after plasticizers fine chemicals, while bromine series flame retardants account for about 39% of the total demand for flame retardants. As people's awareness of environmental protection and health continues to increase, the product structure of my country's flame retardant industry will also be adjusted accordingly. New environmentally friendly flame retardants will gradually replace traditional flame retardants that are harmful to the environment and human health. Brominated epoxy resin is a new type of brominated flame retardant developed in recent years. It has satisfactory melt flow rate and high f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/06C08K5/00C08K5/524C08K5/521C08K5/38C08K5/053C08K5/05
Inventor 汤冬英周建宏王新龙喻林蔡立
Owner CHINA PETROLEUM & CHEM CORP
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