Process for producing octabromodiphenyl ethane

A technology of octabromodiphenylethane and diphenylethane, which is applied in the field of preparation of octabromodiphenylethane and achieves the effects of high bromine content, small investment and simple reaction control

Active Publication Date: 2009-05-13
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Tests have shown that octabromodiphenylethane and tetrabromobisphenol A have similar melting points and melting ranges. Tetrabromobisphenol A has been widely used as a flame retardant to manufacture ABS resins, but octabromodiphenylethane is used as a flame retardant. Burning agent has not been used to make ABS resin until now

Method used

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  • Process for producing octabromodiphenyl ethane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 0.9 g of aluminum powder to 500 g of liquid bromine, stir and react for 20 minutes to generate a reaction mixture A of bromine and aluminum powder; The addition time was 15 minutes. After the dropwise addition was completed, the stirring reaction was continued for 0.5 hours at a temperature of 5° C. to obtain a mixture B; under stirring conditions, 120 grams of water and 0.6 grams of ethylenediaminetetraacetic acid were added to the above mixture B, and stirred for 30 Minutes later, the mixture C was obtained; the above-mentioned mixture C was distilled under the condition of negative pressure -0.06Mpa. When the temperature rose to 77°C, the distillation was completed, and then the product after the distillation was suction filtered to obtain 44 grams of crude octabromodiphenylethane; Add 110 grams of water and 0.88 grams of solid caustic soda to the above-mentioned crude product of octabromodiphenylethane, then carry out wet pulverization, and after wet pulverizatio...

Embodiment 2

[0026] Add 1.1 g of iron powder to 500 g of liquid bromine, stir and react for 22 minutes to generate a reaction mixture A of bromine and iron powder; The addition time was 20 minutes. After the dropwise addition was completed, the stirring reaction was continued for 0.5 hours at a temperature of 4°C to obtain a mixture B; under stirring conditions, 150 g of water and 1.0 g of sodium edetate were added to the above mixture B, and stirred After 32 minutes, the mixture C was obtained; the above-mentioned mixture C was distilled under the condition of negative pressure -0.07Mpa. When the temperature rose to 76°C, the distillation was completed, and then the product after distillation was filtered with suction to obtain 53.2 grams of crude octabromodiphenylethane Add 128 grams of water and 2.4 grams of sodium sulfite to the above-mentioned octabromodiphenylethane crude product, then carry out wet pulverization, and after wet pulverization for 9.5 hours, carry out suction filter, ob...

Embodiment 3

[0028] Add 1.3 g of a mixture of aluminum powder and iron powder to 500 g of liquid bromine, and stir for 25 minutes to generate a reaction mixture A of bromine, aluminum powder and iron powder; 14 grams of diphenylethane, the dropwise addition time is 22 minutes, after the dropwise addition is completed, the stirring reaction is continued for 40 minutes at a temperature of 5° C. to obtain a mixture B; under stirring conditions, 160 grams of water and a concentration of 4 grams of 30% hydrochloric acid, after stirring for 34 minutes, mixture C was obtained; under the condition of negative pressure ~ 0.075Mpa, the above mixture C was distilled. When the temperature rose to 75°C, the distillation ended, and then the product was filtered and distilled to obtain eight Brominated diphenyl ethane crude product 59.99 grams; Add 132 grams of water and 3.9 grams of soda ash in the above-mentioned octabromodiphenyl ethane crude product, carry out wet pulverization then, after wet pulveri...

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Abstract

The invention discloses a method for preparing octabromo-diphenylethane. The method comprises the following steps: catalyst is added into liquid bromine and stirred for reaction, and a mixture A of the liquid bromine and the catalyst is obtained; diarylethane is dripped into the mixture A under the condition of stirring, and continuously stirred for reaction after the dripping process is over, and a mixture B is obtained; water and a metallic ion remover are added into the mixture B under the condition of stirring, and a mixture C is obtained; the mixture C is distilled for removal of superfluous liquid bromine and superfluous catalyst, and a product obtained after distillation is filtered to obtain a coarse octabromo-diphenylethane product; the octabromo-diphenylethane is added with water and a debrominating agent, crushed by the wet method, and subjected to solid-liquid separation after crushing to obtain a filter cake; and the filter cake is dried, and subjected to gas flow crushing to obtain white or primrose octabromo-diphenylethane solid powder. The method has easily obtained raw materials and small investment, and is simple in reaction control and easy in industrial production control. The bromine content of the product is high and can reach between 78 and 78.6.

Description

technical field [0001] The invention relates to a preparation method of octabromodiphenylethane. Background technique [0002] As an additive brominated flame retardant, octabromodiphenylethane has a bromine content of up to 78.62%. At present, there is no synthesis process for octabromodiphenylethane products at home and abroad, and as a theoretical basis for octabromodiphenylethane Research is also almost blank. Tests have shown that octabromodiphenylethane and tetrabromobisphenol A have similar melting points and melting ranges. Tetrabromobisphenol A has been widely used as a flame retardant to manufacture ABS resins, but octabromodiphenylethane is used as a flame retardant. Burning agents have not been used to make ABS resin until now. Contents of the invention [0003] The object of the present invention is to provide a method for preparing a high-quality novel brominated flame retardant octabromodiphenylethane with stable bromine content, low cost and no pollution....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/18C07C17/10
Inventor 王善华孟烨李世祥唐星三邢晓华
Owner SHANDONG TIANYI CHEM
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