Method for producing tetrabromobisphemol A with high whiteness degree

A technology of tetrabromobisphenol and high whiteness, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large product loss, low total product yield, high production cost, etc., and achieve whiteness Good, environment-friendly effect

Inactive Publication Date: 2009-05-13
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high solubility of tetrabromobisphenol A in chlorinated benzene, the product loss is re

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1

[0016] 160g of chlorinated benzene, 27.5g of bisphenol A, and 35g of water were put into a three-necked flask with stirring, 30ml of 27.5% hydrogen peroxide was added under stirring, and cooling water was passed through at the same time. When the temperature of the solution is lower than 20°C, add 40g of bromine dropwise and keep the temperature lower than 50°C. After bromine addition is completed, keep it warm for 0.2 to 3 hours. Warm up to 92°C, keep the temperature for 10 minutes, add 8% sodium sulfite solution to eliminate the color of bromine, let stand to separate the water layer, then add 1g hydroxylamine hydrochloride, 30g water, stir, cool down to 20°C with cooling water, and filter by suction. The obtained crystals were dried at 80°C. The obtained product is 51 g, with a purity of 99.4% and a melting point of 180°C. Whiteness (AHPA)≤10

Example Embodiment

[0017] Example 2

[0018] The mother liquor of Example 1, 27.5 g of bisphenol A, and 35 g of water were put into a three-necked flask with stirring, 30 ml of 27.5% hydrogen peroxide was added under stirring, and cooling water was passed through at the same time. When the temperature of the solution is lower than 20°C, add 40g of bromine dropwise and keep the temperature lower than 50°C. After bromine addition is completed, keep it warm for 0.2 to 3 hours. Warm up to 92°C, keep the temperature for 10 minutes, add 8% sodium sulfite solution to eliminate the color of bromine, let stand to separate the water layer, then add 1g hydroxylamine hydrochloride, 30g water, stir, cool down to 20°C with cooling water, and filter by suction. The obtained crystals were dried at 80°C. 63 g of the product was obtained, the purity of the product was 99.4%, and the melting point was 180°C. Whiteness (AHPA)≤10. The mother liquor was reused, and the results are listed in Table 1.

[0019] Table 1 The ...

Example Embodiment

[0021] Example 3

[0022] 160 g of chlorinated benzene, 27.5 g of bisphenol A, and 35 g of water were put into a three-necked flask with stirring, and 43 ml of 27.5% hydrogen peroxide was added under stirring, and cooling water was passed through at the same time. When the temperature of the solution is lower than 20°C, add 40g of bromine dropwise and keep the temperature lower than 45°C. After bromine addition is complete, keep it warm for 0.25 to 3 hours. Raise the temperature to 92℃, keep the temperature for 10 minutes, add 8% sodium sulfite solution to make the solution red disappear, separate the water layer, add 1g ascorbic acid to the organic layer, cool down to 20℃ with cooling water, and filter the obtained crystals at 80℃ drying. The obtained product is 50 g, with a purity of 99.5% and a melting point of 180°C. Whiteness (AHPA)≤10.

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Abstract

The invention relates to a method for producing high-whiteness tetrabromobisphenol A, which comprises the following steps: bromine and bisphenol A are subjected to substitution reaction in a benzene chloride solvent by the prior art to generate tetrabromobisphenol A; the temperature is raised to 92 DEG C, and superfluous oxyful is fully decomposed; and superfluous bromine is reduced by sodium sulfite, and coloured substances are reduced by a reducing agent, so as to obtain the high-whiteness tetrabromobisphenol A. The technology does not generate substances which pollute the environment in the production process, and is environment-friendly; the whiteness of the products is good; a mother liquor can not be forced to be distilled and purified because the whiteness of the products can not reach the national standards; and the tetrabromobisphenol A is produced in the benzene chloride solvent, so that manufacturing enterprises can produce the high-whiteness tetrabromobisphenol A by the method without purchasing equipment.

Description

Technical field: [0001] The invention belongs to a production method of flame retardant tetrabromobisphenol A. Background technique: [0002] Tetrabromobisphenol A is a reactive flame retardant and an additive flame retardant, which is widely used in the production of flame retardant plastics and has good flame retardant effect. As a reactive flame retardant, it can be used in the production of flame retardant resins such as epoxy resin and polycarbonate; as an additive flame retardant, it can be used in the production of flame retardant resins such as polystyrene resin, ABS resin and phenolic resin. . [0003] To produce tetrabromobisphenol A, methanol can be used as a solvent, bisphenol A is dissolved in methanol, and then reacted with bromine to prepare tetrabromobisphenol A. In this process, methyl bromide is generated. Methyl bromide is considered an ozone depleting substance and is banned. [0004] Domestic production of tetrabromobisphenol A generally uses chlorina...

Claims

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Application Information

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IPC IPC(8): C07C39/367C07C37/02
Inventor 孔庆池
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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