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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 relatively large, the total yield of the product is low, and the production cost is relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

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

example 2

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

[0019] Table 1 Effect of mother liquor reuse times on whiteness

...

example 3

[0022] Add 160g of chlorinated benzene, 27.5g of bisphenol A, and 35g of water into a three-necked flask with stirring, add 43ml of 27.5% hydrogen peroxide while stirring, and pass cooling water at the same time. When the temperature of the solution is lower than 20°C, add 40g of bromine dropwise, and keep the temperature below 45°C. After the addition of bromine is completed, keep warm for 0.25 to 3 hours. Raise the temperature to 92°C, keep it warm for 10 minutes, add 8% sodium sulfite solution to make the red color of the solution disappear, separate the water layer, add 1g of ascorbic acid to the organic layer, pass cooling water to cool down to 20°C, filter with suction, and put the obtained crystals at 80°C drying. 50 g of the product was obtained 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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