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ECO-friendly method of preparation of high purity tetrabromobisphenol-A

A technology of tetrabromobisphenol and bisphenol, applied in the field of preparation that does not harm the ecological environment, to achieve the effect of easy washing and easy separation

Inactive Publication Date: 2009-08-05
科学和工业研究会
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that it uses liquid bromine as the brominating agent and requires a non-brominated compound (which decomposes naturally at room temperature) to use the hydrobromic acid formed during the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Under stirring condition, in the 25g (0.11mol) bisphenol-A in the 75ml carbon tetrachloride in the 500ml two-neck round bottom flask, add 31.62g (0.31mol or 2.80 equivalent) sodium bromide and dissolve in 50ml water 0.05g of sodium lauryl sulfate and 45ml (0.54 moles) of 12N hydrochloric acid. The flask was cooled to 10°C by placing it in a cold water bath. Within 4 h, 22.1 g (0.15 mol or 1.34 eq) of sodium bromate in 75 ml of aqueous solution were slowly added under stirring conditions. The contents were stirred for an additional 30 minutes, the organic layer containing fine colorless crystals of TBBPA at the bottom of the flask was separated, and the organic layer was concentrated to a quarter of its volume. The product was filtered, washed twice with deionized water and dried in an oven at 100°C to obtain additional amounts of tetrabromobisphenol-A. The overall isolated yield of tetrabromobisphenol-A was 92.28%. The recorded characteristic data of the isolated sam...

Embodiment 2

[0079] Under stirring condition, in the 25g (0.11mol) bisphenol-A in the 75ml dichloromethane in the 500ml two-neck round bottom flask, add 31.62g (0.31mol or 2.80 equivalent) sodium bromide and dissolve in 50ml water 0.05g sodium lauryl sulfate and 45ml (0.54mol) 12N hydrochloric acid. The flask was cooled to 10°C by placing it in a cold water bath. Within 4 h, 22.1 g (0.15 mol or 1.34 eq) of sodium bromate in 75 ml of aqueous solution were slowly added under stirring conditions. The contents were stirred for an additional 30 minutes. The crystalline product was filtered, washed twice with deionized water and dried in an oven at 100°C to afford 37.20 g (62.42% yield) of tetrabromobisphenol-A (mp, 181-182°C). The organic layer was separated from the mother liquor and concentrated to a quarter of its volume. To obtain an additional 16.70 g of tetrabromobisphenol-A (28.02% yield), the total isolated yield of tetrabromobisphenol-A was 90.44%. The characteristic data recorded ...

Embodiment 3

[0081] Under stirring condition, in the 25g (0.11mol) bisphenol-A in the 75ml dichloromethane in the 500ml two-neck round bottom flask, add 31.62g (0.31mol or 2.80 equivalent) sodium bromide and dissolve in 50ml water 0.05g sodium lauryl sulfate and 45ml (0.54mol) 12N hydrochloric acid. The flask was cooled to 10°C by placing it in a cold water bath. Within 4 h, 22.1 g (0.15 mol or 1.34 eq) of sodium bromate in 75 ml of aqueous solution were slowly added under stirring conditions. The contents were stirred for an additional 30 minutes. The crystalline product was filtered, washed twice with deionized water and dried in an oven at 100°C to afford 39.70 g (66.61% yield) of tetrabromobisphenol-A (mp 181-182°C). The organic layer (70ml) was separated and used for the test of Example 4. The recorded characteristic data for the isolated sample are 1 H-NMR (CD 3OD, 200MHz): 1.58δ(s, 6H), 7.25δ(s, 4H), elemental components: 32.9(%C), 2.19(%H) and 58.3(%Br).

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Abstract

In the first batch, high-purity colorless tetrabromobisphenol-A (TBBPA) with a melting point of 178-182°C was prepared in a yield of 50-70%, and the yield was 90-100%. In this method, the caustic liquid bromine is replaced by sodium bromide / hydrobromic acid as the brominating agent. In addition, sodium bromate was used as an oxidizing agent as well as a brominating agent to utilize hydrobromic acid generated during bisphenol-A (BPA) bromination. The reaction is carried out in the presence of hydrochloric acid and sodium lauryl sulfate in a mixture of dichloromethane-water or carbon tetrachloride-water at 10-15°C. The crystalline product precipitated at the bottom of the reaction vessel was filtered, washed, dried and weighed. Recycling of the spent organic layer in subsequent batches maximizes the yield of product recovered directly as a solid and minimizes the generation of organic emissions.

Description

technical field [0001] The invention relates to a preparation method of high-purity tetrabromobisphenol-A which does not harm the ecological environment. Background of the invention [0002] Tetrabromobisphenol-A, (CH 3 ) 2 C(C 6 h 2 Br 2 Oh) 2 (TBBPA, 79-94-7) is an important substance among various brominated compounds. It is a brominated derivative of bisphenol-A (BPA). The high stability and adaptability as an additive and reactive compound make it useful as a flame retardant, which accounts for more than one-third of the total brominated flame retardants. TBBPA is also used in the preparation of acrylonitrile butadiene styrene (ABS) polymers and in the preparation of epoxy and polycarbonate resins. These resins are widely used in the manufacture of electronic equipment, especially computer printed circuit boards. Since TBBPA's high activity allows it to be used at relatively low loadings, the resin is also used as a flame retardant in the manufacture of coating...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/367C07C37/62C07C
CPCC07C37/62C07C39/367
Inventor G·拉马钱德兰P·K·高希A·S·梅赫塔P·P·拉杰什A·D·杰特瓦S·S·瓦格海拉S·N·米斯拉
Owner 科学和工业研究会
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