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Process for prepn of non-hazardous brominating agent

A technology for bromination reagents and oxidants, applied in the direction of bromine/hydrogen bromide, oxybromide, bromine, etc., can solve the problems of increased cost and large volume, and achieve the effect of avoiding demand

Inactive Publication Date: 2006-09-20
COUNCIL OF SCI & IND RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is the larger volume of hypochlorite solution required to achieve the desired ratio of bromide to bromate, which unnecessarily increases the cost of the method, or requires larger vessels to handle the bromination reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A basic bromine mixture (1.0 liters) with a ratio of bromide to bromate of 4.4:1 was added to a three-necked round-bottomed flask, and 2.0 liters of deionized water containing 13.05 moles of NaOH was added to the mixture, and stirred at 25°C mix. With the temperature maintained at 25° C., chlorine gas was bubbled into the reaction mixture at a rate of 300 ml / min, and the gas flow was continued until brown vapor was generated. Chlorine sparging was stopped and the reaction mixture was transferred to another vessel. In this vessel, the reaction mixture was diluted with 4.0 liters of basic bromine mixture and 0.5 liters of deionized water while keeping the whole under stirring, and stirring was continued for 10 minutes. The solid brominating reagent thus formed having a bromide to bromate ratio of 2:1 was isolated by evaporating the water and drying the product at 70°C by known techniques. The resulting active bromine content was 45.3%.

Embodiment 2

[0054] Add 3.0 liters of an alkaline bromide mixture with a ratio of bromide to bromate of 4.4:1 into a three-necked round-bottomed flask, add 3.5 liters of deionized water containing 26.10 moles of NaOH to the mixture, and stir and mix at 30°C . With the temperature maintained at 30° C., chlorine gas was passed into the reaction mixture at a rate of 300 cc / min, and the chlorine gas was continued until brown vapor was generated. Chlorine sparging was stopped and the reaction mixture was transferred to another vessel. In this vessel, the reaction mixture was diluted with 7.0 liters of basic bromine mixture and 0.5 liters of deionized water while keeping the whole under stirring, and stirring was continued for 10 minutes. The solid brominating reagent thus formed having a bromide to bromate ratio of 2:1 was isolated by evaporating the water and drying the product at 70°C by known techniques. The resulting active bromine content was 50.3%.

Embodiment 3

[0056] Add 3.0 liters of an alkaline bromide mixture with a ratio of bromide to bromate of 4.4:1 into a three-necked round-bottomed flask, add 3.5 liters of deionized water containing 26.10 moles of NaOH to the mixture, and stir and mix at 38°C . With the temperature maintained at 38°C, chlorine gas was bubbled into the reaction mixture at a rate of 300 cc / min, and the gas flow was continued until brown vapor was generated. Chlorine sparging was stopped and the reaction mixture was transferred to another vessel. In this vessel, the reaction mixture was diluted with 7.0 liters of basic bromine mixture and 0.5 liters of deionized water while keeping the whole under stirring, and stirring was continued for 10 minutes. The solid brominating reagent thus formed having a bromide to bromate ratio of 2:1 was isolated by evaporating the water and drying the product at 70°C by known techniques. The resulting active bromine content was 50.3%.

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PUM

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Abstract

A cost-effective process is described for the preparation of a stable and non-hazardous brominating reagent containing 2:1 stoichiometric ratio of alkali bromide to alkali bromate. The process comprises of reacting alkaline bromine intermediate mixture, obtained from bromine recovery plant, with chlorine gas in the presence of a strong alkali to oxidize the bromide ions to bromate ions. This brominating reagent is useful for the bromination of aromatic compounds by substitutions.

Description

field of invention [0001] The present invention relates to an improved process for the preparation of harmless brominating reagents. In particular, the invention relates to a process for the preparation of brominating reagents from basic intermediate bromide-bromate mixtures obtained from bromine recovery plants. The obtained reagent is convenient to handle, non-toxic, easy to transport and can be effectively used to prepare various aromatic bromine compounds. Background of the invention [0002] Liquid bromine is used to prepare a variety of bromides by substitution reactions. These include commercially important products such as i) tetrabromobisphenol A (TBBPA) - a flame retardant, ii) tetrabromofluorescein - a pigment used in human health products, iii) N-acetyl Bromoaniline - an analgesic and antipyretic, iv) tribromophenol - used in the manufacture of antimicrobials, fungicides, fungicides, fire extinguishing fluids, flame retardants, and v) 2-Bromo-4-nitro-N- Acetan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B11/20C01B7/09
CPCC01B7/096C01B11/20
Inventor 拉马钱德拉亚·加德普什皮托·库马尔·高希阿迪穆尔蒂·苏巴拉亚帕阿舒托什·瓦桑特·贝代克尔迪帕克·阿尔万特拉·舒克拉
Owner COUNCIL OF SCI & IND RES
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