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
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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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