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Preparation method of dichloramine T or dichloramine B

A technology of dichloramine and chlorine gas is applied in the preparation of sulfonic acid amide, the preparation of organic compounds, chemical instruments and methods, etc., to achieve the effects of short process reaction time, stable quality and low price

Pending Publication Date: 2022-05-24
SHOUGUANG NUOMENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there is no report on the relevant production process in China

Method used

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  • Preparation method of dichloramine T or dichloramine B
  • Preparation method of dichloramine T or dichloramine B
  • Preparation method of dichloramine T or dichloramine B

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 86.04g of p-toluenesulfonamide (content 99.5%, 0.5mol), 136.7g of 30%wt sodium hydrogen hydride solution into a 500ml four-neck flask, stir and dissolve, cool down to 10°C in a water bath, and add 74.6g of chlorine gas (99.95% chlorine gas content ) into a four-necked bottle (the molar ratio of the reaction materials is 1:2.05:2.1), the temperature is controlled at 10°C for about 3 hours, the pH value is detected at 10-11, and the first stage of chlorine flow is completed; add 4.3 grams of catalyst sodium acetate (for The mass ratio of toluenesulfonamide: sodium acetate = 1:0.05), continue to feed the remaining chlorine gas, control the temperature at 10°C, and pass chlorine for about 3 hours. The detected pH value is less than 4, and the reaction is complete. Naturally raise the temperature to about 30°C, add 60 grams of dichloromethane, dissolve and extract, let the material dissolve and separate into layers, separate the brine layer, cool the material liquid to 0°...

Embodiment 2

[0026] Add 86.04g of p-toluenesulfonamide (content 99.5%, 0.5mol), 140g of 30%wt sodium hydrogen hydride solution into a 500ml four-necked bottle, stir and dissolve, cool down to 10°C in a water bath, and add 78.14g of chlorine gas (99.95% of chlorine gas content) Pass it into a four-necked bottle (the molar ratio of the reaction materials is 1:2.1:2.2), control the temperature at 10°C for about 3 hours, check the pH value of 10-11, and complete the first stage of chlorine passage; add 3.44 grams of catalyst sodium acetate (p-toluene The mass ratio of sulfonamide: sodium acetate = 1:0.04), continue to feed the remaining chlorine gas, control the temperature at 10°C, and pass the chlorine for about 3 hours. The detected pH value is less than 4, and the reaction is completed. Naturally raise the temperature to about 30°C, add 60 grams of dichloromethane, dissolve and extract, let the material dissolve and separate into layers, separate the brine layer, cool the material liquid to...

Embodiment 3

[0028] Add 86.04g of p-toluenesulfonamide (content 99.5%, 0.5mol), 136.7g of 30%wt sodium hydrogen hydride solution into a 500ml four-neck flask, stir and dissolve, cool down to 10°C in a water bath, and add 74.6g of chlorine gas (99.95% chlorine gas content ) into a four-necked bottle (the molar ratio of the reaction materials is 1:2.05:2.1), the temperature is controlled at 10°C for about 3 hours, the pH value is detected at 10-11, and the first stage of chlorine flow is completed; add 4.3 grams of catalyst sodium acetate (for The mass ratio of toluenesulfonamide: sodium acetate = 1:0.05), continue to feed the remaining chlorine gas, control the temperature at 10°C, and pass chlorine for about 3 hours. The detected pH value is less than 4, and the reaction is complete. Naturally raise the temperature to about 30°C, add 60 grams of dichloromethane, dissolve and extract, let the material dissolve and let it stand for stratification, separate the brine layer, cool the material l...

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Abstract

The invention belongs to the technical field of chemical production, and particularly relates to a preparation method of dichloramine T or dichloramine B. The preparation method comprises the following steps: (1) substitution reaction: mixing p-toluene sulfonamide or benzenesulfonamide with a sodium hydroxide solution, heating and dissolving, introducing chlorine, and carrying out substitution reaction; (2) dissolving and extracting: adding dichloromethane for dissolving and extracting, and standing for layering to form a salt water layer and a feed liquid layer; and (3) refining: cooling and crystallizing a feed liquid layer, centrifuging and drying. The method is wide in raw material source, low in price and short in process reaction time, after the reaction, sodium chloride brine is extracted and separated from the materials through the solvent, then recrystallization is conducted in the solvent, the materials and impurities can be thoroughly separated, the product content is high, the available chlorine content can reach 58% or above, the yield can reach 97% or above, and through the recrystallization process, the product purity is high. And the crystallized product is not easy to decompose, long in preservation time and stable in quality.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a preparation method of dichloramine T or dichloramine B. Background technique [0002] Dichloramine T and Dichloramine B are disposable disinfectants for external use, which can kill bacteria, viruses, fungi and spores, and are also important organic chemical intermediates. [0003] At present, there is no report on the relevant production process in China. Contents of the invention [0004] The purpose of the present invention is to provide a short reaction time, high yield, low cost, environmental protection, the preparation method of dichloramine T or dichloramine B with stable product quality, to solve the problems raised in the above-mentioned background technology. [0005] In order to achieve the above-mentioned technical purpose, technical scheme of the present invention: [0006] A preparation method of dichloramine T or dichloramine B, compr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/36C07C311/48C07C303/44
CPCC07C303/36C07C303/44C07C311/48
Inventor 李庆山胡新河刘在成张光
Owner SHOUGUANG NUOMENG CHEM
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