Synthetic method for bronopol

A synthesis method and bronopol technology are applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effects of easy reaction process, avoidance of explosion, and improved synthesis yield

Inactive Publication Date: 2015-09-23
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the invention is to solve the shortcoming that exists in the existing bronopo...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 130.0g (1.6mol) of 37% formaldehyde, 64.0g methanol, 90.6g (0.88mol) sodium bromide, and 80.0g deionized water into a 500ml four-necked flask, cool down to 10°C with an ice-salt bath while stirring, and add 15.0 g (0.15 mol) of 40% sodium hydroxide solution, adjust the pH of the solution to 13, start adding 48.8 g (0.80 mol) of nitromethane dropwise, control the condensation reaction temperature -4-10°C, and continue stirring when the solution temperature drops to 10°C The condensation reaction was complete in 10 minutes. Then 65.0 g (0.65 mol) of 40% sodium hydroxide solution was added dropwise, and the neutralization reaction temperature was controlled at 20-30°C. When the temperature stopped rising, the neutralization reaction was completed. Cool the reactant to 0-4°C under stirring, then introduce about 56.8g (0.80mol) of chlorine gas under stirring to carry out the bromination reaction, and control the rate of chlorine gas introduction to make the solution ligh...

Embodiment 2

[0028] Add 130.0g (1.6mol) of 37% formaldehyde, 100.0g methanol, 94.8g (0.92mol) sodium bromide, and 100.0g deionized water into a 500ml four-necked flask, and cool down to -4-0 with an ice-salt bath while stirring. ℃, add 15.0 g (0.15 mol) of 40% sodium hydroxide solution, adjust the pH of the solution to 13, start adding 48.8 g (0.80 mol) of nitromethane dropwise, and control the condensation reaction temperature -4-0 ℃, when the solution temperature drops to 0 ℃ Then continue to stir for 30 minutes and the condensation reaction is completed. Then 65.0 g (0.65 mol) of 40% sodium hydroxide solution was added dropwise, and the neutralization reaction temperature was controlled at 0-10°C. When the temperature no longer rose, the neutralization reaction was completed. Cool the reactant to -4-0°C under stirring, then introduce about 56.8g (0.80mol) of chlorine gas under stirring to carry out the bromination reaction, and control the rate of chlorine gas feeding to make the soluti...

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PUM

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Abstract

The invention discloses a synthetic method for bronopol. The synthetic method comprises the following steps: under an alkaline condition, condensing nitromethane and formaldehyde to generate 2-nitryl propylene glycol; then, synthesizing bronopol by virtue of a bromination route. The synthetic method is characterized in that bromine is generated by carrying out in-situ oxidization on sodium bromide in a reaction liquid by chlorine gas to replace a mode of directly adding bromine into 2-nitryl propylene glycol salt to synthesize the bronopol. According to the method, a bromine raw material which is liable to volatilize and strong in corrosion is not used, the synthetic reaction conditions are stable, the reaction process is easy to control, and the synthetic yield is increased.

Description

technical field [0001] The invention relates to a synthesis method of bronopol, in particular to a method for synthesizing bronopol by replacing bromine with chlorine gas, which belongs to the field of fine chemical industry. Background technique [0002] Bronopol (English Bronopol), chemical name 2-bromo-2-nitro-1,3 propanediol, common name Bronopol, bacteriostatic alcohol, Pi Lebao, etc. The pure product of bronopol is a white crystalline powder with a melting point of 130°C. It is easily soluble in water, ethanol, and propylene glycol, but hardly soluble in chloroform, acetone, and benzene. Bronopol is a new type of bactericidal preservative, mainly used as a cosmetic preservative, and as a bactericide in pesticides and medicines. Since the 1990s, bronopol has been popularized and applied in feed antiseptic, air-conditioning circulating water antibacterial, oilfield water antibacterial and slime prevention, vehicle and ship disinfection, etc., and the demand has grown r...

Claims

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Application Information

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IPC IPC(8): C07C205/26C07C201/12
Inventor 李建生李霞张成昊
Owner TIANJIN VOCATIONAL INST
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