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Improved method for synthesizing bronopol

A synthesis method and bronopol technology are applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve the problems of high production cost, easy explosion of nitro compounds, and safety, and achieve low consumption. , the effect of avoiding the explosion of nitro compounds

Inactive Publication Date: 2008-06-18
TIANJIN VOCATIONAL INST
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0009] With the shortcoming of above two kinds of methods synthesis bronopol one, raw material bromine consumption is many, and production cost height;

Method used

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  • Improved method for synthesizing bronopol
  • Improved method for synthesizing bronopol

Examples

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Effect test

Embodiment 1

[0021] Add 130.0g of 37% formaldehyde, 64.0g of methanol, and 80.0g of deionized water into a 500ml four-necked flask, cool down to below 4°C with an ice-salt bath under stirring, add 15.0g (0.15mol) of 40% sodium hydroxide solution, 48.8 g (0.80 mol) of nitromethane was added dropwise, and the condensation reaction temperature was controlled at 4-10° C. When the solution temperature dropped to 4° C., stirring was continued for 10 minutes to complete the condensation reaction. Then 65.0 g (0.65 mol) of 40% sodium hydroxide solution was added dropwise, and the neutralization reaction temperature was controlled at 4-20° C., and the neutralization reaction was completed when the temperature no longer rose. Under stirring, the reactant was further cooled to below -4°C, and then 67.2g (0.42mol) of bromine was added dropwise, and the reaction temperature was controlled at -4-0°C. When the bromine color faded, the bromination reaction was completed by 50%-55%. Then feed about 27.0 g ...

Embodiment 2

[0024] Add 48.8 g (0.80 mol) of nitromethane and 440 g of deionized water into a 500 ml four-necked flask, cool down to below 4°C with an ice-salt bath under stirring, and add 80.0 g (0.80 mol) of 40% sodium hydroxide solution dropwise, The reaction temperature is controlled at 4-20° C., and the neutralization reaction is completed when the reaction temperature no longer rises. Under stirring, it was further cooled to below -4°C, then 67.2g (0.42mol) of bromine was added dropwise, and the reaction temperature was controlled at -4-0°C. When the color of bromine faded away, the bromination reaction was 50% complete. Then feed about 27.0 g (0.38 mol) of chlorine gas to continue the bromination reaction, and the chlorination process ends when the pH value of the reaction solution becomes acidic. The reaction solution was steam-distilled to separate the organic phase to obtain 112.0 g of bromonitromethane product. According to gas chromatography analysis, the bromonitromethane prod...

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Abstract

Theoretic dosage of 50-percent of bromine is dropped into the sodium hydroxide solution of nitromethane or 2-nitro propylene glycol; firstly, 50-55 percent of raw material is bromized to achieve bromonitromethane or 2-bromine-2-nitro propylene glycol; then, chlorine gas is injected into the reaction fluid under -5-20 DEG C and normal pressure to transform the sodium bromide byproduct into bromine, the produced bromine bromizes all the raw materials, and the 2-chlorine-2- nitro propylene glycol impurity in the achieved bronopol is 0.06-0.2 percent. The method only consumes 50 percent of bromine needed by the traditional method; thereby, the explosion of nitro compound is avoided during sodium bromide concentration and reclamation, and the production cost is largely reduced. The product can be applied to cosmetics, pesticides, medicines and universal bactericides for water treatment.

Description

technical field [0001] The invention relates to an improved synthesis method of bronopol, in particular to a method for synthesizing bronopol with half the amount of bromine using bromine chloride. Background technique [0002] The chemical name of bronopol is 2-bromo-2-nitropropanediol, which is a new type of broad-spectrum fungicide. In the past, bronopol was mainly used as a fungicide in cosmetics, pesticides, and medicines. In recent years, it has been used as a fungicide in feed, paint, and fur, antibacterial in air-conditioning circulating water, antibacterial in oilfield water and prevention of slime, toilet disinfection in airplanes, vehicles, and ships, etc. It has been widely used and its demand is growing rapidly. [0003] A synthetic route of bronopol is that formaldehyde and nitromethane are condensed under alkaline conditions to generate 2-nitropropanediol, then neutralized with sodium hydroxide to generate 2-nitropropanediol sodium salt, and then brominated t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/26C07C201/12
Inventor 李建生吕平吴静
Owner TIANJIN VOCATIONAL INST
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