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Bronopol refining process

A technology of bronopol and process, which is applied in the field of bronopol refining process and chemical product refining process, can solve the problems of low product yield and waste water pollution, and achieve the effects of content reduction, environmental protection pressure and waste water treatment cost

Active Publication Date: 2017-05-10
河北美邦工程科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the invention is to provide a bronopol refining process, which solves the problem of low product yield and existing waste water pollution in the existing bronopol refining process

Method used

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  • Bronopol refining process

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1 A bronopol refining process comprises the following steps:

[0021] (1) Using conventional methods, nitromethane, formaldehyde and liquid bromine were used to carry out hydroxyalkylation and bromination reactions to obtain 1000L bronopol crude product crystallization liquid, wherein the content of bronopol was 232.5kg / L;

[0022] (2) Distill the 1000L bronopol crude crystallization solution obtained in step (1) under reduced pressure at a temperature of 58°C to obtain bronopol concentrate A, and the distilled water is discharged after biochemical treatment up to standard;

[0023] (3) Add crystallization agent acetonitrile to bronopol concentrated solution A obtained in step (2) for crystallization, keep for 25 minutes, then cool down to 3°C and continue stirring for 55 minutes; then filter and wash to obtain sodium bromide crystals and Contain the bronopol mother liquor B of crystallization agent acetonitrile, sodium bromide crystal is vacuum-dried at 40 D...

Embodiment 2

[0030] Embodiment 2 A bronopol refining process comprises the following steps:

[0031] (1) Using conventional methods ， Utilize nitromethane, formaldehyde and liquid bromine to carry out hydroxyalkylation reaction and bromination reaction to obtain 1000L bronopol crude product crystallization liquid, wherein bronopol content is 240kg / L;

[0032] (2) Distill the 1000L bronopol crude product obtained in step (1) under reduced pressure at a temperature of 65°C to obtain bronopol concentrated solution A, and the distilled water is discharged after biochemical treatment up to standard;

[0033] (3) Add crystallization agent ethanol to the bronopol concentrated solution A obtained in step (2) to crystallize, keep for 26 minutes, then cool down to 2°C and continue stirring for 60 minutes; then filter and wash to obtain sodium bromide crystals and Containing the bronopol mother liquor B of crystallization agent ethanol, the sodium bromide crystal is vacuum-dried at 41 DEG C to obtai...

Embodiment 3

[0040] Embodiment 3 A bronopol refining process comprises the following steps:

[0041] (1) Using conventional methods, use nitromethane, formaldehyde and liquid bromine to carry out hydroxyalkylation and bromination reactions to obtain 1000L bronopol crystallization liquid, wherein the content of bronopol is 235kg / L;

[0042] (2) Distill the 1000L bronopol crude product obtained in step (1) under reduced pressure at a temperature of 60°C to obtain bronopol concentrated solution A, and the distilled water is discharged after biochemical treatment up to standard;

[0043] (3) Add 235L crystallization agent methyl formate to the bronopol concentrated solution A obtained in step (2) for crystallization, stir while crystallizing, keep for 30min, then cool down to 1°C and keep stirring for 65min; then filter, After washing, sodium bromide crystals and bronopol mother liquor B containing crystallizer methyl formate were obtained, and the sodium bromide crystals were vacuum-dried at ...

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Abstract

The invention discloses a bronopol refining process. The process comprises the following steps: performing reduced pressure distillation on a bronopol crude product crystalline liquid prepared by a conventional method to obtain a concentrate, adding crystallization agent into the concentrate, and crystallizing to obtain a sodium bromide product; further distilling the mother solution, adding pure water, and crystallizing to obtain a bronopol product; and performing resin adsorption on the residual bronopol in the obtained mother solution, resolving, and returning to the bronopol crude product crystalline liquid, wherein in the whole technical process, no loss of bronopol exists, and wastewater is directly subjected to biochemical treatment. According to the invention, sodium bromide and bronopol products with purities of 99% or above can be obtained, and the yield of the bronopol is more than 99%.Compared with the existing one-step reduced pressure distillation and crystallization process, the bronopol refining process increases the bronopol yield and lowers the bronopol and sodium bromide contents in wastewater, so that the wastewater can be directly discharged into a biochemical system, thereby lowering the wastewater treatment cost and reducing environmental pollution.

Description

technical field [0001] The invention relates to a process for refining chemical products, in particular to a process for refining bronopol, and belongs to the technical field of fine chemicals. Background technique [0002] Bronopol, chemical name: 2-bromo-2-nitro-1,3-propanol, also known as bronopol, 2-nitro-2-1,3-propanediol, 2-bromo- 2-Nitro-1,3-propanediol (Bropol), Pi Le Bao, etc. Soluble in acetone, 2-methoxyethanol, toluene and other organic solvents, the purity of industrial products is higher than 90%, and it is slightly hygroscopic. Bronopol is a new type of bactericidal preservative, mainly used in cosmetics and leather antisepsis. It is used as a fungicide in agriculture and medicine. It is also a broad-spectrum and efficient industrial fungicide, which is used to prevent the growth and reproduction of bacteria and algae in papermaking, industrial circulating cooling water, lubricating oil for metal processing, pulp, wood, paint and plywood. It is widely used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/26C07C201/16C07C201/12
CPCC07C201/12C07C201/16C07C205/26
Inventor 卢远峰吕志刘东闫利军魏朝帅王素霞
Owner 河北美邦工程科技股份有限公司
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