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Method for purifying trichloracetic aldehyde waste sulfuric acid

A technology of trichloroacetaldehyde and waste sulfuric acid, applied in sulfur trioxide/sulfuric acid, chemical instruments and methods, organic chemistry, etc., can solve the problems of harsh operating conditions, large water addition, high energy consumption, etc., and achieve low treatment cost, The effect of large production volume and simple process

Inactive Publication Date: 2015-04-08
NANNING CHEMICAL INDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the existing research, a single extraction, distillation or adsorption technology is generally used, and there are many problems such as large water addition, high energy consumption, low dealdehyde effect, harsh operating conditions and secondary pollution, making it difficult to realize industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 40mL of chloral aldehyde waste sulfuric acid with a chloral concentration of 20mg / mL in a packed tower, feed 100mL / min of carbon dioxide, and at 25°C, the chloral concentration of 20mg / mL waste sulfuric acid The chloral is desorbed for 3 hours, and the desorption gas is passed into the packed tower to react with 30% dimethyl phosphite aqueous solution at 50°C to obtain trichlorfon, and the tail gas passes through an absorption pool with water as the absorption liquid. emptying. After desorption, the aldehyde content of waste sulfuric acid is 468ppm, and the aldehyde content of discharged water is 15ppm.

Embodiment 2

[0018] Put 40mL of chloral waste sulfuric acid with a chloral concentration of 20mg / mL in a packed tower, feed 300mL / min of air, and desorb the chloral in the waste sulfuric acid at 45°C for 3.5h, The desorption gas is passed into the packed tower to react with 60% dimethyl phosphite solution at 60°C to obtain trichlorfon, and the tail gas is then emptied after passing through an absorption pool with water as the absorption liquid. After desorption, the aldehyde content of the waste sulfuric acid was 18 ppm, and the aldehyde content of the discharged water was 11 ppm.

Embodiment 3

[0020] Put 40mL of chloral waste sulfuric acid with a chloral concentration of 20mg / mL in a packed tower, feed 500mL / min of nitrogen, and desorb the chloral in the waste sulfuric acid at 55°C for 4.0h, The desorption gas is passed into the packed tower to react with 80% dimethyl phosphite solution at 25°C to obtain trichlorfon, and the tail gas is then emptied after passing through an absorption pool with water as the absorption liquid. After desorption, the aldehyde content of the waste sulfuric acid was 16 ppm, and the aldehyde content of the discharged water was 17 ppm.

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PUM

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Abstract

The invention discloses a method for purifying trichloracetic aldehyde waste sulfuric acid. The method comprises the following steps: introducing air into the trichloracetic aldehyde waste sulfuric acid for desorbing trichloracetic aldehyde from the waste sulfuric acid; then, introducing a desorbing gas mixture into dimethyl phosphate for reacting the trichloracetic aldehyde with the dimethyl phosphate to generate trichlorfon (O,O-dimethyl-(2,2,2-trichlorine-1-hydroxyl ethyl)phosphonate). The method disclosed by the invention is simple in process and can be used for effectively removing harmful substance trichloracetic aldehyde in the trichloracetic aldehyde waste sulfuric acid to obtain byproduct trichlorfon, and recycling the waste sulfuric acid.

Description

technical field [0001] The invention belongs to a method for purifying waste produced in the production process of chloral, in particular to a method for purifying chloral waste sulfuric acid. Background technique [0002] Chloral is an important pesticide intermediate and the main raw material of trichlorfon, a backbone pesticide necessary for agricultural production. my country's chloral production currently adopts the process route of multi-stage ethanol chlorination and concentrated sulfuric acid dehydration, and a large amount of waste sulfuric acid containing organic impurities such as chloral (acid) will be produced in the production process. The concentration of waste sulfuric acid is 60% to 70%, and the content of organic impurities is 4% to 15%, mainly trichloroacetaldehyde and trichloroacetic acid. Because chloral (acid) can destroy the polar structure and differentiation of plant protoplasm, and make the nucleus division disorder. After the use of phosphate fert...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C01B17/90
Inventor 秦祖赠覃卫国陈军龙锋
Owner NANNING CHEMICAL INDUSTRY CO LTD