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Hydrodechlorination method for high chlorine acetone

A technology for hydrodechlorination and high-chlorinated acetone is applied in the field of environmental pollution control and resource utilization, which can solve the problems of complex process, harsh conditions, explosion, etc., and achieves overcoming complex process, mild processing conditions and low cost. Effect

Inactive Publication Date: 2017-07-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are relatively few studies on the treatment of chlorinated acetone residues at home and abroad. Some studies continue to chlorinate the chlorinated acetone residues into hexachloroacetone, and then decompose it to prepare chloroform. However, the process is complicated and the conditions are harsh, and may produce explosion hazard

Method used

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  • Hydrodechlorination method for high chlorine acetone
  • Hydrodechlorination method for high chlorine acetone
  • Hydrodechlorination method for high chlorine acetone

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Get 10mL of perchloracetone residue on a certain folic acid production line in a three-necked flask, add 100mL deionized water to mix, add 0.5g carbon-based hydrogenation catalyst and 0.25g NaOH solid, magnetically stir, and hydrogen (10%H 2 ) into the system, the flow rate is 50mL / min, the reaction temperature is 80-100°C, the reaction is continuous for 6-12 hours, the residue completely disappears, and the water phase product is yellow.

[0031] The product was separated from the carbon-based hydrogenation catalyst, and the aqueous phase was added dropwise with AgNO 3 The solution produces a white precipitate, which proves that there is Cl - produce. After the high chloroacetone residue was extracted with methyl tert-butyl ether, it was monitored by gas chromatography-mass spectrometry and found to contain 1,1,3-trichloroacetone, 1,1,1-trichloroacetone, 1,1,3 ,3-tetrachloroacetone, 1,1,1,3-tetrachloroacetone, pentachloroacetone and hexachloroacetone. Among them, th...

Embodiment 2

[0035] The difference between this embodiment and Example 1 is that the amount of NaOH solid added is 0.5 g, and other reagents added, reaction temperature, and reaction time are the same. After the reaction, the residue disappeared completely, and the aqueous phase product was yellow, and darker than the product obtained in Example 1.

[0036] The product was separated from the carbon-based hydrogenation catalyst, and the aqueous phase was added dropwise with AgNO 3 The solution produces a white precipitate, which proves that there is Cl - produce. After the water phase is extracted with methyl tert-butyl ether, it is monitored by gas chromatography-mass spectrometry. The monitored chloroacetone substances are 1,1,3-trichloroacetone, a small amount of 1,1,3,3-tetrachloroacetone With a very small amount of 1,3-dichloroacetone, the overall reaction of the dechlorination reaction that takes place is the same as in Example 1.

[0037] The content of 1,1,3-trichloroacetone in t...

Embodiment 3

[0039] The difference between this example and Example 1 is that the amount of NaOH solid added is 1.0 g, and other reagents added, reaction temperature, and reaction time are the same. After the reaction, the residue disappeared completely, and the product in the aqueous phase was yellow, and darker than the products obtained in Example 1 and Example 2.

[0040] The product was separated from the carbon-based hydrogenation catalyst, and the aqueous phase was added dropwise with AgNO 3 The solution produces a white precipitate, which proves that there is Cl - produce. After the aqueous phase is extracted with methyl tert-butyl ether, it is monitored by gas chromatography-mass spectrometry. Among the monitored chloroacetone substances are 1,1,3-trichloroacetone, a small amount of 1,1,3,3-tetrachloro Acetone and very small amounts of 1,3-dichloroacetone.

[0041] The content of 1,1,3-trichloroacetone in the product after dechlorination of high-chlorine acetone residue is betw...

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Abstract

The invention discloses a hydrodechlorination method for a by-product, high chlorine acetone residue, produced in a production process of 1,1,3-trichloroacetone according to an acetone chlorination process. The method mainly comprises the following steps: (1) mixing high chlorine acetone residue with water at certain ratio; (2) adding NaOH for regulating the pH value of a mixed solution; (3) introducing H2 into a system for performing dechlorinating reaction under the effect of a carbon-base hydrogenation catalyst; (4) separating a reaction product from the catalyst. According to the invention, the problem of environmental pollution caused by tetrachloroacetone, acetone pentachloride and hexachloroacetone produced in the process of preparing 1,1,3-trichloroacetone through acetone chlorination due to poor reaction selectivity is solved, and meanwhile, 1,1,3-trichloroacetone which is converted from high chlorine acetone residue with hydrogen can be used as a raw material, so that the purpose of recycling is achieved. The method has important research significance and application value in constructing a harmless and recyclable production technology for preparing 1,1,3-trichloroacetone through acetone chlorination.

Description

technical field [0001] The invention relates to a method for hydrogenation and dechlorination of by-product perchloracetone residue produced in the production process of 1,1,3-trichloroacetone prepared by acetone chlorination, and belongs to the field of environmental pollution control and resource utilization. Background technique [0002] 1,1,3-Trichloroacetone is an important chemical raw material, mainly used to produce folic acid. Folic acid, also known as vitamin B9, is the basic variety of vitamins. It is an essential substance when the human body uses sugar and amino acids. It can be reduced to tetrahydrofolate in tissues such as liver, intestinal wall, and bone marrow. Tetrahydrofolate participates in purine nucleic acid in the body Synthesis and transformation of pyrimidine nucleotides. At the same time, folic acid is an indispensable substance for the manufacture of red blood cells. The lack of folic acid in the human body can lead to abnormal red blood cells, an...

Claims

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Application Information

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IPC IPC(8): C07C45/85C07C45/61C07C49/16
CPCY02P20/584C07C45/85C07C45/61C07C49/16
Inventor 余江杜君张婷婷李颖阳李佳璠
Owner BEIJING UNIV OF CHEM TECH
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