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Synthesis of chloroacetic acid

A technology of chloroacetic acid and acetic acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as slow reaction speed, and achieve the effect of improving speed and selectivity

Inactive Publication Date: 2007-01-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using activated carbon alone as a cocatalyst cannot fundamentally inhibit the generation of dichloroacetic acid, and the reaction rate is also relatively slow, because the chlorination reaction of acetic acid is an acid-catalyzed reaction, which can only be fundamentally improved under the appropriate acid catalysis. Reaction selectivity and reaction speed

Method used

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  • Synthesis of chloroacetic acid
  • Synthesis of chloroacetic acid

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Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0014] Add 25ml of glacial acetic acid and 2.5ml of acetic anhydride to a homemade 50ml hard glass chlorination reactor, and add solid super acid SO 4 2- / 1.5%Cr / Fe 2 o 3 Cocatalyst 0.2g, chlorine gas reaction at 100°C, it is advisable to control the chlorine gas speed with a slight excess of chlorine gas, after 6 hours the reaction ends, and the composition of the reaction solution is: chloroacetic acid 95.3%, dichloroacetic acid 3.0%, acetic acid 1.7% %.

Embodiment approach 2

[0016] Add 25ml of glacial acetic acid and 2.5ml of acetic anhydride to the above chlorination reactor, and add solid super acid SO 4 2- / 0.5%Mn / Fe 2 o 3Co-catalyst 0.4g, react with chlorine gas at 115°C, it is advisable to control the rate of chlorine gas with a slight excess of chlorine gas, the reaction ends after 6 hours, and the composition of the measured reaction solution is: 93.4% of chloroacetic acid, 3.8% of dichloroacetic acid, 2.8% of acetic acid %.

Embodiment approach 3

[0018] Add 25ml of glacial acetic acid and 3.0ml of acetic anhydride to the above chlorination reactor, and add solid super acid SO 4 2- / 2.0%Sn / Fe 2 o 3 Co-catalyst 0.3g, activated carbon 1.5g, react with chlorine gas at 105°C, control the rate of chlorine gas with a slight excess of chlorine gas, the reaction ends after 6 hours, and the composition of the measured reaction solution is: chloroacetic acid 96%, dichloroacetic acid 3.2 %, acetic acid 0.8%.

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Abstract

Synthesis of chloroacetic acid is characterized by taking acetic anhydride as catalyst, and taking SO42- / MxOy or SO42- / MxOy-C, S2O82- / MxOy or S2O82- / MxOy-C as auxiliary catalyst. It adopts acetic acid chlorine gas chlorinating method. MxOy can be ZrO2, or TiO2, or Fe2O3, or Cr2O3, or MnO2, or Sn2O3, or WO3, or MoO3, or can be mixture of them. It achieves higher reacting speed, shorter reacting time, and less content of by-products.

Description

1. Technical field: [0001] The invention discloses a method for synthesizing chloroacetic acid, which belongs to the field of organic synthesis and catalysis science. 2. Background technology: [0002] Chloroacetic acid is an important organic chemical intermediate. It is no longer a fine chemical product traditionally defined. In recent years, the world's total consumption has exceeded 600,000 tons, and China's total consumption has also exceeded 100,000 tons. It is a synthetic dye , pesticides, pharmaceuticals, spices, oilfield chemicals, paper chemicals, textile auxiliaries, surfactants and other important raw materials. At present, there are two main industrial production methods of chloroacetic acid: one is the hydrolysis of trichloroethylene, and the other is the chlorination of acetic acid. The former can obtain high-purity chloroacetic acid, but the consumption of raw materials is large, the process is long, and the cost is high; the latter has a simple synthesis pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/16C07C51/363
Inventor 李福祥吴岚吕志平薛建伟
Owner TAIYUAN UNIV OF TECH