Technology and device for preparing chloroacetic acid through catalytic chlorination by means of micro-channel reactor

A microchannel reactor, chloroacetic acid technology, applied in the field of chloroacetic acid, can solve the problems of high equipment investment, high operating cost, easy generation of temperature difference, etc., and achieve the effects of improving reaction efficiency, reducing operating cost, and reducing difficulty

Active Publication Date: 2018-10-12
山东民基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the investment in batch production equipment is small, but the by-products are more and energy-consuming; while the continuous production technology is expensive to introduce, equipment investment is high, and operating costs are high, but the product quality is high and stable.
[0003] However, the current continuous production technology also has defects, such as local temperature differences are easy to occur, and when the concentration of chlorine gas is too high, it often leads to the production of the main by-product dichloroacetic acid, resulting in low product yield and low product purity.

Method used

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  • Technology and device for preparing chloroacetic acid through catalytic chlorination by means of micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 500kg of acetic acid and 65kg of acetic anhydride into the mixer for pretreatment for 15 minutes to form a mixed solution, then mix the mixed solution with 590kg of liquid chlorine in the pipeline before the precatalytic tank, and enter the inner wall with a solid acid catalyst SO4 2- / ZrO 2 -Eu 2 o 3 The pre-catalytic reaction is carried out in the pre-catalytic tank; the pre-catalytic tank is controlled at normal pressure, the temperature is 75°C, and the reaction residence time is 10s; the solid acid catalyst SO4 on the inner wall of the pre-catalytic tank 2- / ZrO 2 -Eu 2 o 3 The thickness of the coating was 5 mm.

[0031] Then enter the inner wall of the microchannel with solid acid catalyst SO4 2- / ZrO 2 -Eu 2 o 3 Catalytic chlorination reaction is carried out in the microchannel reactor to obtain the chloroacetic acid reaction solution; the microchannel reaction system is controlled at a pressure of 0.35MPa, a temperature of 90°C, and a reaction resid...

Embodiment 2

[0034] Put 500kg of acetic acid and 42kg of acetic anhydride into the mixer for pretreatment for 10 minutes to form a mixed solution, then mix the mixed solution with 620kg of liquid chlorine in the pipeline before the precatalytic tank, and enter the inner wall with a solid acid catalyst SO4 2- / ZrO 2 -Eu 2 o 3 The pre-catalytic reaction is carried out in the pre-catalytic tank; the pre-catalytic tank is controlled at normal pressure, the temperature is 50°C, and the reaction residence time is 100s; the solid acid catalyst SO4 on the inner wall of the pre-catalytic tank 2- / ZrO 2 -Eu 2 o 3 The thickness of the coating was 7 mm.

[0035] Then enter the inner wall of the microchannel with solid acid catalyst SO4 2- / ZrO 2 -Eu 2 o 3 Catalytic chlorination reaction is carried out in the microchannel reactor to obtain the chloroacetic acid reaction solution; the microchannel reaction system is controlled at a pressure of 0.4MPa, a temperature of 80°C, and a reaction resid...

Embodiment 3

[0038] Put 500kg of acetic acid and 80kg of acetic anhydride into the mixer for pretreatment for 20 minutes to form a mixed solution, then mix the mixed solution with 610kg of liquid chlorine in the pipeline before the precatalytic tank, and enter the inner wall with a solid acid catalyst SO4 2- / ZrO 2 -Eu 2 o 3 The pre-catalytic reaction is carried out in the pre-catalytic tank; the pre-catalytic tank is controlled at normal pressure, the temperature is 60°C, and the reaction residence time is 50s; the solid acid catalyst SO4 on the inner wall of the pre-catalytic tank 2- / ZrO 2 -Eu 2 o 3 The thickness of the coating was 6 mm.

[0039] Then enter the inner wall of the microchannel with solid acid catalyst SO4 2- / ZrO 2 -Eu 2 o 3 Catalytic chlorination reaction is carried out in the microchannel reactor to obtain the chloroacetic acid reaction solution; the microchannel reaction system is controlled at a pressure of 0.3MPa, a temperature of 95°C, and a reaction reside...

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Abstract

The invention relates to chloroacetic acid,in particular to a technology and device for preparing chloroacetic acid through catalytic chlorination by means of a micro-channel reactor. The technology comprises the following steps that acetic acid and acetic anhydride are pretreated to form a mixed solution,the mixed solution and liquid chlorine are mixed in a pipeline in front of a pre-catalytic tank,and the mixture enters the pre-catalytic tank with a solid acid catalyst SO42-/ZrO2-Eu2O3 attached to the inner wall; then the mixture enters the micro-channel reactor with a solid acid catalyst SO42-/ZrO2-Eu2O3 attached to the inner wall of a micro channel,reaction is carried out,and chloroacetic acid reaction liquid is obtained; after gas-liquid separation,a chloroacetic acid product is evaporated out. According to the technology,solid superacid SO42-/ZrO2-Eu2O3 is attached to the inner wall of the pre-catalytic tank and the inside of the micro channel of the micro-channel reactor,the reaction efficiency is improved,the consumption of chlorine is reduced,the difficulty of subsequent treatment is reduced,and the operation cost is reduced.

Description

technical field [0001] The invention relates to chloroacetic acid, in particular to a process and a device for preparing chloroacetic acid by catalytic chlorination of a microchannel reactor. Background technique [0002] Chloroacetic acid is an important fine chemical intermediate, which is widely used in pesticides, medicines, dyes, daily chemicals, chemical reagents, food additives and other fields. The existing production processes of chloroacetic acid mainly include trichlorethylene hydrolysis method, chloroacetyl chloride method and acetic acid catalytic chlorination method, among which the acetic acid catalytic chlorination method is the most convenient and widely used, and the acetic acid catalytic chlorination method is divided into batch method production and continuous production. Among them, the investment in batch production equipment is small, but the by-products are more and energy-intensive; while the continuous production technology is expensive to introduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/363C07C53/16
CPCC07C51/363C07C53/16
Inventor 韦兵张海朋李建军王建芹杨中原祝新涛张瑞扈世琳李萍林苗苗
Owner 山东民基新材料科技有限公司
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