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A kind of method that microchannel reactor prepares chlorenyne

A microchannel reactor, chloroenyne technology, applied in chemical instruments and methods, chemical/physics/physicochemical reactors, preparation of carboxylic acid halides, etc. There are hidden dangers in production safety, and the appearance of products is prone to yellowing, etc., to avoid explosive accidents, reduce the generation of by-products, and have a large heat exchange contact surface.

Active Publication Date: 2020-05-26
中山致安化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the synthesis process of chloroalkenes, the requirements for water are high, the reaction control temperature is low, and a large amount of heat is released during the reaction process. If the process control is not good, safety accidents are likely to occur
If the amount of feed to the reactor is large, it will greatly increase the hidden dangers of production safety; at the same time, the fluctuation of the traditional production method is large, and the appearance of the product is prone to yellowing; the crude oil must be crystallized by adding a catalyst again to obtain high-efficiency chloroenyne Raw powder
[0005] So far, there has not been any research on the preparation of chloroalkenes using microchannel reactors

Method used

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  • A kind of method that microchannel reactor prepares chlorenyne
  • A kind of method that microchannel reactor prepares chlorenyne
  • A kind of method that microchannel reactor prepares chlorenyne

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A microchannel reactor (direct current channel module + V-shaped structure module, module material 316 stainless steel) is used, connected according to the drawings in the manual, the number of modules is determined according to the flow rate and reaction residence time, the material is injected into the heat exchange module through a metering pump, and the heat exchange is performed. The medium is heat transfer oil.

[0043] (1) Prepare a mixed solution of pentynyl alcohol and diisopropylamine, mix the pentynyl alcohol and diisopropylamine in toluene, and store them in the raw material tank for later use. The molar ratio of the materials is pentynyl alcohol:diisopropylamine:toluene=1: 0.0001:2.

[0044](2) After the prepared mixed solution enters the heat exchange module with a metering pump for heat exchange, it will be mixed and reacted synchronously with the trans-DV-chrysanthemum acid chloride after entering the heat exchange module 1 through the metering pump in t...

Embodiment 2

[0049] A microchannel reactor (direct current channel module + cone trapezoidal structure module, module material PEEK) is used, connected according to the drawings in the manual, the number of modules is determined according to the flow rate and reaction residence time, the material is injected into the heat exchange module through a metering pump, and the heat exchange medium For heat transfer oil.

[0050] (1) Prepare a mixture of pentynyl alcohol and tetramethylguanidine, mix the pentynyl alcohol and tetramethylguanidine in dichloroethane, store it in a raw material tank for later use, and the molar ratio of the materials is pentynyl alcohol:tetramethylguanidine Guanidine: dichloroethane = 1:0.0005:4.

[0051] (2) After the prepared mixed solution enters the heat exchange module with a metering pump for heat exchange, it is mixed and reacted synchronously with the trans-DV-chrysanthemum acid chloride after entering the heat exchange module through the metering pump, and th...

Embodiment 3

[0056] A microchannel reactor (direct current channel module + cone-trapezoidal structure module, module material Hastelloy alloy) is used, connected according to the drawings in the manual, the number of modules is determined according to the flow rate and reaction residence time, and the material is pumped into the heat exchange module through a metering pump. The heat medium is water.

[0057] (1) Prepare a mixed solution of pentynyl alcohol and diisopropylamine, mix the pentynyl alcohol and diisopropylamine in chloroform, and store them in a raw material tank for later use. The molar ratio of the materials is pentynyl alcohol: diisopropylamine: chloroform =1:0.001:3.

[0058] (2) After the prepared mixed solution enters the heat exchange module with a metering pump for heat exchange, it will react synchronously with the DV-chrysanthemum acid chloride after entering the heat exchange module through the metering pump in the mixing module. The mixing reaction temperature is c...

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PUM

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Abstract

The invention discloses a method for preparing chlorempenthrin with a microchannel reactor. In the microchannel reactor with a specific internal structure, trans DV-chrysanthemoyl chloride and acetylene amyl alcohol are taken as main raw materials which are fed into the microchannel reactor through a metering pump in the presence of an organic solvent and a catalyst, chlorempenthrin crude oil is obtained via preheating, mixing, reacting and aftertreating, and chlorempenthrin raw powder is obtained after the crude oil is subjected to crystallization and drying treatment. The microchannel reactor is adopted, so that the method has the advantages that liquid remaining volume of equipment is low, so that safety in production operation is greatly improved as compared with a traditional reaction kettle taking cube as unit levels; mass transfer rate is high, and reaction time is shortened from several hours to tens of seconds and a few minutes; the heat transfer contact surface is large, heat generated from reaction can be removed in time, explosive accident caused by steep temperature rise can be avoided, byproduct generation in reaction products is reduced, and synthesis stability is high; 4), small size, flexible motion, simpleness and easiness in operation are achieved.

Description

technical field [0001] The invention relates to a method for preparing chloroalkenes in a microchannel reactor. Background technique [0002] Chlorenyne is an important high-efficiency pyrethroid, which is widely used in the deep processing of pyrethroids such as fly incense. Chemical name: 1-ethynyl-2-methylpent-2-enyl-trans-2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropanecarboxylate. [0003] At present, the main production processes of chlorenyne are pyridine method and triethylamine method. Due to the low control of moisture and reaction temperature in the production process, the reaction temperature is -10~10°C, poor control during the reaction is likely to generate by-products, which will affect the quality and yield of the product. Simultaneously, due to the high-temperature instability of pentynyl alcohol, the residual raw materials in the reaction process are not easy to recover, which has an impact on product stability. [0004] The current industrial methods of c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/14C07C69/747B01J19/00
CPCB01J19/0093C07C67/14C07C69/747
Inventor 李国江欧雪盈陈浩瀚罗江
Owner 中山致安化工科技有限公司
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