High-selectivity 2-methyl allyl chloride synthesis method and synthesis reactor

A synthesis reactor and synthesis reaction technology, applied in chemical/physical/physicochemical reactors, chemical methods for reacting gaseous media with gaseous media, chemical instruments and methods, etc., can solve many side reactions, low selectivity, Unable to control the temperature and other problems, to achieve the effect of stable reaction process, improved reaction efficiency and high reaction selectivity

Active Publication Date: 2018-06-15
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The disadvantage of the above-mentioned chlorination technology is that there is no cooling surface in the reaction place, and the temperature cannot be controlled. Therefore, there are many side reactions, low selectivity, and the nozzle or nozzle will be blocked due to coking due to excessive chlorination.
[0010] Aiming at the problem that the nozzle is easy to coke, CN202044960 proposes to use a flat nozzle in the utility model patent, and at the same time remove the heat of reaction by circulating the chlorination reactant directly in contact with the reaction gas to cool, but the patent does not provide examples to prove the solution The problem of coking has been solved, and there is no example to prove that the product content in the reaction solution has reached 88%.

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  • High-selectivity 2-methyl allyl chloride synthesis method and synthesis reactor
  • High-selectivity 2-methyl allyl chloride synthesis method and synthesis reactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] in such as figure 1 The microchannel reactor shown (the channel diameter is 0.2mm, and the heat exchange area calculated according to the actual reaction volume is 20000m 2 / m 3 ) into isobutene and chlorine respectively, by adjusting and controlling the flow of isobutene and chlorine, the reaction residence time reaches 1 second, the molar ratio of isobutene to chlorine is 1.005:1, and the reaction temperature is controlled by freezing brine to 0°C. After stable operation for 30 minutes, the composition of the liquid product was sampled and analyzed from the outlet of the reactor, and its mass content was: 2-methallyl chloride was 89.6%, chloro-tert-butane 2.3%, isobutenyl chloride 1.3%, dichloro-tert- Butane 5.6%, dichloroisobutene 1.2%; the selectivity of 2-methallyl chloride is calculated as 91.4%.

Embodiment 2

[0036] in such as figure 1 The shown microchannel reactor (the channel diameter is 0.5mm, and the heat exchange area calculated according to the actual reaction volume is 8000m 2 / m 3 ) into isobutene and chlorine respectively, by adjusting and controlling the flow of isobutene and chlorine, the reaction residence time reaches 0.1 second, the molar ratio of isobutene and chlorine is 1.02:1, and the reaction temperature is controlled by low temperature water to 30°C. After stable operation for 30 minutes, the composition of the liquid product was sampled and analyzed from the outlet of the reactor, and its mass content was: 2-methallyl chloride was 88.7%, chloro-tert-butane 2.1%, isobutenyl chloride 1.5%, dichloro-tert- Butane 6.0%, dichloroisobutene 1.5%; the selectivity of 2-methallyl chloride is 90.5%.

Embodiment 3

[0038] in such as figure 1 The shown microchannel reactor (the channel diameter is 0.4mm, and the heat exchange area calculated according to the actual reaction volume is 10000m 2 / m 3 ) into isobutene and chlorine respectively, by adjusting and controlling the flow of isobutene and chlorine, the reaction residence time reaches 0.5 seconds, the molar ratio of isobutene and chlorine is 1.01:1, and the reaction temperature is controlled by freezing brine to 10°C. After stable operation for 30 minutes, the composition of the liquid product was sampled and analyzed from the outlet of the reactor, and its mass content was: 2-methallyl chloride was 89.3%, chloro-tert-butane 2.3%, isobutenyl chloride 1.4%, dichloro-tert- Butane is 5.7%, dichloroisobutene is 1.3%, and the selectivity of 2-methallyl chloride is calculated to be 91.1%.

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Abstract

The invention relates to a high-selectivity 2-methyl allyl chloride synthesis method and a synthesis reactor. Isobutene and chlorine are taken as the raw materials to have a gaseous phase chlorinationreaction in a microchannel reactor with a cooling surface to obtain the 2-methyl allyl chloride. The isobutene and the chlorine are reacted in the T-shaped microchannel reactor, the mixing speed is quite fast, meanwhile, the huge heat exchange area in the unit reaction volume guarantees the stable reaction at the basically constant temperature, the controllability is good; therefore, the side reaction caused by too high local temperature is effectively inhibited, the reaction selectivity is high, and no phenomenon of coking is caused.

Description

technical field [0001] The invention relates to the chlorination reaction and equipment of organic matter, and belongs to the field of organic synthesis reaction. Background technique [0002] 2-Methyl-3-chloroallyl is an important intermediate in organic synthesis, widely used in medicine, pesticides, spice monomers, polymer materials and other fields. [0003] 2-Methyl-3-chloroallyl is usually obtained by gas-phase chlorination of isobutylene with chlorine. [0004] The early chlorination reaction is carried out in a tubular reactor with a cooling jacket. The reaction temperature is below 100°C, the pressure is normal pressure, and the reaction residence time is in the range of 0.5 seconds to several seconds. In order to avoid deep chlorination side reactions, It is usually necessary to maintain an excess of isobutene, and the two raw materials are injected into the reaction tube by injection. [0005] In order to avoid temperature fluctuations in the reaction process, D...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/067C07C17/10
CPCC07C17/10C07C21/067C07C17/06B01J19/0093B01J2219/00792B01J2219/00873B01J2219/00869B01J12/00B01J19/2415B01J19/2425B01J2219/00094B01J2219/00247
Inventor 尹红陈志荣王新荣王伟松余渊荣王胜利王月芬马振强赵兴军钱建芳
Owner ZHEJIANG UNIV
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