Method for preparing 1-(1-chlorocyclopropyl)ethanone by using micro-channel reactor

A micro-channel reactor and channel reactor technology, which are applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, carbon-based compound preparation, etc. and other problems, to achieve the effect of improving the conversion rate of raw materials and product yield, reducing the generation of by-products, and reducing the incidence of tar

Inactive Publication Date: 2019-09-20
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the batch production in the batch reactor is adopted. The batch reactor needs auxiliary operations such as loading and unloading, and the product quality is not easy to stabilize. Many, obvious amplification effect and other disadvantages
In addition, the time required for the synthesis in the reactor is longer, which will cause the synthesized 1-(1-chlorocyclopropyl)ethanone to stay in an alkaline environment for too long, and produce by-products, resulting in severe coking
[0007] In addition, due to the complexity of the cyclization reaction, there are many influencing factors. At low temperature, the main product is α-chlorocyclopentanone, and tar will be produced at high temperature. Therefore, the reaction process must be strictly controlled.
[0008] At present, the preparation method of 1-(1-chlorocyclopropyl)ethanone is single, and the microchannel reactor is rarely applied to the preparation of 1-(1-chlorocyclopropyl)ethanone

Method used

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  • Method for preparing 1-(1-chlorocyclopropyl)ethanone by using micro-channel reactor
  • Method for preparing 1-(1-chlorocyclopropyl)ethanone by using micro-channel reactor
  • Method for preparing 1-(1-chlorocyclopropyl)ethanone by using micro-channel reactor

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Experimental program
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Effect test

Embodiment 1

[0049] Such as figure 2 Shown, control metering pump 3,6 so that 20% liquid caustic soda is with the flow rate of 1kg / h, catalyst tetra-n-butylammonium bromide is with 0.25m 3 The flow velocity of / h enters the first mixing module 7 of microchannel reactor, and the mixing time of the first mixing module 7 is set as 1 minute, enters the first preheating module 8 after mixing 1 minute, the setting of the first preheating module 8 The fixed temperature is 70°C, and the preheating time is 2 minutes; the metering pump 4 is controlled so that 3,5-dichloro-2-pentanone enters the second preheating module 9 at a flow rate of 2.2kg / h, and the second preheating module 9 The set temperature is 70°C, and the preheating time is 2 minutes; after 2 minutes of preheating, the mixture of 20% and catalyst and 3,5-dichloro-2-pentanone are simultaneously passed into the second mixing module 10 for cyclic For the cyclization reaction, the set temperature of the second mixing module 10 is 70° C., ...

Embodiment 2

[0051] Such as figure 2 Shown, control metering pump 3,6 so that 20% liquid caustic soda is with the flow rate of 1kg / h, catalyst tetra-n-butylammonium bromide is with 0.25m 3 The flow velocity of / h enters the first mixing module 7 of microchannel reactor, and the mixing time of the first mixing module 7 is set as 3 minutes, enters the first preheating module 8 after mixing 3 minutes, the setting of the first preheating module 8 The fixed temperature is 70°C, and the preheating time is 5 minutes; the metering pump 4 is controlled so that 3,5-dichloro-2-pentanone enters the second preheating module 9 at a flow rate of 2.2kg / h, and the second preheating module 9 The set temperature is 70°C, and the preheating time is 5 minutes; after 5 minutes of preheating, the mixture of 20% and the catalyst and 3,5-dichloro-2-pentanone are simultaneously passed into the second mixing module 10 for cyclic cyclization reaction, the temperature of the second mixing module 10 is set at 70°C, a...

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Abstract

The invention provides a method for continuously preparing 1-(1-chlorocyclopropyl)ethanone by using a micro-channel reactor. Mixing and preheating of a raw material a and a catalyst, preheating of a 3,5-dichloro-2-pentanone, a cyclization reaction of the raw material a and the 3,5-dichloro-2-pentanone and cooling of the product are all carried out in the micro-channel reactor. The method has the advantages of simplicity in operation, high raw material conversion rate, high product yield, great shortening of the reaction time, reduction of byproducts, accuracy in control of the temperature in the reaction process, and continuity in the reaction.

Description

technical field [0001] The invention relates to the technical field of preparing 1-(1-chlorocyclopropyl)ethanone, in particular to a method for preparing 1-(1-chlorocyclopropyl)ethanone using a microchannel reactor. Background technique [0002] Prothioconazole is a new type of broad-spectrum triazolethione fungicide developed by Bayer, mainly used to prevent and control many diseases of cereals, wheat and legumes. Prothioconazole has low toxicity, no teratogenicity, and no mutagenicity. Type, non-toxic to embryos, safe to humans and the environment. [0003] The molecular formula of 1-(1-chlorocyclopropyl)ethanone is C 5 h 7 ClO, with a molecular weight of 118.562 and a structural formula as follows, is an important intermediate of prothioconazole. [0004] [0005] At present, 1-(1-chlorocyclopropyl)ethanone mainly uses 3,5-dichloro-2-pentanone as a raw material, and 3,5-dichloro-2-pentanone is quickly dropped into a reaction kettle equipped with liquid caustic soda....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/327C07C45/61B01J19/00
CPCB01J19/0093C07C45/61C07C2601/02C07C49/327
Inventor 纪传武魏星朱新江孙新
Owner XINYI AGRI CHEM PLANT JIANGSU PROV
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