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Preparing method of high-purity alpha-chloroethylene cyclopropane

A technology of dichloroethylcyclopropane and phenylcyclopropane, which is applied in the field of preparation of high-purity α-chlorovinylcyclopropane, to achieve the effects of ensuring uniformity, reducing side reactions, and promoting mass transfer process

Active Publication Date: 2019-04-12
JIANGSU YUXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing technical routes need to be improved in terms of environmental friendliness and cost

Method used

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  • Preparing method of high-purity alpha-chloroethylene cyclopropane
  • Preparing method of high-purity alpha-chloroethylene cyclopropane
  • Preparing method of high-purity alpha-chloroethylene cyclopropane

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) In the jet loop reactor based on the Venturi effect, (its operation principle is based on the Venturi effect, the loop operation is downward flow, and the end of the jet mixer 1 of the reactor is immersed in the liquid phase of the loop reactor Middle), add α,α-dichloroethylcyclopropane raw material (139.1kg, 1kmol) through the material feed port 5, deoxygenate and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0033] (2) Control the temperature by heat exchanger 2 at 20°C, feed 34 kg of ammonia raw material through alkali raw material feed port 6 and catalyst potassium iodide 1.66 kg through material feed port 5 and slowly feed into the injection loop reactor, spray and mix And to realize the full reaction of the three, the feeding time is 24 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 8 hours.

[0034] (3) After the reaction is fin...

Embodiment 2

[0036] (1) In the jet loop reactor based on the Venturi effect, (its operation principle is based on the Venturi effect, the loop operation is downward flow, and the end of the jet mixer 1 of the reactor is immersed in the liquid phase of the loop reactor Middle), add α,α-dichloroethylcyclopropane raw material (139.1kg, 1kmol) through the material feed port 5, deoxygenate and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0037] (2) Control the temperature at 80°C by the heat exchanger 2, and slowly feed 62.1kg of the trimethylamine raw material into the injection loop reactor through the alkali raw material feed port 6 and the catalyst sodium iodide 7.49 kg through the material feed port 5 , jet mixing and full reaction of the three, the addition time is 3 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 1 hour.

[0038] (3) After the reaction is f...

Embodiment 3

[0040] (1) In the jet loop reactor based on the Venturi effect, (its operation principle is based on the Venturi effect, the loop operation is downward flow, and the end of the jet mixer 1 of the reactor is immersed in the liquid phase of the loop reactor Middle), add α,α-dichloroethylcyclopropane raw material (139.1kg, 1kmol) through the material feed port 5, deoxygenate and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0041] (2) at 30 DEG C by heat exchanger 2 control temperature, monomethylamine raw material 46.6kg enters in the injection loop reactor through the feed inlet 5 of material feed inlet 5 slowly through alkali raw material inlet 6 and potassium iodide 5.0kg, Jet mixing and full reaction of the three were achieved, and the addition time was 12 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 4 hours.

[0042](3) After the reaction is...

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Abstract

The invention discloses a preparing method of high-purity alpha-chloroethylene cyclopropane. The preparing method comprises the steps of adding raw alpha-alpha-dichloro ethyl cyclopropane materials into a jetting loop reactor based on a Venturi effect, conducting deoxygenization, filling the reactor with inert gas for replacement protection, then starting vacuum, starting an external circulating pump for high-speed jetting mixing, controlling the temperature to be 20-80 DEG C, and slowly adding raw alkaline materials and a catalyst into the jetting loop reactor. According to the preparing method, the novel jetting loop reactor based on the Venturi effect is adopted, sufficient mass transfer and reactions can be achieved between an organic phase and the raw alkaline materials in a system, the reaction efficiency is greatly improved, the occurrence of side effects is lowered, and salt-type products obtained through the reactions can be quickly diffused from the reaction system under thestrong mass transfer function of high-speed jetting mixing; meanwhile, good nucleation growth can be achieved due to the existence of the catalysts, filtering is facilitated, and rightward steady proceeding of the reactions is facilitated.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing high-purity α-chlorovinyl cyclopropane. Background technique [0002] ɑ-Chlorovinyl cyclopropane, the molecular structure is as follows: [0003] [0004] It is an important intermediate for the synthesis of cyclopropylacetylene, which is an important pharmaceutical and pesticide intermediate, especially an important intermediate for the anti-AIDS drug efavirenz. The synthesis of this product has important market value. [0005] Li Jianjun (CN200910101763.4) of Zhejiang University of Technology discloses a synthetic method of α-chlorovinyl cyclopropane, which is characterized in that the synthetic method is: cyclopropylmethyl ketone and bis(trichloromethyl)carbonic acid The ester is used as a raw material, which is completely reacted in an organic solvent at 0-150°C under the action of an organic amine catalyst, and the reaction liquid is dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/25C07C17/383C07C22/00
CPCC07C17/25C07C17/383C07C2601/02C07C22/00
Inventor 张治国徐官根徐林斌黄剑程红伟
Owner JIANGSU YUXIANG CHEM
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