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A kind of continuous synthesis method of chlorinated alkanes

A technology for chlorinated alkanes and a synthesis method, which is applied to the preparation of halogenated hydrocarbons, chemical instruments and methods, chemical recovery, etc., can solve the problems of high manufacturing cost, low production efficiency, long reaction time and the like of tetrafluoroethylene-lined autoclaves, Achieve the effect of high production efficiency, less equipment investment and simple operation

Active Publication Date: 2015-09-23
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages are that the reaction is batch production, cumbersome operation, long reaction time, and low production efficiency; the manufacturing cost of the tetrafluoroethylene-lined autoclave is high; the uniform dispersion of iron powder in the solution and the problem of blockage of equipment and pipelines during catalyst recovery Not easy to solve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 10L stainless steel reactor with external circulation, add 2L carbon tetrachloride and 300 mesh iron powder mixture, the mass ratio of carbon tetrachloride and iron powder is 1:0.3. Start the circulation pump, draw the reaction solution containing iron powder from the bottom of the reactor, pressurize it through the circulation pump, and then pump it into the reactor from the top of the reactor. Continuously add a mixture of carbon tetrachloride and triethyl phosphite with a molar ratio of 47:1 into the reactor from the bottom of the reactor, raise the temperature and control the reaction temperature to 100°C, and at the same time pass the Continuously feed ethylene to control the reaction pressure to 1.0MPa for reaction. The reaction liquid is continuously drawn from the overflow port on the upper part of the reactor, and after rectification, the unreacted carbon tetrachloride is recovered, and the 1,1,1,3-tetrachloropropane product, 1,1,1,3-tetrachloropropane is ...

Embodiment 2

[0033] In a 10L stainless steel reactor with external circulation, add 2L of carbon tetrachloride and 500 mesh iron powder mixture, the mass ratio of carbon tetrachloride and iron powder is 1:0.1. Start the circulation pump, draw the reaction solution containing iron powder from the bottom of the reactor, pressurize it through the circulation pump, and then pump it into the reactor from the top of the reactor. Continuously add a mixture of carbon tetrachloride and triethyl phosphite with a molar ratio of 40:1 into the reactor from the bottom of the reactor, raise the temperature and control the reaction temperature to 120°C, and at the same time pass the mixture from the bottom of the reactor to the reactor Continuously feed ethylene to control the reaction pressure to 1.2MPa for reaction. The reaction liquid is continuously drawn from the overflow port on the upper part of the reactor, and after rectification, the unreacted carbon tetrachloride is recovered, and the 1,1,1,3-t...

Embodiment 3

[0035] In a 10L stainless steel reactor with external circulation, add 1L carbon tetrachloride and 400 mesh iron powder mixture, the mass ratio of carbon tetrachloride to iron powder is 1:0.8. Start the circulation pump, draw the reaction solution containing iron powder from the bottom of the reactor, pressurize it through the circulation pump, and then pump it into the reactor from the top of the reactor. A mixture of carbon tetrachloride and triethyl phosphite with a molar ratio of 50:1 was continuously added to the reactor from the bottom of the reactor. The temperature was raised and the reaction temperature was controlled to be 150° C., and at the same time, ethylene was continuously fed into the reactor from the bottom of the reactor to control the reaction pressure to be 0.5 MPa to carry out the reaction. The reaction liquid is continuously drawn from the overflow port on the upper part of the reactor, and after rectification, the unreacted carbon tetrachloride is recov...

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PUM

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Abstract

The invention discloses a continuous synthetic method of chloralkane. The method comprises the following steps: (1) adding a mixture of carbon tetrachloride and iron powder into a reactor, wherein the volume of the mixture is 10-30% of the volume of the reactor, and the mass ratio of carbon tetrachloride to the iron powder in the mixture is 1:(0.1-1); (2) continuously adding a mixture of carbon tetrachloride and a catalyst with the molar ratio of (40-50):1 to the reactor from the bottom of the reactor, controlling the reaction temperature at 90-150 DEG C, and meanwhile, continuously introducing olefin to the reactor from the bottom of the reactor to control the reaction pressure at 0.5-1.2MPa to react; (3) collecting a reacting liquid overflowing from the upper part of the reactor and rectifying the reacting liquid to obtain a chloralkane product. The method provided by the invention has the advantages of simplicity in operation, less equipment investment, high production efficiency and recycling of the catalyst without separation.

Description

technical field [0001] The invention relates to a continuous synthesis method of chlorinated alkanes. Background technique [0002] Carbon tetrachloride, a by-product of the production of methane chloride, is banned in cleaning agents as an ozone-depleting substance. The most feasible way to solve a large amount of carbon tetrachloride is to use it as a chemical raw material and convert it into a non-ODS substance. The telomerization reaction between carbon tetrachloride and olefins to generate chlorinated alkanes, which are further fluorinated into fluoroalkanes, has been widely used. This synthesis method must be carried out in the presence of a catalyst, and there are many reports in the literature. The catalysts mainly include peroxides, metal inorganic salts and nitriles, metal carbonyl compounds, alkyl phosphites and metal chlorides. [0003] As a catalyst, the telomerization reaction of peroxide is too violent, difficult to control, and has the risk of explosion, so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/01C07C17/275
CPCY02P20/584
Inventor 耿为利韩金铭周强王树华
Owner JUHUA GROUP TECH CENT