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Method for preparing dichlorooctafluorobutane by means of liquid-phase photochlorination

A technology of dichlorooctafluorobutane and chlorination method, which is applied in the fields of chemical instruments and methods, preparation of halogenated hydrocarbons, preparation of halogen addition, etc. It can solve the problem of relatively harsh reaction conditions, easy polymerization and purification of perfluorobutene Difficult separation and other problems, to achieve the effect of simple and efficient preparation, avoid high temperature self-polymerization, and low equipment requirements

Inactive Publication Date: 2018-11-23
ZHEJIANG JUSHENG FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, dichlorooctafluorobutane is mainly prepared from 2,3-dichlorohexafluoro-2-butene or chlorotrifluoroethylene through multi-step reactions, but the yield is as low as about 65%. Multiple by-products, subsequent purification and separation are difficult
Literature (J.Phys.Chem., 1957,61,1124-1125) reported the method of using perfluorobutene as raw material to prepare dichlorooctafluorobutane, which is gas-phase catalytic chlorination to prepare dichlorooctafluorobutane , this method has strict requirements on the reaction conditions. The catalyst preparation, filling and reaction must be carried out under the condition of isolating oxygen. The high reaction temperature perfluorobutene is easy to polymerize and carbon deposits, resulting in the failure of the catalyst.

Method used

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  • Method for preparing dichlorooctafluorobutane by means of liquid-phase photochlorination

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Embodiment 1

[0029] Put 2000mol of perfluoro-2-butene into a 500L enamel reactor equipped with a light source irradiation port, under the irradiation of a light source with a power of 1kw and a wavelength of 400nm, continuously feed 2000mol of chlorine gas for reaction, and the reaction temperature is controlled at -10°C , the reaction pressure was controlled at 20kPa, and the material was discharged after the reaction was completed, washed with alkali, dried, and purified by rectification to obtain 1992mol of product 2,3-dichlorooctafluorobutane, with a yield of 99.6%.

Embodiment 2

[0031] Put 2000mol of perfluoro-2-butene into a 500L enamel reaction tower equipped with a light source irradiation port. Under the irradiation of a light source with a power of 2kw and a wavelength of 315nm, 3000mol of chlorine gas is continuously introduced to react. The reaction temperature is controlled at 0°C. The pressure was controlled at 60kPa, and the material was discharged after the reaction was completed, washed with alkali, dried, and purified by rectification to obtain 1996mol of the product 2,3-dichlorooctafluorobutane, with a yield of 99.8%.

Embodiment 3

[0033] Put 2000mol of perfluoro-2-butene into a 500L enamel reaction tower equipped with a light source irradiation port. Under the irradiation of a light source with a power of 3kw and a wavelength of 250nm, 4000mol of chlorine gas is continuously introduced to react. The reaction temperature is controlled at 10°C. The pressure was controlled at 100kPa, and the material was discharged after the reaction was completed, washed with alkali, dried, and purified by rectification to obtain 1974mol of the product 2,3-dichlorooctafluorobutane, with a yield of 98.7%.

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Abstract

The invention discloses a method for preparing dichlorooctafluorobutane by means of liquid-phase photochlorination. The method comprises the steps continuously introducing chlorine gas into perfluorobuttene under photocatalysis for reacting, and after the reaction is finished, carrying out alkali washing, drying and rectification to obtain the dichlorooctafluorobutane product. The method has the advantages of simple process, easily available raw materials, mild reaction conditions, high yield and environmental protection.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing chloroalkane, in particular to a method for preparing dichlorooctafluorobutane by a liquid-phase photochlorination method. Background technique [0002] Fluoropolymers, also known as fluororesins, have been developed for decades and are now widely used in various industries. For example, it is used for medical materials, automobiles, industrial coatings, communication cables, wires, semiconductors, chemical anticorrosion, inner villages of chemical equipment, surface layers of rollers, etc. [0003] The solvent used in the polymerization process of fluoropolymers is F113, that is, 1,1,2-trichlorotrifluoroethane, which is a chlorofluorocarbon with a large ozone depletion potential. Therefore, more than 140 countries in the world, including China, have restricted its use. Since December 30, 2005, the use of F113 except as a raw material for chlorotrifluoroethylene has been stopped. F1...

Claims

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Application Information

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IPC IPC(8): C07C17/04C07C17/383C07C19/10
CPCC07C17/04C07C17/383C07C19/10
Inventor 王志辉余考明朱洪吉陈伟峰叶怀英
Owner ZHEJIANG JUSHENG FLUOROCHEM
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