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Method for preparing polyhalogenated hydrocarbon through telomerization

A polyhalogenated hydrocarbon and telomerization technology, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of high reaction temperature, difficult storage, long reaction time, etc., and achieve mild reaction conditions and easier reaction. Storage, effect of high catalytic activity

Active Publication Date: 2016-01-06
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The technology for preparing polyhalogenated hydrocarbons reported in the above literature has the disadvantages of relatively high reaction temperature or relatively long reaction time, while the telomerization catalyst cuprous chloride is easily oxidized by air and is not easy to store

Method used

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  • Method for preparing polyhalogenated hydrocarbon through telomerization
  • Method for preparing polyhalogenated hydrocarbon through telomerization
  • Method for preparing polyhalogenated hydrocarbon through telomerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The main catalyst ferric chloride 8.13g (0.05mol), the cocatalyst tributyl phosphate 39.9g (0.15mol), the organic activator 1,1-azobiscyclohexanenitrile 12.2 (0.05mol) and CCl 4 770g (5mol) was successively added to a 1L stainless steel autoclave. Seal the autoclave, start stirring, and replace the air in the autoclave with nitrogen for three times. Then add CH all at once 2 =CHCl156.25g, the reactor temperature was heated to 80°C, and the reaction was completed after 1 hour. After the autoclave was lowered to room temperature, the autoclave was unloaded and the material was taken out. A liquid sample was taken with a pipette and analyzed by chromatography. The conversion rate of vinyl chloride was 95.5%, and the selectivity of HCC-240fa was 96.1%.

Embodiment 2

[0025] The operating process of embodiment 2 is similar to embodiment 1, and difference is that main catalyst is ferric bromide. The product was analyzed by chromatographic method, the conversion rate of vinyl chloride was 96.5%, and the selectivity of HCC-240fa was 93.1%.

Embodiment 3～9

[0027] The operating process of Examples 3-9 is similar to that of Example 1, except that the cocatalyst and organic activator are changed, and the reaction temperature is adjusted to match the activity of the telomerization catalyst. The reaction results are shown in Table 1.

[0028] Table 1

[0029]

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Abstract

The invention discloses a method for preparing polyhalogenated hydrocarbon through telomerization. According to the method, chlorinated hydrocarbon R1R2CCl2 and olefin CH2 = CR3R4 perform telomerization reaction to prepare the polyhalogenated hydrocarbon in the presence of a telomerization catalyst, the reaction temperature is 25-100 DEG C, and the reaction time is 0.5-10 hours. The telomerization catalyst consists of a main catalyst, a catalyst promoter and an organic activator, wherein the main catalyst is halogenated copper salt or halogenated ferric salt, the catalyst promoter is alkyl phosphate ester, diisopropyl phosphite or organic tertiary amine, the organic activator is azodiisobutyronitrile, 2,2'-azobis(4-methoxy-2,4-dimethylvaleronitrile), 1,1'-azobis-cyclohexanecarbonitril, 2,3,4,5,6-pentahydroxyl-2-hexenic acid-4-lactone, 2,3,4,5,6-pentahydroxyl aldehyde, phenyl hydrazine or methoxy phenol. The telomerization catalyst adopted by the method has the advantages of existing in a reaction system in a homogeneous phase mode and being moderate in reaction condition and stable to air and can be used for catalyzed synthesis of lots of valuable polyhalogenated hydrocarbons.

Description

technical field [0001] The invention relates to a method for preparing polyhalogenated hydrocarbons through telomerization, specifically refers to the chlorinated hydrocarbon R 1 R 2 CCl 2 with alkene CH 2 =CR 3 R 4 Preparation of polyhalogenated hydrocarbons by telomerization. Background technique [0002] The telomerization reaction of chlorinated hydrocarbons and olefins is an important method for the preparation of polyhalogenated hydrocarbons. This method can be used to synthesize important intermediates for the production of fluorinated hydrocarbons. Fluorocarbons are widely used in refrigerants and heat transfer media , foaming agent and spray, etc., are one of the chemicals necessary for modern life. [0003] Chinese patent CN1986507A has reported CCl 4 with CH 2 = CHCl telomerization method to synthesize 1,1,1,3,3-pentachloropropane (HCC-240fa), HCC-240fa is the method for preparing 1,1,1,3,3-pentafluoropropane (HFC-245fa) intermediate. The reaction is cat...

Claims

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Application Information

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IPC IPC(8): C07C17/278C07C19/01
Inventor 曾纪珺吕剑唐晓博韩升张伟亢建平王博杜咏梅郝志军杨志强李凤仙
Owner XIAN MODERN CHEM RES INST
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