Method for preparing 1,1,1,3,3-pentachlorobutane

A technology of pentachlorobutane and chloropropene, applied in the field of preparation of 1,1,1,3,3-pentachlorobutane, which can solve the problems of high reaction temperature, difficult storage, and easy oxidation of cuprous chloride by air , to achieve the effect of mild reaction conditions and easier storage

Active Publication Date: 2016-03-23
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation HCC-360jfa technology reported in the above literature has the disadvantage of high reaction temperature, and 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 1,1,1,3,3-pentachlorobutane
  • Method for preparing 1,1,1,3,3-pentachlorobutane

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 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 carbon tetrachloride 770g (5mol) were sequentially added to a 1L stainless steel autoclave. Seal the autoclave, start stirring, and replace the air in the autoclave with nitrogen for three times. Subsequently, 156.25 g of 2-chloropropene was added at one time, the temperature of the reactor 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 2-chloropropene was 96%, and the selectivity of HCC-360jfa was 97%.

Embodiment 2

[0022] 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 2-chloropropene was 94.5%, and the selectivity of HCC-360jfa was 94.3%.

Embodiment 3～9

[0024] 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.

[0025] Table 1

[0026]

[0027]

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Abstract

The invention discloses a method for preparing 1,1,1,3,3-pentachlorobutane. According to the method, carbon tetrachloride and 2-chloropropene have a telomerization reaction through a telomerization catalyst to prepare 1,1,1,3,3-pentachlorobutane, wherein the reaction temperature ranges from 25 DEG C to 100 DEG C, and the reaction time ranges from 0.5 h to 5 h. The telomerization catalyst is prepared from a main catalyst, an auxiliary catalyst and an organic active agent, wherein halogenated copper salt or halogenated iron salt serves as the main catalyst, alkyl phosphate or diisopropyl phosphate or organic tertiary amine serves as the auxiliary catalyst, azodiisobutyronitrile, 2,2-azobis(4-methoxy-2,4-dimethylvaleronitrile), 1,1-azo-Biscyclohexanecarbonitrile, ascorbic acid, 2,3,4,5,6-5-hydroxy aldehyde, phenylhydrazine or metoxyphenol serves as the organic active agent, and the molar ratio of the main catalyst to the auxiliary catalyst to the organic active agent is 1:(0.5-20):(0.1-20). The telomerization catalyst has the advantages of being mild in reaction conditions and stable in air and can be used for catalyzing the telomerization reaction between carbon tetrachloride and 2-chloropropene to prepare 1,1,1,3,3-pentachlorobutane.

Description

technical field [0001] The present invention relates to a kind of method of preparing 1,1,1,3,3-pentachlorobutane, specifically refers to in the presence of a telomerization catalyst composed of a main catalyst, a cocatalyst and an organic activator, carbon tetrachloride and 2 A method for preparing 1,1,1,3,3-pentachlorobutane through telomerization of chloropropene. Background technique [0002] 1,1,1,3,3-Pentachlorobutane (HCC-360jfa) is an intermediate for the preparation of 1,1,1,3,3-pentafluoropropane (HFC-365mfc). The atmospheric ozone depletion potential (ODP) of HFC-365mfc is zero, and it has excellent environmental performance. It is an ideal substitute for 1,1,1-dichlorofluoroethane (HCFC-141b) and fluorodichloromethane (CFC-11) Products, widely used as foaming agent, solvent and cleaning agent. [0003] In the existing HCC-360jfa preparation technology, carbon tetrachloride and 2-chloropropene are mainly used as raw materials, which are synthesized under the act...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/01C07C17/278
CPCC07C17/278C07C19/01
Inventor 吕剑唐晓博韩升赵波郝志军曾纪珺张伟王博亢建平杜咏梅杨志强李凤仙
Owner XIAN MODERN CHEM RES INST
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