Method for preparing 1,1,1,3,3 - pentachlorobutane from materials of chloropropene and carbon tetrachloride under tempering and polymerizing catalyst

A technology of carbon tetrachloride and pentachlorobutane, applied in 1 field, can solve the problems of increased production cost, potential safety hazard, reaction temperature and reaction pressure, and achieves the effects of reduced production cost, reduced potential safety hazard, and easy separation

Active Publication Date: 2007-05-09
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (1). Catalysts are highly toxic; if copper salts, cuprous salts and amines are used as catalysts, a viscous semi-solid will be formed after the reaction, which is difficult to separate except for washing with water in actual operation. Bring waste water treatment and recovery of copper ions;
[0010] (2). Low conversion rate of raw materials and low product yield;
[0011] (3). The reaction system requires a large amount of organic solvents to participate, and the reaction temperature and reaction pressure are high
[0012] Above-mentioned defect promptly will increase production cost, has brought potential safety hazard again; And reaction product 1,1,1,3,3-pentachlorobutane will pass through complex separation operation, a series of problems such as catalyst recycling cost height, all will affect industrial production

Method used

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  • Method for preparing 1,1,1,3,3 - pentachlorobutane from materials of chloropropene and carbon tetrachloride under tempering and polymerizing catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] With ferrous chloride as the main catalyst and triethyl phosphite as the co-catalyst, the reaction temperature is 95°C, and the molar ratio of the materials is: carbon tetrachloride / 2-chloropropene / ferrous chloride / triethyl phosphite Ester=1:0.4:0.02:0.02; the reaction time is 5 hours, and the reaction pressure is ≤0.45MPa. GC analysis was performed after the reaction, and the conversion rate of 2-chloropropene was 98%, and the selectivity of 1,1,1,3,3-pentachlorobutane based on 2-chloropropene was 95%.

Embodiment 2

[0041] With iron and ferric chloride as the main catalyst, trimethyl phosphate as the co-catalyst, the reaction temperature is 85°C, and the molar ratio of the materials is: carbon tetrachloride / 2-chloropropene / iron and ferric chloride / trimethyl phosphate Ester=1:0.4:0.03:0.02; the reaction time is 6 hours, and the reaction pressure is ≤0.40MPa. GC analysis was performed after the reaction, and the conversion rate of 2-chloropropene was 98%, and the selectivity of 1,1,1,3,3-pentachlorobutane based on 2-chloropropene was 95%.

Embodiment 3

[0043] Iron and ferric chloride are used as the main catalyst, and mixed esters of triethyl phosphate and tributyl phosphate are used as co-catalysts. The reaction temperature is 85°C, and the molar ratio of materials is: carbon tetrachloride / 2-chloropropene / iron And ferric chloride / phosphoric acid mixed ester=1:0.4:0.03:0.02; the reaction time is 6 hours, and the reaction pressure is ≤0.35MPa. GC analysis was performed after the reaction, and the conversion rate of 2-chloropropene was 99%, and the selectivity of 1,1,1,3,3-pentachlorobutane based on 2-chloropropene was 95%.

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Abstract

This invention relates to a method for preparing 1, 1, 1, 3, 3-pentachorobutane from 2-chloropropylene and tetrachloromethane in the presence of telomerization catalyst. The major catalyst is selected from Fe (II) salts, Fe and Fe (III) salts. The assistant catalyst is selected from alkyl phosphites and/or alkyl phosphates. This invention solves the problems of high catalyst toxicity, uneasy washing and recovery of viscous semi-solid catalyst, low conversion rate of the raw materials, low yield of the product, and large quantities of solvents needed faced by present techniques. The method in this invention does not need organic solvent, and can easily control the reaction temperature and pressure. The catalyst can be easily separated from the product, and can be recycled.

Description

technical field [0001] The present invention relates to the preparation method of 1,1,1,3,3-pentachlorobutane, especially telomerization of 2-chloropropene and carbon tetrachloride as raw materials to prepare 1,1,1,3,3-pentachlorobutane butane method. Background technique [0002] 1,1,1,3,3-pentachlorobutane (referred to as HCC-360jfa) is the raw material for the preparation of 1,1,1,3,3-pentafluorobutane (referred to as HFC-365mfc), 1,1,1 , 3,3-pentafluorobutane is a hydrofluoroalkane, its ODP value (atmospheric ozone depletion potential value) is 0, and its GWP value (global warming potential) is 830. It is a substitute for HCFC-141b and CFC-11 , can be widely used as foaming agent, cleaning agent and other fields. [0003] As we all know, multi-carbon halogenated alkanes are prepared by the catalytic addition of alkenes and halogenated alkanes. In the existing 1,1,1,3,3-pentachlorobutane preparation technology, there are already quite a few...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/01C07C17/278B01J27/128B01J31/18B01J31/30
CPCB01J27/128B01J31/0258B01J31/0259C07C17/278B01J31/30
Inventor 韩国庆吴江平杨箭方小青
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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