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Production method of 1,1,1,3,3-pentachlorobutane

A technology of pentachlorobutane and a production method, which is applied in the field of continuous reaction synthesis, can solve the problems of difficult continuous quantitative addition to a reaction system, complicated separation process, and difficult industrialized implementation, etc., and achieves easy implementation, volume reduction, and easy recycling. Effect

Inactive Publication Date: 2010-12-15
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such as: US20050049443 discloses a method for continuous production of 1,1,1,3,3-pentachlorobutane, the method uses a tank reactor, and the catalytic system is composed of copper salt and amine, which will form a viscous Semi-solid organic amine salt, the separation process is complicated, the recovered catalyst is a solid material, it is not easy to continuously quantitatively add to the reaction system, the operation is difficult, and it is difficult to implement industrially

Method used

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Embodiment 1

[0037] In this embodiment, the telomerization reactor 4 adopts an externally heated tubular reactor with a pipe diameter of ∮25×2.5 mm and a length of 2 meters. The process flow is as follows:

[0038] A, carbon tetrachloride and 2-chloropropene are mixed in a molar ratio of 10:1, and preheated to 150°C;

[0039] B. Preheated carbon tetrachloride and 2-chloropropene enter the tubular reactor together with the catalyst, and carry out telomerization reaction under the conditions of reaction pressure 1.5MPa, reaction temperature 140°C, and residence time of 5 minutes, wherein the catalyst by FeCl 2 , tributyl phosphate and carbon tetrachloride, FeCl 2 , the molar ratio of tributyl phosphate and carbon tetrachloride is 1:10:20, FeCl 2 The molar ratio to 2-chloropropene is 1:100;

[0040] C, telomerization reaction product removes unreacted carbon tetrachloride through flash evaporation, and unreacted carbon tetrachloride is recycled;

[0041] D. The reaction solution after remov...

Embodiment 2

[0044] In this embodiment, the telomerization reactor 3 adopts an adiabatic tubular reactor with a pipe diameter of ∮25×2.5 mm and a length of 2 meters. The process flow is as follows:

[0045] A. Mix carbon tetrachloride and 2-chloropropene in a molar ratio of 1:1, and preheat to 100°C;

[0046] B, preheated carbon tetrachloride and 2-chloropropene enter the tubular reactor together with the catalyst, and carry out the telomerization reaction under the conditions of reaction pressure 0.3MPa, reaction temperature 90°C, and residence time of 60 minutes, wherein The initial catalyst consists of FeCl 2 , triethyl phosphate and carbon tetrachloride, FeCl 2 , the molar ratio of triethyl phosphate and carbon tetrachloride is 1:1:50, and the catalyst is made of FeCl during circulation 2 , triethyl phosphate and telomerization reaction product distillation raffinate; FeCl 2 The molar ratio with 2-chloropropene is 1:20;

[0047] C, telomerization reaction product removes unreacted ...

Embodiment 3

[0053] In this embodiment, the telomerization reactor 4 adopts a Teflon-lined adiabatic tubular reactor with a pipe diameter of ∮38×2.5 mm and a length of 2 meters. The process flow is as follows:

[0054] A, carbon tetrachloride and 2-chloropropene are mixed in a molar ratio of 1.5: 1, and preheated to 130°C;

[0055] B. Preheated carbon tetrachloride and 2-chloropropene enter the tubular reactor together with the catalyst, and carry out telomerization reaction under the conditions of reaction pressure 0.6MPa, reaction temperature 120°C, and residence time of 30 minutes. when the catalyst consists of FeCl 2 , triethyl phosphite and carbon tetrachloride, FeCl 2 , the molar ratio of triethyl phosphate and carbon tetrachloride is 1:3:20, and the catalyst is made of FeCl during circulation 2 , triethyl phosphite and distillation raffinate of telomerization reaction product; FeCl 2 The molar ratio with 2-chloropropene is 1:50;

[0056] C, telomerization reaction product remove...

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Abstract

The invention provides a production method of 1,1,1,3,3-pentachlorobutane (HCC-360jfa), in which carbon tetrachloride and 2-chloropropene are taken as raw materials for continuous reaction in a tubular reactor to synthesize the 1,1,1,3,3-pentachlorobutane. In the method, the carbon tetrachloride and 2-chloropropene are firstly mixed and preheated to reaction temperature; the carbon tetrachloride and 2-chloropropene enter the tubular reactor with a catalyst for telomerization; a product undergoes flash evaporation to remove the un-reacted tetrachloride and 2-chloropropene and then is further distilled to obtain the HCC-360jfa product; the un-reacted tetrachloride and 2-chloropropene are recycled; and the catalyst undergoes activating treatment for recycle. The catalyst used by the invention is liquid, no solid exists in the reaction product, and the tubular reactor is used for reaction, so that the invention is convenient for operation and easy for continuous production.

Description

technical field [0001] The present invention relates to a kind of 1,1,1,3, the production method of 3-pentachlorobutane, relate in particular to a kind of with carbon tetrachloride and 2-chloropropene (2-Cpe) as raw material, in tubular reactor A production method for the continuous reaction synthesis of 1,1,1,3,3-pentachlorobutane. Background technique [0002] 1,1,1,3,3-Pentachlorobutane (HCC-360jfa) is an intermediate for the preparation of 1,1,1,3,3-pentafluorobutane (HFC-365mfc). The atmospheric ozone depletion potential (ODP) of HFC-365mfc is zero. It is a kind of fluorinated hydrocarbon compound that is safe for the atmospheric ozone layer. It is currently mainly used as a fluorodichloromethane (CFC-11) and 1,1,1- Alternative to dichlorofluoroethane (HCFC-141b), widely used as blowing agent, solvent and cleaning agent. [0003] In the existing HCC-360jfa preparation technology, carbon tetrachloride and 2-chloropropene are mainly used as raw materials in the industry...

Claims

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Application Information

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IPC IPC(8): C07C19/01C07C17/278B01J31/30B01J35/12
CPCY02P20/584
Inventor 张伟吕剑寇联岗亢建平李凤仙郝志军杨志强袁俊
Owner XIAN MODERN CHEM RES INST
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