Production method of 1,1,1,3,3-pentachloropropane

A technology of pentachloropropane and production method, applied in the field of continuous reaction synthesis, can solve problems such as difficulty in operation, and achieve the effects of accurate measurement, easy implementation and volume reduction

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

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Problems solved by technology

Such as: US6313360 discloses a kind of method of continuous production 1,1,1,3,3-pentachloropropane, the method adopts tank reactor, and catalytic system is made up of iron powder, ferric chloride and organic phosphate, because The telomerization reaction is carried out under a certain pressure. As a solid material, iron powder is not easy to continuously quantitatively add to the reaction system, and the operation is difficult.

Method used

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  • Production method of 1,1,1,3,3-pentachloropropane
  • Production method of 1,1,1,3,3-pentachloropropane

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Embodiment 1

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

[0038] A. Mix carbon tetrachloride and vinyl chloride at a molar ratio of 10:1, and preheat to 150°C;

[0039] B. The preheated carbon tetrachloride and vinyl chloride enter the tubular reactor together with the catalyst. The telomerization reaction is carried out under the conditions of a reaction pressure of 1.5MPa, a reaction temperature of 140°C and a residence time of 5 minutes. The catalyst is composed of 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 with vinyl chloride is 1:100;

[0040] C. The telomerization reaction product is flashed to remove unreacted carbon tetrachloride, and the unreacted carbon tetrachloride is recycled;

[0041] D. The reaction liquid after removing carbon tetra...

Embodiment 2

[0044] The telomerization reactor 4 in this embodiment adopts an adiabatic tubular reactor with a tube diameter of ∮25×2.5mm and a length of 2 meters. The process flow is:

[0045] A. Mix carbon tetrachloride and vinyl chloride at a molar ratio of 1:1, and preheat to 100°C;

[0046] B. The preheated carbon tetrachloride and vinyl chloride enter the tubular reactor together with the catalyst. The telomerization reaction is carried out under the conditions of a reaction pressure of 0.3MPa, a reaction temperature of 90°C, and a residence time of 60 minutes. Catalyst made 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 residue composition; FeCl 2 The molar ratio with vinyl chloride is 1:20;

[0047] C. The telomerization reaction product is flashed to remove unreacted carbon...

Embodiment 3

[0053] The telomerization reactor 4 in this embodiment adopts an adiabatic tubular reactor lined with tetrafluoroethylene with a diameter of ∮38×2.5mm and a length of 2 meters. The process flow is:

[0054] A. Mix carbon tetrachloride and vinyl chloride at a molar ratio of 1.5:1, and preheat to 130°C;

[0055] B. The preheated carbon tetrachloride and vinyl chloride enter the tubular reactor together with the catalyst. The telomerization reaction is carried out under the conditions of a reaction pressure of 0.6MPa, a reaction temperature of 120°C, and a residence time of 30 minutes. By 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 composed of FeCl during circulation. 2 , Triethyl phosphite and telomerization reaction product distillation residue composition; FeCl 2 The molar ratio with vinyl chloride is 1:50;

[0056] C. The telomerization reaction product is flashed to remo...

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Abstract

The invention provides a production method of 1,1,1,3,3-pentachloropropane (HCC-240fa). The 1,1,1,3,3-pentachloropropane is synthesized by continuously reacting the materials of carbon tetrachloride and chloroethylene in a tubular reactor. The method comprises the steps of firstly mixing the carbon tetrachloride with the chloroethylene and preheating the mixture to a reaction temperature, then introducing the mixture together with a catalyst into the tubular reactor for telomeric reaction, removing the unreacted carbon tetrachloride and chloroethylene through flash evaporation, and then further distilling to obtain the HCC-240fa, wherein the unreacted carbon tetrachloride and chloroethylene are recycled and the catalyst is recycled after being subjected to the activating treatment. The invention adopts the liquid as the activated system and uses the tubular reactor for reaction, thereby ensuring simple and convenient operation as well as continuous production.

Description

Technical field [0001] The invention relates to a production method of 1,1,1,3,3-pentachloropropane, in particular to a continuous reaction synthesis method using carbon tetrachloride and vinyl chloride (VnCl) as raw materials in a tubular reactor. , 1,1,3,3-pentachloropropane production method. Background technique [0002] 1,1,1,3,3-pentachloropropane (HCC-240fa) is an intermediate for the preparation of 1,1,1,3,3-pentafluoropropane (HFC-245fa). The atmospheric ozone depletion potential (ODP) of HFC-245fa is zero. It is a fluorinated hydrocarbon compound that is safe for the atmospheric ozone layer. It is currently mainly used as monofluorodichloromethane (CFC-11) and 1,1,1- An alternative to dichlorofluoroethane (HCFC-141b), it is widely used as a foaming agent, solvent and cleaning agent. [0003] In the existing HCC-240fa preparation technology, carbon tetrachloride and vinyl chloride are mainly used as raw materials in industry. Under the action of a catalyst, a telomerizat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/01C07C17/278B01J31/30B01J35/12
CPCY02P20/584
Inventor 吕剑张伟曾纪珺封利民马洋博杨志强徐强谷玉杰
Owner XIAN MODERN CHEM RES INST
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