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Method for synthesizing hexafluorobutadiene through reaction rectification

A technology of hexafluorobutadiene and reactive distillation, applied in chemical instruments and methods, interhalogen compounds, halogen addition preparation, etc., can solve the problems of long reaction time, low catalytic efficiency, slow reaction speed, etc. Simple equipment, good catalytic activity and easy separation

Inactive Publication Date: 2018-05-29
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] ‍‍Oxygenated organic compounds used as solvents in the prior art will lead to low catalytic efficiency, slow reaction speed, long reaction time and many side reactions. It is necessary to find a more efficient synthesis method

Method used

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Examples

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Effect test

Embodiment 1

[0024] A method for reactive distillation synthesis of hexafluorobutadiene, comprising the following steps:

[0025] Step 1: Iodine and chlorine react in methylene chloride solution to form iodine chloride, the molar ratio of iodine to chlorine is 1:1.8, and the reaction temperature is 40°C;

[0026] Step 2: Reaction of iodine chloride and chlorotrifluoroethylene in dichloromethane solution environment to generate trifluorodichloroiodoethane, molar ratio of iodine chloride to chlorotrifluoroethylene=1:1.9, reaction temperature 50°C, reaction The pressure is 0.5MPa, the reaction product is washed with sodium hydroxide and sodium sulfite solution, neutralized and settled to separate the crude trifluorodichloroethane, and the trifluorodichloroiodoethane is purified by rectification;

[0027] Step 3: Dimerization of trifluorodichloroiodoethane and zinc with ethyl acetate in dichloromethane solution to generate 1, 2, 3, 4-tetrachlorohexafluorobutane and trifluorodichloroiodoethane ...

Embodiment 2

[0033] A kind of reaction synthesis prepares the method for hexafluorobutadiene, comprises the following steps:

[0034] Step 1: Iodine and chlorine react in methylene chloride solution to form iodine chloride, the molar ratio of iodine and chlorine is 1:1.1, and the reaction temperature is 20°C;

[0035] Step 2: Reaction of iodine chloride and chlorotrifluoroethylene in dichloromethane solution environment to generate trifluorodichloroiodoethane, molar ratio of iodine chloride to chlorotrifluoroethylene = 1:1.1, reaction temperature 30°C, reaction The pressure is 0.3MPa, the reaction product is washed with sodium hydroxide and sodium sulfite solution, neutralized and settled to separate the crude trifluorodichloroethane, and the trifluorodichloroiodoethane is purified by rectification;

[0036] Step 3: Dimerization of trifluorodichloroiodoethane and zinc with ethyl acetate in dichloromethane solution to generate 1, 2, 3, 4-tetrachlorohexafluorobutane and trifluorodichloroiodo...

Embodiment 3

[0042] A method for reactive distillation synthesis of hexafluorobutadiene, comprising the following steps:

[0043] Step 1: Iodine and chlorine react in methylene chloride solution to form iodine chloride, the molar ratio of iodine to chlorine is 1:2.5, and the reaction temperature is 50°C;

[0044] Step 2: Reaction of iodine chloride and chlorotrifluoroethylene in dichloromethane solution environment to generate trifluorodichloroiodoethane, molar ratio of iodine chloride to chlorotrifluoroethylene=1:2.2, reaction temperature 70°C, reaction Pressure 1.0MPa, the reaction product was washed with sodium hydroxide and sodium sulfite solution, neutralized and settled to separate crude trifluorodichloroethane, and trifluorodichloroiodoethane was purified by rectification;

[0045] Step 3: Dimerization of trifluorodichloroiodoethane and zinc with ethyl acetate in dichloromethane solution to generate 1, 2, 3, 4-tetrachlorohexafluorobutane and trifluorodichloroiodoethane The molar ra...

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PUM

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Abstract

The invention provides a method for synthesizing hexafluorobutadiene through reaction rectification. The method comprises the following steps of performing preparation by a catalysis distillation column, wherein the catalysis distillation column consists of a rectification section, a reaction section, a stripping section and a column kettle in sequentially connection from the tower top to the tower bottom; and a catalysis distillation element is filled in the reaction section. A preparation method comprises the following steps of uniformly mixing 1,2,3,4-tetrachloro-1,1,2,3,4,4-hexafluoro butane and organic solvents accounting for 500 to 1000 mass percent of the 1,2,3,4-tetrachloro-1,1,2,3,4,4-hexafluoro butane; continuously adding the materials into the catalysis distillation column fromthe rectification section and the stripping section for reaction.

Description

technical field [0001] The invention relates to a method for preparing hexafluorobutadiene, in particular to a method for synthesizing hexafluorobutadiene through reactive distillation. Background technique [0002] Perfluoroalkanes (PFCs), which are currently widely used, do not destroy the ozone layer, but are identified as strong greenhouse gases in the Kyoto Protocol. With the continuous improvement of people's environmental requirements, the use of traditional fluorine-containing electronic gases will be greatly restricted. Therefore, it is necessary to find new environmentally friendly fluorine-containing electronic gases. Hexafluoro-1,3-butadiene (HFBD) has become one of the best substitutes for traditional fluorine-containing electronic gases due to its excellent performance in various aspects. It is a monomer for preparing various fluoropolymer materials, or a A green and environmentally friendly high-efficiency dry etching gas has attracted great attention from s...

Claims

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Application Information

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IPC IPC(8): C07C17/23C07C17/383C07C21/20B01J29/48C01B7/24
CPCB01J29/48B01J2229/183C01B7/24C07C17/04C07C17/23C07C17/281C07C17/383C07C21/20C07C19/10C07C19/12Y02P20/10
Inventor 陈刚张晓东周井森
Owner ZHEJIANG BRITECH CO LTD
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