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Preparation method for chlorotrifluoropropylene

A technology of monochlorotrifluoropropene and trifluorodichloropropane, which is applied in the field of preparation of monochlorotrifluoropropene, can solve the problems of high energy consumption, unsuitability for industrial scale-up production, and impossibility of obtaining it, and achieve low reaction temperature, The effect of meeting the requirements of industrial scale-up production

Inactive Publication Date: 2008-04-30
CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the reaction needs to be carried out under high temperature conditions, that is, fluorination into chlorotrifluoropropene in the next step at high temperature, the reaction products are more complicated, for example, there are about six azeotropic products (pentafluoropropane) between 15.8-20.8 °C , tetrafluoropropene, chlorotetrafluoropropane, dichlorotrifluoropropane, 1-chloro-3,3,3-trifluoropropene and 2-chloro-3,3,3-trifluoropropene, etc.), where 1- Chloro-3,3,3-trifluoropropene and 2-chloro-3,3,3-trifluoropropene are isomers of each other, which makes it almost impossible to obtain monochlorine with ideal purity under ordinary rectification purification conditions. Trifluoropropene, and the yield of chlorotrifluoropropene prepared by traditional method is low (obtaining a purity of 98% chlorotrifluoropropene with pentachloropropane as a benchmark, its yield is only about 60%) energy consumption is high, output is low
Not suitable for industrial scale-up production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 10L stainless steel autoclave with jacket and cooling water coil, add 200 grams of cuprous chloride, 200 grams of dimethylformamide and 500 grams of sulfolane, add 6160 grams of carbon tetrachloride, and feed into the stainless steel autoclave jacket Steam heating, start the stirring of autoclave, when autoclave material system temperature rises to 80 ℃, stop passing steam, press into 1250 grams of vinyl chloride. After stirring for 2 hours, continue to open the jacket steam valve. After the temperature of the reaction system reaches 100° C., control the temperature of the reaction system to maintain at 100-105° C., and keep the reaction system in this temperature range for 13 hours. Cool down to 60 DEG C then, open the discharge bottom valve of autoclave, obtain crude pentachloropropane 4317 grams.

[0020] The 5L four-necked glass flask has a Φ40×2000 glass column, which is filled with a 1900 mm high glass ring packing, and a condenser and a cock for adjusting the ref...

Embodiment 2

[0024] 10L stainless steel autoclave with jacket and cooling water coil, add 200 grams of cuprous chloride and 600 grams of sulfolane, add 6160 grams of carbon tetrachloride, steam into the stainless steel autoclave jacket, start the stirring of the autoclave , when the temperature of the autoclave material system rose to 80°C, the steam was stopped, and 1500 grams of vinyl chloride were pressed. After stirring for 2 hours, continue to open the jacket steam valve. After the temperature of the reaction system reaches 120° C., control the temperature of the reaction system to maintain at 110 to 125° C., and keep the reaction system in this temperature range for 11 hours. Cool down to 60 DEG C then, open the discharge bottom valve of autoclave, obtain crude pentachloropropane 5034 grams.

[0025] The 5L four-necked glass flask has a Φ40×2000 glass column, which is filled with a 1900 mm high glass ring packing, and a condenser and a cock for adjusting the reflux ratio are installe...

Embodiment 3

[0029]10L stainless steel autoclave with jacket and cooling water coil, add 200 grams of cuprous chloride, 200 grams of dimethylformamide and 500 grams of sulfolane, add 6160 grams of carbon tetrachloride, and feed into the stainless steel autoclave jacket Steam heating, start the stirring of autoclave, when autoclave material system temperature rises to 80 ℃, stop passing steam, press into 1750 grams of vinyl chloride. After stirring for 2 hours, continue to open the jacket steam valve. After the temperature of the reaction system reaches 130° C., control the temperature of the reaction system to maintain at 125 to 130° C., and keep the reaction system in this temperature range for 9 hours. Cool down to 60 DEG C then, open the discharge bottom valve of autoclave, obtain crude pentachloropropane 6002 grams.

[0030] The 5L four-necked glass flask has a Φ40×2000 glass column, which is filled with a 1900 mm high glass ring packing, and a condenser and a cock for adjusting the re...

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PUM

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Abstract

A monochloro-fluoropropene preparation belongs to the intermediate preparation technical field of coolant, foaming agent and fluorine compounds, which comprises that under catalyst condition, the telomeric reaction on chloromethane and chloroalkene is processed to prepare pentachloro-propane, which is fluorinated with hydrogen fluoride via the catalysis of composite catalyst to prepare trifluoro-dichloropropane, and hydrogen chloride is removed via the alkali alcohol liquid catalysis to obtain monochloro-fluoropropene as final product. The invention has the advantages that the preparation fluorinates pentachloro-propane into trifluoro-dichloropropane, to remove hydrogen chloride to obtain monochloro-fluoropropene, thereby avoiding azeotropic material and sub isomer generated in the fluorination from pentachloro-propane to monochloro-fluoropropene, while the whole process has low reaction temperature to save energy, and the monochloro-fluoropropene product has reach 99.0-99.6% purity and 80.70-88.05% yield, to meet industrial batch production.

Description

technical field [0001] The invention belongs to the technical field of preparation of intermediates of refrigerants, blowing agents and fluorine compounds, and in particular relates to a preparation method of chlorotrifluoropropene. Background technique [0002] Chlorotrifluoropropene (HCFC-1233zd) is a high-efficiency refrigerant, foaming agent and intermediate of fluorine compounds, and it is mainly an intermediate raw material for the preparation of pentafluoropropane (HFC-245fa). Since pentafluoropropane is the main substitute of monofluorodichloroethane (141b), with the acceleration of the process of monofluorodichloroethane being replaced, the amount of pentafluoropropane will increase accordingly, so that as pentafluoropropane Chlorotrifluoropropene, an intermediate of fluoropropane, has a good industrial application background. [0003] The traditional method of preparing chlorotrifluoropropene is: firstly, pentachloropropane is prepared by telomerization reaction o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/20C07C17/269
CPCY02P20/10
Inventor 司林旭
Owner CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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