Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method for 2,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and pentafluoropropane, which is applied in the field of preparation of fluorine-containing olefins, can solve the problems of large equipment investment, long process route, and high separation cost, and achieve the effects of simplified process, short process flow and simple process

Active Publication Date: 2017-01-11
JUHUA GROUP TECH CENT
View PDF13 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nevertheless, the methods and processes provided by these patents still have the disadvantages of many and complicated steps, large equipment investment, and high separation costs.
[0004] CN105111038A discloses that methylmagnesium chloride and tetrafluoroethylene are used as starting materials to generate 1,1,2-trifluoropropene successively through nucleophilic addition-elimination, and then 1,1,2-trifluoropropene is added with fluorine to generate 1,1,1,2,2-pentafluoropropane, finally 1,1,1,2,2-pentafluoropropane dehydrofluorination three-step reaction method for preparing 2,3,3,3-tetrafluoropropene, but its The disadvantage is that the process route is still long

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method for 2,3,3,3-tetrafluoropropene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of 1,1,1,2,2-pentafluoropropane

[0030] Replace the 2L stainless steel autoclave with nitrogen three times, then add 250g of tetrahydrofuran solution of methylmagnesium chloride (concentration of methylmagnesium chloride is 2mol / Kg) and 750g of tetrahydrofuran, and feed pentafluorochloroethane while stirring at 50°C 160g, continue to react for 3 hours after passing through. After the reaction is over, stop stirring, cool to 0°C, and filter to obtain 1,1,1,2,2-pentafluoropropane synthetic liquid, which has a purity of 99.5% after rectification and purification. Based on methylmagnesium chloride, the yield of 1,1,1,2,2-pentafluoropropane is 81.3%.

[0031] (2) Preparation of 2,3,3,3-tetrafluoropropene

[0032] The 1,1,1,2,2-pentafluoropropane obtained by the reaction in step (1) is passed through a potassium hydroxide solution with an excess mass percent concentration of 40% and a temperature of 70°C, and the gas phase product is collected and dried, C...

Embodiment 2

[0035] (1) Preparation of 1,1,1,2,2-pentafluoropropane

[0036] Replace the 2L stainless steel autoclave with nitrogen three times, then add 250g of tetrahydrofuran solution of methylmagnesium chloride (the concentration of methylmagnesium chloride is 2mol / Kg), 750g of tetrahydrofuran, and 200g of ethylene glycol dimethyl ether, and stir at 60°C 350 g of pentafluorochloroethane was passed through, and the reaction was continued for 1 hour after the passage was completed. After the reaction is finished, stop stirring, cool to 5°C, and filter to obtain 1,1,1,2,2-pentafluoropropane synthetic liquid, which has a purity of 99.5% after rectification and purification. Based on methylmagnesium chloride, the yield of 1,1,1,2,2-pentafluoropropane is 85.6%.

[0037] (2) Preparation of 2,3,3,3-tetrafluoropropene

[0038] The 1,1,1,2,2-pentafluoropropane obtained by the reaction in step (1) is passed through a sodium hydroxide solution with an excess mass percentage concentration of 60% ...

Embodiment 3

[0041] (1) Preparation of 1,1,1,2,2-pentafluoropropane

[0042]Replace the 2L stainless steel autoclave with nitrogen for three times, then add 250g of tetrahydrofuran solution of methylmagnesium chloride (the concentration of methylmagnesium chloride is 2mol / Kg) and 750g of tetrahydrofuran, and feed pentafluorochloroethane while stirring at 20°C 200g, continue to react for 5 hours after passing through. After the reaction is finished, stop stirring, cool to 10°C, and filter to obtain 1,1,1,2,2-pentafluoropropane synthetic liquid, the purity of which is 99.5% after rectification and purification. Calculated on the basis of methylmagnesium chloride, the yield of 1,1,1,2,2-pentafluoropropane is 73.5%.

[0043] (2) Preparation of 2,3,3,3-tetrafluoropropene

[0044] The 1,1,1,2,2-pentafluoropropane obtained by the reaction in step (1) is passed through a calcium hydroxide solution with an excess mass percent concentration of 20% and a temperature of 90°C, and the gas phase produ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method for 2,3,3,3-tetrafluoropropene. The preparation method comprises the following steps: (a) reacting chloropenta fluoroethane and methylmagnesium chloride in an organic solvent, and after the reaction is ended, performing cooling, filteration and rectification to obtain 1,1,1,2,2-perfluoropropane, wherein the methylmagnesium chloride and the chloropenta fluoroethane are in the molar ratio of 1:(1-5), the reacting temperature is 20 to 60 DEG C, and the reacting time is 1 to 5 hours; (b) introducing the 1,1,1,2,2-perfluoropropane which is obtained in the step (a) into an alkaline liquor at 50 to 90 DEG C, collecting a gas product, and drying and condensing the gas product to obtain the product, namely, the 2,3,3,3-tetrafluoropropene; or performing gas phase catalysis on the 1,1,1,2,2-perfluoropropane which is obtained in the step (a) under the action of a catalyst to remove HF and obtain the 2,3,3,3-tetrafluoropropene. The preparation method for the 2,3,3,3-tetrafluoropropene has the advantages that the process is simple, raw materials are easily obtained, and the cost is low.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing olefin, in particular to a preparation method of 2,3,3,3-tetrafluoropropene. Background technique [0002] 2,3,3,3-Tetrafluoropropene, the molecular formula is CF 3 CF=CH 2 , boiling point -28.3°C, CAS number: 754-12-1, its ODP is 0, GWP is 4, it has good life cycle climate performance, the atmospheric life is only 11 days; it has excellent physical and chemical properties, its molecular weight and HFC-134a Similar to HFC-134a, it has a lower boiling point and a higher saturated vapor pressure at room temperature, and has a similar density and critical point to HFC-134a, so it is considered to be a "direct substitute" for HFC-134a and has become the most potential No. One of the four generations of low-carbon refrigerants. [0003] According to literature and patents, the current synthesis routes of 2,3,3,3-tetrafluoropropene mainly include: tetrafluoroethylene method, trifluoropro...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C17/25C07C21/18C07C17/00C07C19/12
CPCC07C17/00C07C17/25C07C17/26C07C21/18C07C19/08C07C19/12
Inventor 李宏峰徐晓波黄雪浩马利勇
Owner JUHUA GROUP TECH CENT
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com