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

Preparation method of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene

A technology of hexafluorobutyne and butene, which is applied in the field of organic fluorine chemical synthesis, can solve problems such as complex reactions and harsh conditions, achieve simple operation, mild preparation conditions, avoid high temperature conditions, highly toxic reagents and expensive metal catalysts The effect of using

Active Publication Date: 2020-08-25
ELECTRIC POWER RES INST OF GUANGDONG POWER GRID
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of this, the application discloses a preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene, which can effectively solve the existing synthetic trans-1,1, The 1,4,4,4-hexafluoro-2-butene method has harsh conditions, complex reactions, severe high temperature conditions, and technical problems of highly toxic reagents and expensive metal catalysts

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 of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene
  • Preparation method of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene
  • Preparation method of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The embodiment of this application discloses according to figure 1 The reaction scheme for the preparation of trans-1,1,1,4,4,4-hexafluoro-2-butene, figure 1 The reaction route is that trifluorotrichloroethane reacts with zinc under hydrogen and nickel catalyst conditions to produce 2-hexafluorobutyne, and 2-hexafluorobutyne reacts with ethyl xanthate potassium under formic acid or water conditions Reaction to prepare trans-1,1,1,4,4,4-hexafluoro-2-butene, the specific steps are as follows:

[0048] 1. Under room temperature, trifluorotrichloroethane (1.86g, 10mmol) and hydrogen with a partial pressure of 2MPa are passed into an autoclave filled with granular 5mol% activated carbon-supported nickel (25wt%) catalyst, and the temperature is gradually raised. Heat to 140°C for 1 hour, monitor the reaction by gas chromatography, cool to room temperature after the reaction, add a small amount of water to the collected product, filter and extract three times with dichloromet...

Embodiment 2- Embodiment 13

[0052] The embodiment of the present application provides the test that changes the consumption of the catalyst of the step 1 of embodiment 1, catalytic reaction temperature, catalytic reaction time and hydrogen pressure, then measure the yield of the pale yellow intermediate of embodiment 2-embodiment 13 ,Specific steps are as follows:

[0053] According to the method of step 1 among the embodiment 1, according to the consumption of gac-loaded nickel catalyst of table 1, the pressure that feeds hydrogen in step 1, the test that reaction time in step 1, reaction temperature in step 1 carries out, in different catalyst consumption, Different hydrogen pressures, different reaction times of trifluorotrichloroethane under hydrogen and activated carbon-supported nickel catalysts, and different reaction temperatures of trifluorotrichloroethane under hydrogen and activated carbon-supported nickel catalysts to prepare intermediates, determination step 1 The yield of the intermediate, ...

Embodiment 14- Embodiment 20

[0059] The embodiment of the present application provides a test of changing the amount of zinc powder in step 2 of embodiment 1, the reaction temperature of step 2, and the reaction time of step 2, and then measuring the 2-hexafluorobutyne of embodiment 14-embodiment 20 The yield, the specific steps are as follows:

[0060] According to the method of step 2 in embodiment 1, according to the solvent that adopts in the zinc powder consumption of table 2, step 2, reaction time in step 2, the test that reaction temperature carries out in step 2, in the consumption of different zinc powders, different kinds 2-hexafluorobutyne was prepared at different solvents, different reaction times and different reaction temperatures, and the yield of 2-hexafluorobutyne was measured. The results are shown in Table 2.

[0061] Table 2

[0062] Example Amount of zinc powder / equivalent solvent Reaction time / h Yield of 2-hexafluorobutyne / % 14 1 Acetic anhydride 10 80 ...

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 belongs to the field of organic fluorine chemical synthesis, and particularly relates to a preparation method of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene. The invention discloses a preparation method of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene, which comprises the following steps: by using trifluorotrichloroethane as a starting raw material, respectively carrying out reduction dimerization reaction and dechlorination reaction under the actions of hydrogen and metal zinc powder to obtain 2-hexafluorobutyne; and enabling 2-hexafluorobutyne to react with potassium ethyl xanthateor sodium ethyl xanthate, formic acid or water to obtain trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene. The invention discloses a preparation method of trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene, and can effectively solve the technical problem that an existing method for synthesizing trans-1, 1, 1, 4, 4, 4-hexafluoro-2-butene is harsh in condition and complex in reaction and needs severe high-temperature conditions, highly toxic reagents and expensive metal catalysts is solved.

Description

technical field [0001] The application belongs to the field of organic fluorine chemical synthesis, and in particular relates to a preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene. Background technique [0002] Trans-1,1,1,4,4,4-hexafluoro-2-butene (CAS: 66711-86-2) is a new type of environmentally friendly insulating gas with a global warming potential (GWP) of 18 , the comprehensive greenhouse effect index ratio of SF 6 Reduced by 99.9%, under certain conditions its insulation performance can reach SF 6 More than 95% of the total, there is a great potential to replace SF 6 Gas can be used as the choice of gas medium for subsequent development of medium-voltage electrical equipment and high-voltage electrical equipment. In addition, due to its unique properties, trans-1,1,1,4,4,4-hexafluoro-2-butene can also be used in organic Rankine cycle, heat pump, blowing agent, propellant , fire extinguishing agent, refrigerant, organic solvent and organic chemical reac...

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): C07C17/354C07C21/18
CPCC07C17/354C07C21/18
Inventor 李丽孙东伟唐念周永言
Owner ELECTRIC POWER RES INST OF GUANGDONG POWER GRID
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