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A kind of preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene

A technology for hexafluorobutyne and butene, applied in the field of organic fluorine chemical synthesis, can solve the problems of complex reaction and harsh conditions, and achieve the effects of simple operation, mild preparation conditions and high yield

Active Publication Date: 2021-09-03
ELECTRIC POWER RES INST OF GUANGDONG POWER GRID
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  • Abstract
  • Description
  • Claims
  • Application Information

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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

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  • A kind of preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene
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  • A kind of preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene

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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 ...

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Abstract

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. The present application discloses a preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene, comprising the following steps: using trifluorotrichloroethane as a starting material, in hydrogen and metallic zinc Reductive dimerization reaction and dechlorination reaction respectively occur under the action of powder to obtain 2-hexafluorobutyne; react 2-hexafluorobutyne with potassium ethyl xanthate or sodium ethyl xanthate, formic acid or water to obtain trans-1,1,1,4,4,4-hexafluoro-2-butene. This application discloses a preparation method of trans-1,1,1,4,4,4-hexafluoro-2-butene, which can effectively solve the existing synthetic trans-1,1,1,4,4, The 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.

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

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Application Information

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Patent Type & Authority Patents(China)
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
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