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A method for synthesizing trans-1,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and pentafluoropropane, which is applied in the field of synthesizing trans-1,3,3,3-tetrafluoropropene, can solve the problems of unfriendly environment, troublesome post-processing, and difficult to recycle, and achieve an environment-friendly Effect

Active Publication Date: 2019-06-18
陕西延长石油集团氟硅化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned synthetic E-HFO-1234ze technology, HFC-245fa alkali stripping method uses organic solvents such as dimethyl sulfoxide, tetrahydrofuran and acetonitrile. Such organic solvents are miscible with alkaline aqueous solution and are difficult to recover, and fluoride salts are formed after the reaction (Potassium fluoride, sodium fluoride) solid waste, troublesome post-processing, unfriendly to the environment

Method used

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  • A method for synthesizing trans-1,3,3,3-tetrafluoropropene
  • A method for synthesizing trans-1,3,3,3-tetrafluoropropene
  • A method for synthesizing trans-1,3,3,3-tetrafluoropropene

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Effect test

Embodiment 1

[0015] The reaction was carried out in a stirred 500mL stainless steel autoclave. Put 5.2g of highly active anhydrous potassium fluoride, 119g of N,N-dimethylformamide, and 119g of HFC-245fa into the reaction kettle in sequence, start stirring, raise the reaction temperature to 120°C, and keep the reaction temperature after 8 hours of reaction , from the gas phase port of the reactor, the reaction materials such as HFC-245fa, HFO-1234ze and HF with low boiling point are slowly exhausted. The conversion of -245fa was 55.9%, the overall selectivity of HFO-1234ze(E / Z) was 99.5%, and the selectivity of E-HFO-1234ze was 81.4%.

Embodiment 2

[0017] Add 119g of HFC-245fa to the reaction kettle after the reaction in Example 1, and continue to heat up to 120°C for reaction. Analysis of the reaction products showed that the conversion rate of HFC-245fa was 55.3%, the total selectivity of HFO-1234ze (E / Z) was 99.6%, and the selectivity of E-HFO-1234ze was 82.1%. The results of Comparative Example 1 show that the potassium fluoride and organic solvents after removal of HFC-245fa, HFO-1234ze and HF still have high reactivity and can continue to be used for the next batch of reactions.

Embodiment 3

[0019] The operation process of embodiment three is similar to embodiment one, and difference is to replace highly active anhydrous potassium fluoride with cesium fluoride, and reaction product analysis shows that the transformation efficiency of HFC-245fa is 60.5%, and HFO-1234ze (E / Z ) was 99.4% overall selectivity, wherein the selectivity of E-HFO-1234ze was 80.1%.

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Abstract

The invention discloses a method for synthesizing trans-1,3,3,3-tetrafluoropropylene. The method is characterized in that 1,1,1,3,3-perfluoropropane generates dehydrofluorination reaction to synthesize the trans-1,3,3,3-tetrafluoropropylene in the presence of alkali metal fluoride and an aprotic polar solvent, wherein a reaction temperature is 50-180 DEG C, and reaction time is 0.5-24 hours; the alkali metal fluoride is potassium fluoride or cesium fluoride; and the aprotic polar solvent is of an ester type, a nitrile type, a ketone type, an amide type or a sulfoxide type. The method for synthesizing trans-1,3,3,3-tetrafluoropropylene provided by the invention has the advantage of being environmental-friendly.

Description

technical field [0001] The present invention relates to a method for synthesizing trans-1,3,3,3-tetrafluoropropene, in particular, in the presence of alkali metal fluoride and aprotic polar solvent, 1,1,1,3,3 - A method for synthesizing trans-1,3,3,3-tetrafluoropropene by dehydrofluorination reaction of pentafluoropropane. Background technique [0002] The ozone depletion value (ODP) of trans-1,3,3,3-tetrafluoropropene (E-HFO-1234ze) is 0, and the greenhouse effect potential value (GWP) is 6, which is recognized by the international community as a high GWP Ideal low-carbon and environmentally friendly substitutes for hydrofluorocarbons (HFCs), such as blowing agents to replace 1,1,3,3,3-pentafluoropropane (HFC-245fa), 1,1,1,2-tetrafluoroethane Alkanes (HFC-134a) and 1,1-difluoroethane (HFC-152a), as an aerosol propellant to replace HFC-134a, etc. [0003] Chinese patent CN104177219A reports that in the presence of solvents including organics containing alkyl and aryl nitri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/25C07C21/18
CPCC07C17/25C07C21/18
Inventor 种欣睿唐晓博李宝太曾纪珺付旭东张伟李立韩升聂剑飞吕剑马家琪李强
Owner 陕西延长石油集团氟硅化工有限公司
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