Method for synthesizing hexafluoro-1,3-butadiene

A technology of butadiene and trifluoroethylene, which is applied in the field of synthesizing hexafluoro-1,3-butadiene, can solve the problems of restricting the industrial production of hexafluorobutadiene, and achieve safe synthesis process, high yield, and source convenient effect

Active Publication Date: 2015-08-19
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These all limit the industrial production of hexafluorobutadiene

Method used

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  • Method for synthesizing hexafluoro-1,3-butadiene

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Experimental program
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Effect test

Embodiment 1

[0036] (1) Load 20ml of Cr-Mg catalyst into a fixed bed reactor. Under the protection of 50ml of nitrogen, the catalyst was first dried at 10°C / min to 200°C for 2 hours, then raised to 400°C at a rate of 10°C / min and dried for 2 hours, then cooled to 330°C, and then passed through The catalyst was activated with 50 ml / min of hydrogen fluoride (HF) gas for 2 hours. This completes the catalyst activation process.

[0037] Heat the reactor to 350°C, then, 50ml / min tetrafluoroethane and 10ml / min nitrogen enter the mixing chamber together and mix well. Afterwards, through the reactor until the buffer bottle, water washing bottle, concentrated alkali solution, and liquid bromine absorption pool, after the experiment, the product is mainly distributed in the cooling collector. The collected product was subjected to GC analysis. GC results showed that the product contained 95.0% 1,2-dibromo-1,1,2-trifluoroethane. Since trifluoroethylene reacts very quickly with liquid bromine, in ...

Embodiment 2

[0041] (1) 20ml of Cr-Fe-Zn catalyst is loaded into a fixed-bed reactor, and the fixed-bed reactor is heated with an open-type tube heating furnace. Under the protection of 50ml of nitrogen, the catalyst was first dried at 10°C / min to 200°C for 2 hours, then raised to 400°C at a rate of 10°C / min and dried for 2 hours, then cooled to 330°C, and then passed through The catalyst was activated with 50 ml / min of hydrogen fluoride (HF) gas for 2 hours. This completes the catalyst activation process.

[0042]Heat the reactor to 350°C, then, 50ml / min tetrafluoroethane and 10ml / min nitrogen enter the mixing chamber together and mix well. After that, it goes through the reactor until buffer bottle, washing bottle, concentrated alkali solution, and liquid bromine absorption pool. After the experiment, the product is mainly distributed in the cooling collector. The collected product was subjected to GC analysis. GC results showed that the product contained 90.0% 1,2-dibromo-1,1,2-trif...

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Abstract

The invention relates to a method for synthesizing hexafluoro-1,3-butadiene, and belongs to the field of organic chemistry synthesis. The method for synthesizing hexafluoro-1,3-butadiene comprises the following steps: removing hydrogen fluoride from tetrafluoro ethane (HFC-134a) under the action of a catalyst to generate trifluoroethylene; rapidly reacting trifluoroethylene with liquid bromine to generate 1,2-dibromo-1,1,2-trifluoroethane, and removing hydrogen bromide under alkaline conditions to obtain trifluorobromoethylene; and reacting trifluorobromoethylene with activated zinc powder and N,N-dimethyl formamide to generate trifluorovinylzinc, and carrying out a coupling reaction on trifluorovinylzinc under the action of Fe<3+> to generate hexafluoro-1,3-butadiene. A solvent can be recovered after above reactions. The method has the advantages of low price and convenient source of raw materials, good stability and long service of the catalyst, simple separation and purification of the above product, and easy industrial production.

Description

technical field [0001] The invention is a method for synthesizing hexafluoro-1,3-butadiene, and relates to a method for synthesizing hexafluoro-1,3-butadiene in an industrialized method. Background technique [0002] Hexafluoro-1,3-butadiene has high industrial value and is a widely used industrial raw material. Its downstream products can be used in precision electronic circuit board cleaning agents, pesticides and insecticides, and in fluorine-containing pharmaceutical intermediates It has high application value in the synthesis of fluorine-containing fine chemicals. In the synthesis of fluorine-containing polymers, it can be used as a polymer monomer to prepare polyhexafluorobutadiene, and it can also be used with other monomers to synthesize fluorine-containing rubber and resins with excellent electrical properties. The current experimental results show that hexafluoro-1,3-butadiene has great application potential in dry etching of VLSI circuits. [0003] At present, m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/269C07C21/20
CPCY02P20/582
Inventor 权恒道周彪周晓猛
Owner 泉州宇极新材料科技有限公司
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