Method for preparing hexafluorobutadiene

A technology of hexafluorobutadiene and bromotrifluoroethylene, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of increased production cost, increased amount of three wastes, and unfavorable industrial application, etc., reaching The effect of reducing raw material cost, improving raw material utilization, and mild reaction conditions

Pending Publication Date: 2020-06-23
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The optimal yield of this method is only 56%, and the equivalent ferric chloride needs to be used as the coupling oxidant, which not only i

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  • Method for preparing hexafluorobutadiene

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Experimental program
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Effect test

Embodiment 1

[0037] Add palladium chloride 0.71g (4mmol) in the 500mL three-necked glass reactor that condensing reflux tube is housed, triphenylphosphine 4.2g (16mmol), then add the N of trifluorovinyl zinc bromide in this reaction bottle, N-dimethylformamide solution 380g (mass fraction 24%, 0.4mol), control internal temperature 20 ℃, slowly pass through 64.0g of trifluoroethylene bromide, the gas generated is collected by liquid nitrogen cold trap. After the passage of bromotrifluoroethylene, the reaction solution was kept warm for 3 hours, then heated up to 130° C., and all the gas was evaporated. A total of 54.5 g of the gas was collected and analyzed by chromatography. The results are shown in the following table:

[0038] Trifluoroethylene Bromotrifluoroethylene Hexafluorobutadiene other 2.77％ 4.83％ 91.80％ 0.60％

[0039] Based on bromotrifluoroethylene, the reaction yield was 77.2%.

Embodiment 2

[0041] Add 0.90g (4mmol) of palladium acetate and 4.2g (16mmol) of triphenylphosphine in a 500mL three-necked glass reactor equipped with a condensing reflux tube, and then add N, N of trifluorovinyl zinc bromide to the reaction flask. - Dimethylformamide solution 380g (mass fraction 24%, 0.4mol), control internal temperature 20 ℃, slowly pass through 64.0g trifluoroethylene bromide, the gas generated is collected by liquid nitrogen cold trap. After the passage of bromotrifluoroethylene, the reaction solution was kept warm for 3 hours, then heated up to 130° C., and all the gas was evaporated. A total of 56.5 g of the gas was collected and analyzed by chromatography. The results are shown in the following table:

[0042] Trifluoroethylene Bromotrifluoroethylene Hexafluorobutadiene other 2.51％ 10.30％ 86.80％ 0.39％

[0043] Based on bromotrifluoroethylene, the reaction yield is 75.7%.

Embodiment 3

[0045] Add palladium diacetylacetonate [Pd(acac) 2 ] 1.22g (4mmol), diphenylethoxyphosphine 3.68g (16mmol), then in this reaction bottle, add the N of trifluorovinyl zinc bromide, N-dimethylformamide solution 380g (mass fraction 24 %, 0.4mol), and the internal temperature was controlled at 20°C, and 64.0 g of bromotrifluoroethylene was slowly introduced, and the generated gas was collected with a liquid nitrogen cold trap. After the passage of bromotrifluoroethylene, the reaction solution was kept warm for 3 hours, then heated up to 130° C., and all the gas was evaporated. A total of 53.9 g of the gas was collected and analyzed by color chromatography, and the results were as follows;

[0046] Trifluoroethylene Bromotrifluoroethylene Hexafluorobutadiene other 3.51％ 25.58％ 70.21％ 0.70％

[0047] Based on bromotrifluoroethylene, the reaction yield was 58.4%.

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Abstract

The invention discloses a method for preparing hexafluorobutadiene. The method is realized by carrying out a coupling reaction between trifluorobromoethylene and trifluorovinyl zinc bromide under theaction of a composite catalyst containing a transition metal compound and an organic phosphorus compound. The provided preparation method has the advantages of high reaction yield, low raw material cost, small amount of three wastes, simple process, mild reaction conditions, and simple process operation.

Description

technical field [0001] The invention relates to a method for preparing perfluoroconjugated olefins, in particular to a method for preparing hexafluorobutadiene. Background technique [0002] Hexafluorobutadiene (C4F6) has a low fluorocarbon ratio (F:C=1.5). As an electronic etching gas, it can etch electronic products with a precision below 100nm. It can be used to manufacture a new generation of 3D NAND flash memory. Key electronic etching gas for high-end chips. In addition to its excellent etching performance, hexafluorobutadiene also has good environmental performance, its ODP=0, GWP(100)=290, and its existence time in the atmosphere is only 1.9d, which is a kind of extremely low greenhouse effect, Green and environmentally friendly etching gas. [0003] For the preparation of hexafluorobutadiene, the prior art makes the following contributions: [0004] US289404 discloses 1,2-dichlorodifluoroethylene in F 2 There is a method of down-regulating the polymerization to ...

Claims

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Application Information

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IPC IPC(8): C07C17/263C07C21/18
CPCC07C17/263C07C21/18Y02P20/584
Inventor 吴海锋谢浩杰刘辉刘武灿陈先进赵翀
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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