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Method for preparing hexafluorobutadiene

A technology of hexafluorobutadiene and hydrofluorochlorobutane, which is applied to the preparation of halogenated hydrocarbons, preparation of dehydrohalogenation, chemical instruments and methods, etc., and can solve problems such as harsh reaction conditions, high raw material prices, and difficult handling of reagents , to achieve the effect of high added value, simple process and convenient operation

Active Publication Date: 2016-03-16
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its advantages are short steps, simple process, and few by-products; but there are also disadvantages such as high raw material prices, harsh reaction conditions, relatively low yield, and difficult handling of reagents used.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] in CHF 2 CCl 2 F and H 2 As the reaction raw material, CHF is prepared by continuous flow hydrodechlorination coupling reaction 2 CClFCClFCHF 2 . The reaction is carried out in a plug-flow tube reactor. The reaction tube of the tube reactor adopts an inner diameter of 18mm and a Ni tube of 50cm in length, and is placed in a tube furnace to heat up. In order to prevent material condensation, all reactions The connecting pipeline is made of stainless steel pipe, and the temperature is kept at about 80°C with the insulation heating jacket, and the H 2 Using a mass flow meter to control the flow rate (400mL / min), the CHF 2 CCl 2 F placed in a bubbler, with the aforementioned H 2 entrained CHF 2 CCl 2 F, adjust the temperature of the bubbler, adjust H 2 Flow and CHF 2 CCl 2 The flow ratio of F is 4, the reaction temperature is stable at 200° C., and the reaction pressure is normal pressure. Before the reaction, set the surface area to 500m 2 / g SiO 2 Using the...

Embodiment 2

[0036] With 1,2-dichloro-1,1,2-trifluoroethane (CHClFCClF 2 , HCFC-123a) and H 2 As the reaction raw material, CClF was prepared by continuous flow hydrodechlorination coupling reaction 2 CHFCHFCClF 2 . The reaction is carried out in a plug-flow tube reactor. The reaction tube of the tube reactor adopts an inner diameter of 18mm and a Ni tube of 50cm in length, and is placed in a tube furnace to heat up. In order to prevent material condensation, all reactions The connecting pipeline is made of stainless steel pipe, and the temperature is kept at about 80°C with the insulation heating jacket, and the H 2 Adopt mass flowmeter to control flow rate (400mL / min), CHClFCClF 2 Placed in a bubbler, with the aforementioned H 2 CHClFCClF 2 , adjust the temperature of the bubbler, adjust H 2 Flow and CHClFCClF 2 The flow rate ratio is 6, the reaction temperature is stable at 330° C., and the reaction pressure is normal pressure. Before the reaction, set the surface area to 50m ...

Embodiment 3

[0038] The CHF that embodiment 1 is separated obtains 2 CClFCClFCHF 2 , to prepare hexafluorobutadiene by catalytic de-HCl reaction in a second fixed-bed reactor.

[0039] The reaction is carried out in a plug-flow tube reactor. The reaction tube of the tube reactor adopts an inner diameter of 18mm and a Ni tube of 50cm in length, and is placed in a tube furnace to heat up. In order to prevent material condensation, all reactions The connecting pipeline is made of stainless steel pipe, and the temperature is kept at about 80°C with a heat-insulating heating jacket, N 2 Using a mass flow meter to control the flow rate (500mL / min), the CHF 2 CClFCClFCHF 2 Placed in a bubbler, with the aforementioned N 2 entrained CHF 2 CClFCClFCHF 2 , adjust the temperature of the bubbler, adjust the N 2 Flow and CHF 2 CClFCClFCHF 2 The flow rate ratio is 5, the reaction temperature is stable at 350° C., and the reaction pressure is normal pressure. Before the reaction, Ba(NO 3 ) 2 a...

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Abstract

The invention discloses a method for preparing hexafluorobutadiene. The method comprises the following steps: carrying out a hydrogenation dechlorination dimerization reaction on 1,1-dichloro-1,2,2-trifluoroethane or 1,2-dichloro-1,1,2-trifluoroethane on a supported metal catalyst in H2 atmosphere, separating out a target product hexafluorobutadiene, carrying out gas phase thermal cracking on an intermediate hydroflurochlorobutane to remove HCl in order to prepare hexafluorobutadiene, filtering the product generated after above reactions, washing the filtered product with an alkali, washing the washed product with water, drying the product, compressing, and carrying out rectifying purification to obtain the highly pure hexafluorobutadiene. The method for preparing hexafluorobutadiene overcomes the disadvantages of long operating period, low unit volume output and large device investment of present technologies, and has the advantages of high yield, few steps, easy industrialization, realization of production of the highly pure hexafluorobutadiene through selection of reactants and control of reaction conditions, simple process, cheap and easily available raw material, low cost, facilitation of industrial production, continuous production, and great improvement of the unit device productivity.

Description

technical field [0001] The invention belongs to the technical field of chlorofluoroolefin preparation, and the method is a method for preparing hexafluorobutadiene through catalytic hydrogenation dechlorination dimerization. Background technique [0002] Hexafluorobutadiene (C 4 f 6 , also known as perfluorobutadiene), its main application is the plasma etching processing medium of semiconductor products. Compared with traditional plasma etching gas CF 4 、C 2 f 6 、C 3 f 8 , c-C 4 f 8 and NF 3 Compared to C 4 f 6 It has the characteristics of faster etch rate, high etch selectivity and high aspect ratio. At present, hexafluorobutadiene is mainly used for precision etching of critical dimensions (accuracy up to 100nm), and has better selectivity than other etching gases. in C 4 f 6 In the system of etching gas, the active radical CF x The density of (x=1~3) is lower than that of other perfluorocarbons as etching gas systems, and CF with low etching activity is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/20C07C17/26C07C17/25
CPCC07C17/25C07C17/26C07C21/20C07C19/10
Inventor 韩文锋唐浩东李瑛刘化章
Owner ZHEJIANG UNIV OF TECH
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