Process for producing hexafluoroethane and use thereof
View Patent ↗A process for producing hexafluoroethane, comprising a step of distilling a crude hexafluoroethane containing chlorine compounds each having two carbon atoms to distill out hexafluoroethane as a top flow from the top of a distillation column and separate a hexafluoroethane mixture containing the chlorine compounds as a bottom flow from the bottom, and a step of contacting the bottom flow with hydrogen fluoride in the gas phase at a temperature of 300 to 500° C. in the presence of a fluorination catalyst to fluorinate the chlorine compounds. This process provides hexafluoroethane which can be used mainly as a cleaning gas in the production process of a semiconductor device.
1. A process for producing hexafluoroethane, comprising a step of distilling a crude hexafluoroethane containing chlorine compounds each having two carbon atoms to distill out hexafluoroethane as a top flow from the top of a distillation column and separate a hexafluoroethane mixture containing said chlorine compounds as a bottom flow from the bottom of the distillation column, and a step of contacting said bottom flow with hydrogen fluoride in the gas phase at a temperature of 300 to 500° C. in the presence of a fluorination catalyst to fluorinate said chlorine compounds.
2. A process for producing hexafluoroethane, comprising (I) a step of producing a crude hexafluoroethane containing chlorine compounds each having two carbon atoms, (II) a step of distilling said crude hexafluoroethane to distill out hexafluoroethane as a top flow from the top of a distillation column and separate a hexafluoroethane mixture containing said chlorine compounds as a bottom flow from the bottom of the distillation column, and (III) a step of contacting said bottom flow with hydrogen fluoride in the gas phase at a temperature of 300 to 500° C. in the presence of a fluorination catalyst to fluorinate said chlorine compounds.
3. The process for producing hexafluoroethane as claimed in claim 1 , wherein the chlorine compound having two carbon atoms contained in said crude hexafluoroethane is at least one compound selected from the group consisting of dichlorotetrafluoroethane, chloropentafluoroethane, 1-chloro-2,2,2-trifluoroethane, 1,1-dichloro-2,2,2-trifluoroethane and 1-chloro-1,2,2,2-tetrafluoroethane.
4. The process for producing hexafluoroethane as claimed in claim 1 , wherein the top flow contains at least 80 vol % of the hexafluoroethane introduced into the distillation column.
5. The process for producing hexafluoroethane as claimed in claim 1 , wherein said fluorination catalyst is a supported or bulk catalyst comprising a trivalent chromium oxide as the main component.
6. The process for producing hexafluoroethane as claimed in claim 1 , wherein the molar ratio of the hydrogen fluoride to the hexafluoroethane mixture contained in said bottom flow (hydrogen fluoride/hexafluoroethane mixture) is from 0.05 to 10.
7. The process for producing hexafluoroethane as claimed in claim 1 , wherein the concentration of said chlorine compounds contained in said hexafluoroethane mixture is 1 vol % or less.
8. The process for producing hexafluoroethane as claimed in claim 1 , wherein said crude hexafluoroethane is a gas obtained by reacting dichlorotetrafluoroethane and/or chloropentafluoroethane with hydrogen fluoride in the gas phase in the presence of a fluorination catalyst.
9. The process for producing hexafluoroethane as claimed in claim 1 , wherein said crude hexafluoroethane is a gas obtained by reacting 1,1,1,2-tetrafluoroethane and/or pentafluoroethane, containing the chlorine compounds as impurities, with a fluorine gas.
10. The process for producing hexafluoroethane as claimed in claim 9 , wherein the reaction with the fluorine gas is carried out in a gas phase in the presence of a diluent gas.
11. The process for producing hexafluoroethane as claimed in claim 10 , wherein the diluent gas is a gas containing at least one of tetrafluoromethane, hexafluoroethane, octafluoropropane and hydrogen fluoride.
12. The process for producing hexafluoroethane as claimed in claim 10 , wherein the diluent gas is a gas rich in hydrogen fluoride.
13. The process for producing hexafluoroethane as claimed in claim 9 , wherein the reaction with the fluorine gas is carried out at a temperature of 250 to 500° C.
14. The process for producing hexafluoroethane as claimed in claim 9 , wherein the concentration of 1,1,1,2-tetrafluoroethane at the inlet of a reactor is 4 mol % or less in the reaction with the fluorine gas.
15. The process for producing hexafluoroethane as claimed in claim 9 , wherein the concentration of pentafluoroethane at the inlet of a reactor is 6 mol % or less in the reaction with the fluorine gas.
16. The process for producing hexafluoroethane as claimed in claim 9 , wherein the reaction with the fluorine gas is carried out under a pressure of 0 to 3 MPa.
17. The process for producing hexafluoroethane as claimed in claim 2 , wherein after removing acidic components from the gas obtained through said step (III), at least a part of said gas is re-circulated to the step (I) and/or the step (II).
18. The process for producing hexafluoroethane as claimed in claim 1 , wherein the hexafluoroethane mixture contains 90 mol % or more of CF 3 CF 3 .
19. The process for producing hexafluoroethane as claimed in claim 2 , wherein the hexafluoroethane mixture contains 90 mol % or more of CF 3 CF 3 .