Production process for 1,2,3,4-tetrachlorohexafluorobutane and refining process
View Patent ↗The production process for 1,2,3,4-tetrachlorohexafluorobutane of the present invention is characterized in that 1,2,3,4-tetrachlorobutane is reacted with fluorine in the presence of a solvent containing hydrogen fluoride. The 1,2,3,4-tetrachlorobutane may be obtained by chlorination of 3,4-dichlorobutene-1. Further, the present invention provides as well a process of refining 1,2,3,4-tetrachlorohexafluorobutane obtained in the manner described above. According to the present invention, 1,2,3,4-tetrachlorohexafluorobutane which is useful, for example, as a synthetic raw material for hexafluoro-1,3-butadiene used as an etching gas for semiconductors can industrially efficiently be produced by using 1,2,3,4-tetrachlorobutane which is a by-product of chloroprene and which has so far been disposed.
1. A production process for 1,2,3,4-tetrachlorohexafluorobutane characterized in that 1,2,3,4-tetrachlorobutane is reacted with fluorine under the presence of a solvent containing hydrogen fluoride, wherein an amount of hydrogen fluoride in the reaction solvent falls in a range of 10 to 60% by mass and a concentration of 1,2,3,4-tetrachlorobutane in the reaction solvent falls in a range of 10 to 50% by mass.
2. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in claim 1 , wherein a reaction temperature of the reaction falls in a range of −20° C. to 70° C.
3. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in claim 1 , wherein a reaction pressure of the reaction falls in a range of 0.1 MPa to 2.0 MPa.
4. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in claim 1 , wherein a concentration of the fluorine gas reacted with 1,2,3,4-tetrachlorobutane is 40% by volume or more.
5. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in claim 1 , wherein at least a part of 1,2,3,4-tetrachlorobutane is obtained by chlorination of 3,4-dichlorobutene-1.
6. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in claim 5 , wherein 1,2,3,4-tetrachlorobutane obtained by the chlorination of 3,4-dichlorobutene-1 described above contains a dl form which is an optical isomer of 1,2,3,4-tetrachlorobutane in an amount of 40% by mass or more.
7. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in claim 1 , wherein the solvent contains a chlorocarbon and/or a chlorofluorocarbon.
8. The production process for 1,2,3,4-tetrachlorohexafluorobutane as described in any of claims 1 to 7 , wherein a reaction liquid containing 1,2,3,4-tetrachlorohexafluorobutane produced by reacting 1,2,3,4-tetrachlorobutane with fluorine in the presence of the solvent containing hydrogen fluoride is introduced into a distillation column to separate at least a part of 1,2,3,4-tetrachlorohexafluorobutane from the reaction liquid; at least a part of the solvent containing hydrogen fluoride from which at least a part of 1,2,3,4-tetrachlorohexafluorobutane has been separated is returned to a reaction apparatus in which 1,2,3,4-tetrachlorobutane is reacted with fluorine to be cyclically used.
9. A refining process of 1,2,3,4-tetrachlorohexafluorobutane, wherein a reaction liquid containing 1,2,3,4-tetrachlorohexafluorobutane produced by reacting 1,2,3,4-tetrachlorobutane with fluorine in the presence of a solvent containing hydrogen fluoride is introduced into a distillation column to separate at least a part of 1,2,3,4-tetrachlorohexafluorobutane from the reaction liquid; and the separated 1,2,3,4-tetrachlorohexafluorobutane is brought into contact with an alkaline substance and/or water.
10. The refining process of 1,2,3,4-tetrachlorohexafluorobutane as described in claim 9 , wherein 1,2,3,4-tetrachlorohexafluorobutane contacted with the alkaline substance and/or water is further brought into contact with a porous refining material.
11. The refining process of 1,2,3,4-tetrachlorohexafluorobutane as described in claim 10 , wherein the porous refining material is zeolite.