Process for separating hydrogen fluoride from organic feedstocks
View Patent ↗Provided is a process for purifying an organic feedstock comprising (a) distilling a raw organic feedstock comprising hydrogen fluoride, 2-chloro-1,1,1,2-tetrafluoropropane, and 2-chloro-3,3,3-trifluoropropene to produce a first distillate stream comprising an azeotrope-like composition of 2-chloro-1,1,1,2-tetrafluoropropane, 2-chloro-3,3,3-trifluoropropene, and hydrogen fluoride, and a first bottoms stream rich in hydrogen fluoride; (b) cooling said first distillate stream to produce an intermediate composition comprising an organic layer rich in 2-chloro-1,1,1,2-tetrafluoropropane and 2-chloro-3,3,3-trifluoropropene, and an acid layer rich in hydrogen fluoride; and, optionally but preferably, (c) distilling said organic layer to produce a second distillate stream comprising an azeotrope-like composition of 2-chloro-1,1,1,2-tetrafluoropropane, 2-chloro-3,3,3-trifluoropropene, and hydrogen fluoride, and a second bottoms stream comprising a purified organic feedstock substantially free of hydrogen fluoride.
1. A process for preparing 2-chloro-1,1,1,2-tetrafluoropropane comprising:
a. reacting a first feed stream comprising 2-chloro-3,3,3-trifluoropropene with a second feed stream comprising hydrogen fluoride, and optionally with one or more recycle streams comprising hydrogen fluoride, to produce a crude product stream comprising 2-chloro-1,1,1,2-tetrafluoropropane, hydrogen fluoride, and 2-chloro-3,3,3-trifluoropropene;
b. distilling said crude product stream to produce a first distillate stream comprising an azeotrope-like composition of 2-chloro-1,1,1,2-tetrafluoropropane, 2-chloro-3,3,3-trifluoropropene, and hydrogen fluoride, and a first bottoms stream rich in hydrogen fluoride; and
c. cooling said first distillate stream to produce an intermediate composition comprising an organic layer rich in 2-chloro-1,1,1,2-tetrafluoropropane and 2-chloro-3,3,3-trifluoropropene, and an acid layer rich in hydrogen fluoride.
2. The process of claim 1 further comprising
d. distilling said organic layer to produce a second distillate stream comprising an azeotrope-like composition of 2-chloro-1,1,1,2-tetrafluoropropane, 2-chloro-3,3,3-trifluoropropene, and hydrogen fluoride, and a second bottoms stream comprising an organic composition rich in 2-chloro-1,1,1,2-tetrafluoropropane and substantially free of hydrogen fluoride.
3. The process of claim 2 wherein said cooling produces a first distillate stream having a temperature of about −30° C. to about +10° C.
4. The process of claim 3 wherein said second bottoms stream comprises at least about 80 weight percent of the combined mass of said 2-chloro-1,1,1,2-tetrafluoropropane and 2-chloro-3,3,3-trifluoropropene in said crude product stream.
5. The process of claim 4 wherein said crude product stream comprises about 60 to about 70 weight percent hydrogen fluoride.
6. The process of claim 5 further comprising reboiling said first bottoms stream to produce a first recycle stream comprising at least about 95 weight percent hydrogen fluoride, wherein said first recycle stream is combined with said second feed stream prior to step (a) and/or is introduced into step (a) as said one or more recycle streams.
7. The process of claim 5 further comprising combining said acid layer with said second feed stream prior to step (a) and/or introducing said acid layer into step (a) as said one or more recycle streams, wherein said acid layer comprises at least about 80 weight percent hydrogen fluoride.
8. The process of claim 5 further comprising combining said second distillate stream with said second feed stream prior to step (a) and/or introducing said acid layer into step (a) as said one or more recycle streams.