Methods for purifying halosilane-containing streams
View Patent ↗Methods for purifying a halosilane-containing process stream include a process stream purified by removing arsenic and phosphorous impurities by use of distillation.
1. A method for purifying a halosilane-containing stream, the halosilane-containing stream comprising a halosilane, arsenic and phosphorous, the method comprising introducing the halosilane-containing stream into a distillation column to produce an overhead fraction containing halosilane and less than about 50% of the arsenic introduced into the distillation column in the halosilane-containing stream and less than about 50% of the phosphorous introduced into the distillation column in the halosilane-containing stream, the halosilane-containing stream not being contacted with a complexing agent prior to or during distillation and not being a product stream of a previous distillation column operation, the distillation column operating with a reflux ratio of about 50 or less, the distillation column including packing or plates, wherein when the distillation column includes packing, the distillation column includes less than about 100 theoretical stages, and when the distillation column includes plates, the distillation column includes less than about 100 plates.
2. The method of claim 1 , wherein the distillation column includes packing, the distillation column having a height equivalent of a theoretical stage of between about 0.25 meters and about 0.75 meters.
3. The method of claim 1 , wherein the distillation column includes packing, the packing being a structured packing.
4. The method of claim 1 , wherein the distillation column operates at a reflux ratio of less than about 30.
5. The method of claim 1 , wherein the overhead fraction contains less than about 50 ppbw arsenic-containing compounds.
6. The method of claim 1 , wherein the overhead fraction contains less than about 50 ppbw phosphorous-containing compounds.
7. The method of claim 1 , wherein the overhead fraction contains less than about 10% of the arsenic introduced into the distillation column in the halosilane-containing stream.
8. The method of claim 1 , wherein the overhead fraction contains less than about 10% of the phosphorous introduced into the distillation column in the halosilane-containing stream.
9. The method of claim 1 , wherein the halosilane-containing stream contains arsenic-containing compounds of about 1 ppbw or more.
10. The method of claim 1 , wherein the halosilane-containing stream contains phosphorous-containing compounds of about 1 ppbw or more.
11. The method of claim 1 , wherein the temperature of the overhead fraction is from about 70° C. to about 135° C.
12. The method of claim 1 , wherein the pressure of the overhead fraction is about 1.5 bar or more.
13. The method of claim 1 , wherein a bottoms fraction is produced from the distillation column, the bottoms fraction containing less than about 15% of the halosilane introduced into the column in the halosilane-containing stream.
14. The method of claim 1 , wherein the halosilane-containing stream is a gas, the method further comprising the step of condensing the halosilane-containing stream prior to introduction into the distillation column.
15. The method of claim 1 , wherein the halosilane-containing stream is a liquid.
16. The method of claim 1 , wherein the halosilane contains a halogen selected from group consisting of chlorine, bromine and iodine.
17. The method as set forth in claim 1 , wherein:
at least about 50% of the arsenic in the halosilane-containing stream prior to or during distillation is present as AsX 3 , AsHX 2 , and AsH 2 X, or other arsenic compounds having 5 or less atoms, wherein X is a halogen; and
at least about 50% of the phosphorous in the halosilane-containing stream prior to or during distillation is present as PX 3 , PHX 2 , and PH 2 X, or as other phosphorous compounds having 5 or less atoms.
18. The method as set forth in claim 1 , wherein:
at least about 90% of the arsenic in the halosilane-containing stream prior to or during distillation is present as AsX 3 , AsHX 2 , and AsH 2 X, or other arsenic compounds having 5 or less atoms, wherein X is a halogen; and
at least about 90% of the phosphorous in the halosilane-containing stream prior to or during distillation is present as PX 3 , PHX 2 , and PH 2 X, or as other phosphorous compounds having 5 or less atoms.
19. The method as set forth in claim 1 , wherein:
at least about 99% of the arsenic in the halosilane-containing stream prior to or during distillation is present as AsX 3 , AsHX 2 , and AsH 2 X, or other arsenic compounds having 5 or less atoms, wherein X is a halogen; and
at least about 99% of the phosphorous in the halosilane-containing stream prior to or during distillation is present as PX 3 , PHX 2 , and PH 2 X, or as other phosphorous compounds having 5 or less atoms.