Granted Patent B2

US 8,529,860 · App. 12/969,089 · Granted Sep 10, 2013

Abstract

Claims (40)

1. A method for producing silicon tetrafluoride, the method comprising:

contacting a fluoroaluminate feed comprising at least about 30% by weight fluoride salts of alkali metal or alkaline earth-metal and aluminum with an acid comprising hydrochloric acid and a source of silicon to thereby produce silicon tetrafluoride and at least one by-product.

2. The method as set forth in claim 1 wherein the feed is a by-product of silane production.

3. The method as set forth in claim 1 wherein silicon tetrafluoride is separated from the by-product to recover silicon tetrafluoride as a product.

4. The method as set forth in claim 1 wherein the source of silicon is selected from the group consisting of sand, quartz, flint, diatomite, mineral silicates, metallurgical grade silicon, fumed silica, fluorosilicates and mixtures thereof.

5. The method as set forth in claim 1 wherein the fluoride salt of alkali metal or alkaline earth-metal and aluminum is selected from the group consisting of NaAlF 4 , Na 5 Al 3 F 14 , Na 3 AlF 6 and mixtures thereof.

6. The method as set forth in claim 1 wherein hydrogen fluoride and a chloride or sulfate salt of alkali or alkaline earth-metal are produced as by-products.

7. The method as set forth in claim 6 wherein the hydrogen fluoride is contacted with a source of silicon to produce silicon tetrafluoride.

8. The method as set forth in claim 1 wherein the fluoride salt of alkali metal or alkaline earth-metal and aluminum and the source of silicon are introduced to a reaction vessel;

further wherein the fluoride salt of alkali metal or alkaline earth-metal and aluminum and the source of silicon are contacted in the reaction vessel with aqueous acid; and

further wherein said contact among the fluoride salt of alkali metal or alkaline earth-metal and aluminum, the source of silicon, and the aqueous acids produces a product gas comprising silicon tetrafluoride and a slurry containing a by-product.

9. The method as set forth in claim 8 wherein the fluoride salt of alkali metal or alkaline earth-metal and aluminum and the source of silicon are continuously fed to the reaction vessel and the slurry and product gas are continuously removed from the reaction vessel.

10. The method as set forth in claim 8 wherein the product gas comprises silicon tetrafluoride and hydrogen fluoride.

11. The method as set forth in claim 10 comprising separating hydrogen fluoride and silicon tetrafluoride in a distillation column.

12. The method as set forth in claim 9 wherein the slurry is introduced into a solid-liquid separation unit to produce a solid fraction and a liquid fraction, the solid fraction containing a chloride or sulfate salt of an alkali metal or alkaline earth-metal, the liquid fraction containing water, hydrogen fluoride, unreacted acid and a chloride or sulfate salt of an alkali metal or alkaline earth-metal.

13. The method as set forth in claim 12 comprising separating at least one of water, hydrogen fluoride and unreacted acid in a distillation column.

14. The method as set forth in claim 1 wherein the fluoride salt of alkali metal or alkaline earth-metal and aluminum and the source of silicon are contacted with substantially anhydrous acid and the fluoride salt and the source of silicon are introduced to a fluidized bed reactor which contains acid as a fluidizing gas.

15. The method as set forth in claim 14 wherein a product gas and particulate chloride or sulfate salt of alkali or alkaline earth-metal is produced in the fluidized bed reactor, the product gas comprising silicon tetrafluoride, hydrogen fluoride and unreacted acid.

16. The method as set forth in claim 15 comprising separating silicon tetrafluoride from at least one other gas in a distillation column.

17. The method as set forth in claim 1 wherein the fluoride salt is particulate with an average nominal diameter of less than about 500 μm.

18. The method as set forth in claim 1 wherein the acid and fluoride salt are added to a reaction vessel in a molar ratio of at least about 1:1.

19. The method as set forth in claim 1 wherein the source of silicon and fluoride salt are added to a reaction vessel in a molar ratio based on the number of silicon atoms and fluorine atoms of about 1:4.

20. The method as set forth in claim 1 wherein a source of silicon is added to a reaction vessel such that silicon atoms are added in at least about a 5% molar excess relative to fluorine atoms of the fluoride salts of alkali metal or alkaline earth-metal.

21. A method for producing silicon tetrafluoride, the method comprising:

contacting a fluoride salt of alkali metal or alkaline earth-metal and aluminum with an acid comprising hydrochloric acid and a source of silicon to thereby produce silicon tetrafluoride and at least one by-product; and

separating silicon tetrafluoride from the by-product to recover silicon tetrafluoride as a product.

22. The method as set forth in claim 21 wherein the silicon tetrafluoride is condensed for storage as a liquid product.

23. A method for producing silane and silicon tetrafluoride, the method comprising:

contacting silicon tetrafluoride and an alkali or alkaline earth-metal salt of aluminum tetrahydride to produce silane and an effluent comprising a fluoride salt of alkali metal or alkaline earth-metal and aluminum;

contacting the effluent with an acid comprising hydrochloric acid and a source of silicon to thereby produce silicon tetrafluoride and at least one by-product; and

separating the silicon tetrafluoride from the by-product.

24. The method as set forth in claim 23 wherein the silicon tetrafluoride is bubbled through a reaction solution that contains the aluminum tetrahydride.

25. The method as set forth in claim 23 wherein the silicon tetrafluoride and aluminum tetrahydride are contacted in a reaction medium that is maintained from about 30° C. to about 80° C.

26. The method as set forth in claim 25 wherein the fluoride salt is separated from the reaction medium in a solid-liquid separation unit.

27. The method as set forth in claim 23 wherein the silicon tetrafluoride separated from the by-product is used to produce additional silane by reacting the silicon tetrafluoride with an alkali or alkaline earth-metal salt of aluminum tetrahydride.

28. The method as set forth in claim 23 wherein the effluent comprises from about 30% to about 95% by weight fluoride salts of alkali metal or alkaline earth-metal and aluminum.

29. A method for producing silane and silicon tetrafluoride, the method comprising:

contacting a fluoroaluminate feed comprising a fluoride salt of alkali metal or alkaline earth-metal and aluminum with an acid comprising hydrochloric acid and a source of silicon to thereby produce silicon tetrafluoride and at least one by-product;

separating the silicon tetrafluoride from the by-product; and

reacting the silicon tetrafluoride with alkali or alkaline earth-metal salt of aluminum tetrahydride to produce silane.

Assignments (11)