Reverse osmosis for purifying mixtures of hydrofluoric acid and nitric acid

Patent metadata

Field	Value
Publication number	US-9840667-B2
Application number	US-201414786211-A
Country	US
Kind code	B2
Filing date	Apr 16, 2014
Priority date	Apr 25, 2013
Publication date	Dec 12, 2017
Grant date	Dec 12, 2017

Abstract

Disclosed is a method of purifying a solution containing hydrofluoric acid, nitric acid and at least one silicon impurity by treating the solution with at least one reverse osmosis membrane. According to the method of the present invention, silicon impurities contained in the solution containing hydrofluoric acid and nitric acid can be selectively removed or reduced. This method can be advantageously used in the photovoltaic industry or in the battery component industry.

First claim

The invention claimed is:

1. A method of purifying a solution containing hydrofluoric acid, nitric acid and at least one silicon impurity, the method comprising treating the solution with at least one reverse osmosis membrane,
wherein at least 90% of the at least one silicon impurity is rejected, and wherein hydrofluoric acid and nitric acid in the solution are not significantly rejected.

2. The method according to claim 1 , wherein the solution mainly contains hydrofluoric acid and nitric acid and comprises silicon compound as an impurity.

3. The method according to claim 1 , wherein the content of nitric acid in the solution before the purification is from 0.1% w/w to 10% w/w.

4. The method according to claim 1 , wherein the content of hydrofluoric acid in the solution before the purification is from 0.001% w/w to 50% w/w.

5. The method according to claim 1 , wherein the content of silicon impurity in the solution before the purification is from 0.1% w/w to 30% w/w.

6. The method according to claim 1 , wherein one or more reverse osmosis membranes are used, in series or in parallel, or in combination of series and parallel.

7. The method according to claim 1 , wherein the silicon impurity is generated by contacting a solution containing hydrofluoric acid and nitric acid with a silicon containing surface.

8. The method according to claim 7 , wherein the contacting a solution containing hydrofluoric acid and nitric acid with a silicon containing surface is a surface texturing of solar cells or an etching of silicon based electrode for batteries.

9. The method according to claim 7 , further comprising recycling the purified solution to a flow of treatment of the silicon containing surface.

10. The method according to claim 1 , further comprising a step of adding hydrofluoric acid and/or nitric acid to set the concentration of hydrofluoric acid and nitric acid contained in the solution to a target level.

11. A process of manufacturing a silicon based solar cell, the process comprising purifying a solution containing hydrofluoric acid, nitric acid and at least one silicon impurity in accordance with the method according to claim 1 .

12. A process of manufacturing a silicon based electrode for a battery, the process comprising purifying a solution containing hydrofluoric acid, nitric acid and at least one silicon impurity in accordance with the method according to claim 1 .

13. The process according to claim 11 , further comprising recycling the purified solution to a flow of treatment of a silicon containing surface during the manufacturing process.

14. The process according to claim 11 , wherein the reverse osmosis membrane is made of polyamides, polypiperazine amides, polyacrylonitriles, polysulfones, cellulose acetates, polybenzimidazolines, polyoxadiazoles, polyfuranes, polyether-polyfuranes, polyvinyl amines, polypyrrolidines, carboxylated polysulfones or sulfonated polysulfones.

15. The process according to claim 12 , further comprising recycling the purified solution to a flow of treatment of a silicon containing surface during the manufacturing process.

16. The process according to claim 12 , wherein the reverse osmosis membrane is made of polyamides, polypiperazine amides, polyacrylonitriles, polysulfones, cellulose acetates, polybenzimidazolines, polyoxadiazoles, polyfuranes, polyether-polyfuranes, polyvinylamines, polypyrrolidines, carboxylated polysulfones or sulfonated polysulfones.

17. The method according to claim 1 , wherein the content of nitric acid in the solution before the purification is from 2% w/w to 10% w/w.

18. The method according to claim 1 , wherein the content of hydrofluoric acid in the solution before the purification is from 0.5% w/w to 30% w/w.

19. The method according to claim 1 , wherein the content of silicon impurity in the solution before the purification is from 0.5% w/w to 20% w/w.

20. The method according to claim 1 , wherein ⅔ of the hydrofluoric acid and nitric acid are not rejected.

Assignees

• Solvay

Inventors

• Collard Jean-Marie

Classifications

• H01M4/386

  Silicon or alloys based on silicon · CPC title

• C01B21/46

  Purification; Separation {; Stabilisation (C01B21/40 takes precedence)} · CPC title

• C01B7/195

  Separation; Purification · CPC title

• B01D61/025

  Reverse osmosis; Hyperfiltration · CPC title

• H01M4/1395

  of electrodes based on metals, Si or alloys · CPC title