IP Library Granted Patent US 8,540,958
Granted Patent B2
US 8,540,958 · App. 13/494,717 · Granted Sep 24, 2013

Cascading purification

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Quick Facts
Patent No.
US 8,540,958
App. No.
13/494,717
Granted
Sep 24, 2013
Kind
B2
Abstract

The present invention provides a method of purifying a material using a cascading dissolution and washing process. The dissolution and washing processes can contain single or multiple stages. Water and dissolving chemicals are recycled through the process towards the beginning of the process.

Claims (48)

1. A method for increasing the purity of silicon, comprising:

combining a first silicon-aluminum complex with a first hydrochloric acid solution to allow the first complex to react at least partially with the first hydrochloric acid solution, to provide a first mixture;

separating the first mixture, to provide a third silicon-aluminum complex and the first hydrochloric acid solution;

combining the third silicon-aluminum complex with a second hydrochloric acid solution to allow the third complex to react at least partially with the second hydrochloric acid solution, to provide a third mixture, wherein the second hydrochloric acid solution is stronger than the first hydrochloric acid solution;

separating the third mixture, to provide a first silicon and the second hydrochloric acid solution;

transferring portions of the second hydrochloric acid solution to the first hydrochloric acid solution to maintain the pH of the first hydrochloric acid solution, the volume of the first hydrochloric acid solution, the specific gravity of the first hydrochloric acid solution, or a combination thereof;

combining the first silicon with a first rinse solution, to provide a fourth mixture;

separating the fourth mixture, to provide a wet purified silicon and the first rinse solution;

drying the wet purified silicon, sufficient to provide a dry purified silicon.

2. The method of claim 1 , further comprising:

separating the first mixture, to provide a second silicon-aluminum complex and the first hydrochloric acid solution;

combining the second silicon-aluminum complex with a third hydrochloric acid solution to allow the second complex to react at least partially with the third hydrochloric acid solution, to provide a second mixture, wherein the third hydrochloric acid solution is stronger than the first hydrochloric acid solution, and wherein the third hydrochloric acid solution is weaker than the second hydrochloric acid solution;

separating the second mixture, to provide a third silicon-aluminum complex and the third hydrochloric acid solution.

3. The method of claim 1 , further comprising:

separating the fourth mixture, to provide a second silicon and the first rinse solution;

combining the second silicon with a second rinse solution, to provide a fifth mixture;

separating the fifth mixture, to provide the wet silicon and the second rinse solution.

4. The method of claim 1 , further comprising removing portions of the first hydrochloric acid solution from the first hydrochloric acid solution.

5. The method of claim 4 , wherein the portions of the first hydrochloric acid solution are removed from the first hydrochloric acid solution when the pH of the first hydrochloric acid solution is equal to or greater than approximately 1.5 and when the specific gravity of the first hydrochloric acid solution is equal to or greater than approximately 1.3.

6. The method of claim 4 , wherein the removed portions of the first hydrochloric acid solution comprise a product of the reaction of aluminum with at least one of hydrochloric acid or water, wherein the removed portions of the first hydrochloric acid solution comprise a product valuable for water treatment or purification, or a combination thereof.

7. The method of claim 4 , wherein the removed portions of the first hydrochloric acid are transferred to a polyaluminum chloride tank, the tank comprising a settling tank with a pH of approximately 1.5 to 2.5 and a specific gravity of approximately 1.25 to 1.35, wherein the settling tank allows solid material in the tank to settle to the bottom for removal.

8. The method of claim 2 , further comprising transferring portions of third hydrochloric acid solution to the first hydrochloric acid solution to maintain the pH of the first hydrochloric acid solution, the volume of the first hydrochloric acid solution, the specific gravity of the first hydrochloric acid solution, or a combination thereof.

9. The method of claim 1 , wherein the first hydrochloric acid solution comprises hydrochloric acid with a pH of approximately 1.0-3.0 and a specific gravity of less than approximately 1.2-1.4.

10. The method of claim 1 , wherein the dry purified silicon comprises approximately 1000-3000 parts per million weight aluminum.

11. The method of claim 2 , further comprising transferring portions of the second hydrochloric acid solution to the third hydrochloric acid solution to maintain the pH of the third hydrochloric acid solution, the volume of the third hydrochloric acid solution, the specific gravity of the third hydrochloric acid solution, or a combination thereof.

12. The method of claim 2 , wherein the third hydrochloric acid solution comprises hydrochloric acid with a pH of approximately 0.0 to 3.0 and a specific gravity of approximately 1.05-1.3.

13. The method of claim 1 , further comprising transferring portions of the first rinse solution or of a bulk hydrochloric acid solution to the second hydrochloric acid solution to maintain the pH of the second hydrochloric acid solution, the volume of the second hydrochloric acid solution, the specific gravity of the second hydrochloric acid solution, or a combination thereof.

14. The method of claim 1 , wherein the second hydrochloric acid solution comprises hydrochloric acid with a pH of approximately −0.5 to 0.0 and a specific gravity of approximately 1.01-1.15.

15. The method of claim 3 , further comprising transferring portions of the second rinse solution to the first rinse solution to maintain the volume of the first rinse solution.

16. The method of claim 1 , further comprising adding fresh water to the first rinse solution to maintain the volume of the first rinse solution.

17. The method of claim 3 , further comprising adding fresh water to the second rinse solution to maintain the volume of the second rinse solution.

18. The method of claim 1 , wherein at least one of the first, or third silicon-aluminum complex, the first silicon, the wet silicon, or the dry purified silicon are independently approximately 600 to 800 kg.

19. The method of claim 1 , wherein the process is conducted in a batch or continuous fashion.

20. A method for increasing the purity of silicon, comprising:

combining a first silicon-aluminum complex with a first hydrochloric acid solution to allow the first complex to react at least partially with the first hydrochloric acid solution, to provide a first mixture;

separating the first mixture, to provide a third silicon-aluminum complex and the first hydrochloric acid solution;

combining the third silicon-aluminum complex with a second hydrochloric acid solution to allow the third complex to react at least partially with the second hydrochloric acid solution, to provide a third mixture, wherein the second hydrochloric acid solution is stronger than the first hydrochloric acid solution;

separating the third mixture, to provide a first silicon and the second hydrochloric acid solution;

combining the first silicon with a first rinse solution, to provide a fourth mixture;

separating the fourth mixture, to provide a wet purified silicon and the first rinse solution;

drying the wet purified silicon, sufficient to provide a dry purified silicon;

removing portions of the first hydrochloric acid solution from the first hydrochloric acid solution to maintain the pH and specific gravity of the first hydrochloric acid solution;

transferring portions of the second hydrochloric acid solution to the first hydrochloric acid solution to maintain the pH of the first hydrochloric acid solution, the volume of the first hydrochloric acid solution, the specific gravity of the third hydrochloric acid solution, or a combination thereof, wherein the third hydrochloric acid solution is stronger than the first hydrochloric acid solution, and wherein the third hydrochloric acid solution is weaker than the second hydrochloric acid solution;

adding portions of a bulk hydrochloric acid solution to the second hydrochloric acid solution to maintain the pH of the second hydrochloric acid solution, the volume of the second hydrochloric acid solution, the specific gravity of the second hydrochloric acid solution, or a combination thereof;

transferring portions of the first rinse solution to the second hydrochloric acid solution to maintain the pH of the second hydrochloric acid solution, the volume of the second hydrochloric acid solution, the specific gravity of the second hydrochloric acid solution, or a combination thereof; and

adding fresh water to the second rinse solution to maintain the volume of the second rinse solution;

wherein the dry purified silicon comprises approximately 1000-3000 parts per million weight aluminum.

21. The method of claim 20 , wherein the process is conducted in a batch or continuous fashion.

Assignments (6)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 26, 2023
From: SUNNUVELLIR SLHF
To: HIGHLAND MATERIALS, INC.
Reel/Frame 064388/0757 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 25, 2023
From: SILICOR MATERIALS, INC.
To: SUNNUVELLIR SLHF
Reel/Frame 062511/0046 →
LIEN Recorded May 26, 2017
From: SILICOR MATERIALS, INC.
To: SCHWEGMAN, LUNDBERG & WOESSNER, P.A.
Reel/Frame 042592/0974 →
SECURITY INTEREST Recorded Dec 27, 2016
From: SILICOR MATERIALS, INC.
To: SUNNUVELLIR SLHF
Reel/Frame 040777/0104 →
LICENSE Recorded Oct 13, 2015
From: SILICOR MATERIALS, INC.
To: SMS GROUP GMBH
Reel/Frame 036811/0327 →
CHANGE OF NAME Recorded Nov 20, 2012
From: CALISOLAR INC.
To: SILICOR MATERIALS INC.
Reel/Frame 029405/0900 →