# US 8,540,958 B2 · Cascading purification > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,540,958 B2 - Document ID: US8540958B2 - Status: Granted - Kind: B2 - Application number: 13/494,717 - Filed: 2012-06-12 - Published: 2012-10-04 - Granted: 2013-09-24 - Earliest claimed: 2010-04-14 - Assignees: Silicor Materials Inc. - Applicants: Scott Nichol; Anthony Tummillo; Dan Smith - Inventors: Scott Nichol; Anthony Tummillo; Dan Smith - Web page: https://patentgrep.com/patent/US8540958B2 ## CPC - C01B 33/037: Purification (by zone-melting C30B13/00) - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} ## 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 ### Claim 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. ### Claim 2 (depends on 1) 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. ### Claim 3 (depends on 1) 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. ### Claim 4 (depends on 1) The method of claim 1, further comprising removing portions of the first hydrochloric acid solution from the first hydrochloric acid solution. ### Claim 5 (depends on 4) 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. ### Claim 6 (depends on 4) 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. ### Claim 7 (depends on 4) 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. ### Claim 8 (depends on 2) 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. ### Claim 9 (depends on 1) 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. ### Claim 10 (depends on 1) The method of claim 1, wherein the dry purified silicon comprises approximately 1000-3000 parts per million weight aluminum. ### Claim 11 (depends on 2) 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. ### Claim 12 (depends on 2) 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. ### Claim 13 (depends on 1) 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. ### Claim 14 (depends on 1) 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. ### Claim 15 (depends on 3) 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. ### Claim 16 (depends on 1) The method of claim 1, further comprising adding fresh water to the first rinse solution to maintain the volume of the first rinse solution. ### Claim 17 (depends on 3) The method of claim 3, further comprising adding fresh water to the second rinse solution to maintain the volume of the second rinse solution. ### Claim 18 (depends on 1) 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. ### Claim 19 (depends on 1) The method of claim 1, wherein the process is conducted in a batch or continuous fashion. ### Claim 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. ### Claim 21 (depends on 20) The method of claim 20, wherein the process is conducted in a batch or continuous fashion.