CN117568870A - Method for reducing fluoride in electrolyte in operation process of aluminum electrolysis cell - Google Patents
Method for reducing fluoride in electrolyte in operation process of aluminum electrolysis cell Download PDFInfo
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- CN117568870A CN117568870A CN202311545249.6A CN202311545249A CN117568870A CN 117568870 A CN117568870 A CN 117568870A CN 202311545249 A CN202311545249 A CN 202311545249A CN 117568870 A CN117568870 A CN 117568870A
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- electrolyte
- aluminum electrolysis
- electrolysis cell
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 50
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 31
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 37
- 239000011248 coating agent Substances 0.000 claims abstract description 36
- 238000002386 leaching Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000007790 solid phase Substances 0.000 claims abstract description 13
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- -1 alkali metal salts Chemical class 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 5
- 150000004673 fluoride salts Chemical class 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 159000000000 sodium salts Chemical class 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 25
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 2
- 229910001570 bauxite Inorganic materials 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/18—Electrolytes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a method for reducing fluoride in electrolyte in the operation process of an aluminum electrolysis cell, which comprises the following steps: crushing the anode coating to below 60 meshes, carrying out acid leaching, carrying out solid-liquid separation, taking the solid phase material for dehydration, and then entering an aluminum electrolysis system as the anode coating. Based on the solubility difference of aluminum oxide and fluoride in a specific solution in the anode coating, partial elements unfavorable for the electrolyte are selectively removed, and the content of the elements in the anode coating is reduced, so that the impurities in the electrolyte are effectively reduced.
Description
Technical Field
The application relates to the technical field of aluminum electrolysis, in particular to a method for reducing fluoride in electrolyte in the operation process of an aluminum electrolysis cell.
Background
Bauxite generally contains a small amount of impurity elements such as lithium, potassium, calcium, magnesium and the like, and part of lithium, potassium, calcium and magnesium enter the alumina in the process of producing alumina from the bauxite. When aluminum is electrolyzed to produce raw aluminum by taking aluminum oxide as a raw material and adopting a cryolite system as a flux, lithium, potassium, calcium and magnesium in the aluminum oxide are converted into corresponding fluoride in an electrolyte. The lithium content in the alumina is high, which can lead to the lithium fluoride in the electrolyte of some enterprises to be more than 6 percent, the primary crystal temperature of the electrolyte is low, the melting property of the alumina is poor, the normal production is seriously affected, and the economic and technical indexes are deteriorated. The potassium content in alumina is higher, so that the potassium fluoride content in electrolytes of certain enterprises is up to 5% or even more, the problems of high difficulty in carbon residue separation, low current efficiency and the like occur in the production process, and the economic and technical indexes of aluminum electrolysis production are seriously influenced. And when the calcium and magnesium in the electrolyte are high, if the process control is unreasonable, hard crust is easily formed at the bottom of the furnace, and the treatment difficulty is high.
If the impurity in the electrolyte is higher, part of the impurity can be removed from the electrolyte by a chemical method, so that the impurity content in the electrolyte is reduced. When enterprises have a large amount of surplus electrolyte, the method can be adopted, and if the enterprises do not have enough surplus electrolyte, the process flow for removing impurities from the electrolyte by adopting a chemical method is difficult to continuously run, and the method has high cost and high cost. The enterprises need to cool the high-temperature electrolyte to room temperature, and the electrolyte is added into the electrolytic tank again after the impurity removal is finished. The electrolyte consumes a large amount of energy sources in the process of temperature reduction and temperature rising, and consumes a large amount of labor force.
In the production process, the anode coating material for aluminum electrolysis and the electrolyte are subjected to substance exchange continuously, the impurity level in the coating material is equivalent to the impurity level in the electrolyte after the material exchange is balanced, and if the impurity content in the anode coating material is reduced, the impurity content in the electrolyte and an aluminum electrolysis production system can be obviously reduced by using the coating material with low impurity content for a long time, so that a foundation is provided for the stability of aluminum electrolysis production. The cover material circulation amount of the enterprise is large, and a sufficient raw material basis can be provided for reducing the impurity content in the electrolyte by adopting a chemical method.
Disclosure of Invention
The invention provides a method for reducing fluoride in electrolyte in the operation process of an aluminum electrolysis cell, which is based on the solubility difference of aluminum oxide and fluoride in a specific solution in an anode covering material, selectively removes partial elements unfavorable to the electrolyte, and reduces the content of the elements in the anode covering material, thereby effectively reducing impurities in the electrolyte.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the method for reducing fluoride in electrolyte in the operation process of the aluminum electrolysis cell comprises the following steps:
crushing the anode coating to below 60 meshes, carrying out acid leaching, carrying out solid-liquid separation, taking the solid phase material for dehydration, and then entering an aluminum electrolysis system as the anode coating.
Harmful gas generated in the acid leaching process is exhausted after being treated; the solution after solid-liquid separation is recycled after innocent treatment.
Harmful gases generated in the acid leaching process are adsorbed by alumina solids and then are emptied.
Adding soluble aluminum salt into the solution after solid-liquid separation, adjusting the pH value to 5.5-7.0 by sodium salt or sodium hydroxide to generate fluoride salt, filtering, drying the solid to be used as electrolyte raw material, and evaporating and crystallizing the solution to obtain alkali metal salts.
The acid used for acid leaching is one or a mixture of more than one of hydrochloric acid, sulfuric acid and nitric acid.
The molar concentration of the acid used for acid leaching is 1-10mol/L.
The conditions of the acid leaching are as follows: the reaction temperature is 40-100 ℃, the liquid-solid ratio of the acid to the anode covering material is 0.5:1-5:1, and the reaction time is 5-10 hours.
The beneficial technical effects of the invention are as follows:
the method reduces the content of harmful impurities in the anode coating in real time through acid treatment, and the anode coating enters the electrolytic tank to exchange substances with electrolyte in the electrolytic tank after acid leaching treatment, so that the content of the harmful impurities in the electrolyte in the aluminum electrolytic tank is reduced, and the method has good application prospect.
Detailed Description
The present invention will be described in detail with reference to the following examples.
Example 1
The method for reducing fluoride in electrolyte in the operation process of the aluminum electrolysis cell comprises the following steps: crushing the anode coating to below 60 meshes, selectively leaching with 10mol/L hydrochloric acid at a reaction temperature of 40 ℃ and a liquid-solid ratio of 0.5:1 for 8 hours, wherein excessive harmful impurities in the anode coating enter a solution, the rest materials are solid phases, solid-liquid separation is carried out, the mass loss of the coating is 15.0%, and the solid phase materials enter an aluminum electrolysis system after dehydration to be used as anode coating; harmful gas generated in the leaching process is adsorbed by alkali liquor and then is emptied; and (3) regulating the pH value of the solution after solid-liquid separation to 5.5, adding soluble calcium salt and calcium fluoride, and drying to obtain the electrolyte raw material. Evaporating and crystallizing the solution to obtain alkali metal salts. The impurity contents in the anode coating and electrolyte before and after the treatment are shown in table 1.
Example 2
The method for reducing fluoride in electrolyte in the operation process of the aluminum electrolysis cell comprises the following steps: crushing the anode coating to below 80 meshes, selectively leaching with 5mol/L sulfuric acid at a reaction temperature of 100 ℃ and a liquid-solid ratio of 1:1 for 4 hours, wherein excessive harmful impurities in the anode coating enter a solution, the rest materials are solid phases, solid-liquid separation is carried out, the mass loss of the coating is 14.4%, and the solid phase materials enter an aluminum electrolysis system after dehydration to be used as anode coating; harmful gas generated in the leaching process is adsorbed by alumina and then is exhausted; controlling the temperature of the solution after solid-liquid separation, adjusting the pH value to 7.0, adding soluble aluminum salt to generate fluoride salt, and drying to obtain the electrolyte raw material. Evaporating and crystallizing the solution to obtain alkali metal salts.
Example 3
The method for reducing fluoride in electrolyte in the operation process of the aluminum electrolysis cell comprises the following steps: crushing the anode coating to below 100 meshes, selectively leaching with 5mol/L nitric acid at a reaction temperature of 50 ℃, a liquid-solid ratio of 4:1, and a reaction time of 9 hours, wherein excessive harmful impurities in the anode coating enter a solution, the rest materials are solid phases, solid-liquid separation is carried out, the mass loss of the coating is 11.5%, and the solid phase materials enter an aluminum electrolysis system after dehydration to serve as the anode coating; harmful gas generated in the leaching process is adsorbed by alkali liquor and then is emptied; controlling the temperature of the solution after solid-liquid separation, adjusting the pH value to 6.0, adding soluble aluminum salt to generate fluoride salt, and drying to obtain the electrolyte raw material. Evaporating and crystallizing the solution to obtain alkali metal salts.
Example 4
The method for reducing fluoride in electrolyte in the operation process of the aluminum electrolysis cell comprises the following steps: crushing the anode coating to below 150 meshes, selectively leaching by using 1mol/L hydrochloric acid and 4mol/L sulfuric acid mixed acid, wherein the reaction temperature is 60 ℃, the liquid-solid ratio is 5:1, the reaction time is 10 hours, excessive harmful impurities in the anode coating enter a solution, the rest materials are still solid phases, the solid-liquid separation is carried out, the mass loss of the coating is 11.3%, and the solid phase materials enter an aluminum electrolysis system to be used as the anode coating after being dehydrated; harmful gas generated in the leaching process is adsorbed by alumina and then is exhausted; controlling the temperature of the solution after solid-liquid separation, adjusting the pH value to 6.5, adding soluble magnesium salt to generate magnesium fluoride, and drying to obtain the electrolyte raw material. Evaporating and crystallizing the solution to obtain alkali metal salts.
Example 5
The method for reducing fluoride in electrolyte in the operation process of the aluminum electrolysis cell comprises the following steps: crushing the anode coating to below 200 meshes, selectively leaching by using 3mol/L hydrochloric acid and 3mol/L nitric acid mixed acid, wherein the reaction temperature is 50 ℃, the liquid-solid ratio is 3:1, the reaction time is 5 hours, excessive harmful impurities in the anode coating enter a solution, the rest materials are solid phases, the solid-liquid separation is carried out, the mass loss of the coating is 8.2%, and the solid phase materials enter an aluminum electrolysis system to be used as the anode coating after being dehydrated; harmful gas generated in the leaching process is adsorbed by alumina and then is exhausted; controlling the temperature of the solution after solid-liquid separation, adjusting the pH value to 6.7, adding soluble aluminum salt to generate fluoride salt, and drying to obtain the electrolyte raw material. Evaporating and crystallizing the solution to obtain alkali metal salts.
Example 6
The impurity contents in the anode coatings and electrolyte before and after treatment by the methods of examples 1 to 5 are shown in table 1 below:
TABLE 1 impurity levels/%
As shown in Table 1, the impurity content in the anode coating and the electrolyte produced in real time is significantly reduced by the method of the present invention.
The described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (7)
1. A method for reducing fluoride in electrolyte during operation of an aluminum electrolysis cell, comprising the steps of:
crushing the anode coating to below 60 meshes, carrying out acid leaching, carrying out solid-liquid separation, taking the solid phase material for dehydration, and then entering an aluminum electrolysis system as the anode coating.
2. The method for reducing fluoride in electrolyte during operation of an aluminum electrolysis cell according to claim 1, wherein: harmful gas generated in the acid leaching process is exhausted after being treated; the solution after solid-liquid separation is recycled after innocent treatment.
3. The method for reducing fluoride in electrolyte during operation of an aluminum electrolysis cell according to claim 2, wherein: harmful gases generated in the acid leaching process are adsorbed by alumina solids and then are emptied.
4. A method for reducing fluoride in an electrolyte during operation of an aluminum electrolysis cell according to claim 3, wherein: adding soluble aluminum salt into the solution after solid-liquid separation, adjusting the pH value to 5.5-7.0 by sodium salt or sodium hydroxide to generate fluoride salt, filtering, drying the solid to be used as electrolyte raw material, and evaporating and crystallizing the solution to obtain alkali metal salts.
5. The method for reducing fluoride in electrolyte during operation of an aluminum electrolysis cell according to claim 1, wherein: the acid used for acid leaching is one or a mixture of more than one of hydrochloric acid, sulfuric acid and nitric acid.
6. The method for reducing fluoride in electrolyte during operation of an aluminum electrolysis cell according to claim 5, wherein: the molar concentration of the acid used for acid leaching is 1-10mol/L.
7. The method for reducing fluoride in electrolyte during operation of an aluminum electrolysis cell according to claim 1, wherein:
the conditions of the acid leaching are as follows: the reaction temperature is 40-100 ℃, the liquid-solid ratio of the acid to the anode covering material is 0.5:1-5:1, and the reaction time is 5-10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311545249.6A CN117568870A (en) | 2023-11-20 | 2023-11-20 | Method for reducing fluoride in electrolyte in operation process of aluminum electrolysis cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311545249.6A CN117568870A (en) | 2023-11-20 | 2023-11-20 | Method for reducing fluoride in electrolyte in operation process of aluminum electrolysis cell |
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| Publication Number | Publication Date |
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| CN117568870A true CN117568870A (en) | 2024-02-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311545249.6A Pending CN117568870A (en) | 2023-11-20 | 2023-11-20 | Method for reducing fluoride in electrolyte in operation process of aluminum electrolysis cell |
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| CN (1) | CN117568870A (en) |
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2023
- 2023-11-20 CN CN202311545249.6A patent/CN117568870A/en active Pending
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