CN110668483A - Method for preparing aluminum fluoride by electrolyzing aluminum carbon slag - Google Patents
Method for preparing aluminum fluoride by electrolyzing aluminum carbon slag Download PDFInfo
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Abstract
The invention relates to a method for preparing aluminum fluoride by electrolyzing aluminum carbon slag, which comprises the following steps: grinding electrolytic aluminum carbon slag into carbon slag powder, adding a fluorine leaching agent for fluorine leaching to obtain fluorine leaching slurry, and adding a fluorine precipitating agent into the fluorine leaching slurry for fluorine precipitation to obtain fluorine precipitating slurry; and carrying out flotation on the fluorine precipitation slurry to obtain carbon powder and aluminum fluoride. According to the method for preparing the aluminum fluoride from the electrolytic aluminum carbon slag, relatively pure carbon powder can be obtained without secondary treatment, the carbon slag powder is subjected to harmless treatment, the aluminum fluoride can be directly obtained through one-time flotation, multiple times of flotation or filtration are not needed, the process is simplified, and the cost is reduced.
Description
Technical Field
The invention belongs to the technical field of recycling of electrolytic aluminum carbon slag, and particularly relates to a method for preparing aluminum fluoride from electrolytic aluminum carbon slag.
Background
During the aluminum electrolysis process, unburned aggregate particles enter the electrolyte solution to form carbon slag due to selective oxidation. Carbon slag contains carbon powder and fluoride salt, the industry mainly adopts the flotation method to separate the fluoride salt in the carbon slag at present, and after flotation, fluorine is leached and precipitated to obtain aluminum fluoride, thereby realizing the recycling of electrolytic aluminum carbon slag.
The invention patent with application publication number CN109759423A discloses a comprehensive utilization method of aluminum electrolysis carbon slag, which comprises the following steps: crushing and screening: carrying out coarse crushing, ball milling and screening on the aluminum electrolysis carbon slag to obtain carbon slag powder; (2) flotation: putting the carbon residue powder into a flotation tank, and mixing slurry to obtain slurry; then adding inhibitor water glass and collecting agent kerosene into slurry of the flotation tank in sequence for flotation; drying the foam scraped by flotation to obtain carbon; and (3) filtering: filtering the electrolyte discharged from the bottom flow of the flotation tank to obtain a filtrate; (4) dissolution: adding HNO with the final concentration of 0.01-0.05 mol/L into the filtered material3And 0.3 to 0.36mol/L of Al (NO)3)3Reacting the mixed solution at the temperature of between 60 and 65 ℃ for 1 to 1.5 hours to obtain a solid-liquid mixture; in this step, aluminum reacts with fluorine to produce AlF2(OH) precipitation, wherein sodium and calcium form a mixed solution of sodium nitrate and calcium nitrate; (5) separation: carrying out solid-liquid separation on the solid-liquid mixture to obtain filter residue; wherein the filter residue mainly comprises AlF2(OH); (6) acid leaching: mixing the filter residue with a hydrofluoric acid solution with the pH value of 0.1-0.3, and then reacting for 1-1.5 h to obtain a solid-liquid mixture; (7) separation: carrying out solid-liquid separation on the solid-liquid mixture to obtain AlF3. The method adopts a flotation mode to separate carbon powder from filtered substances, at the moment, the carbon powder still contains partial fluorine, harmless carbon powder is not obtained, the carbon powder after flotation generally needs secondary treatment to obtain the harmless carbon powder, and the harmless treatment of carbon slag is not realized. After flotation, the fluorine is leached and precipitated, and at the moment, the filtrate contains more impurities. In addition, the method adopts aluminum nitrate to leach and precipitate fluorine, and the aluminum nitrate is high in price and is not suitable for industrial production.
The invention patent with application publication number CN108728867A discloses a harmless separation method of waste cathode carbon blocks in aluminum electrolysis, which comprises the following steps: crushing and screening the aluminum electrolysis waste cathode carbon blocks to obtain carbon block particles; preparing 1mol/L acid liquor for later use; leaching the carbon block particles in acid liquor under the conditions of heating and stirring, wherein the PH of the solution is controlled to be less than 5 in the adding process, and when the leaching rate of fluoride ions is higher than 94%, the leaching is finished to obtain a leaching solution; filtering the leaching solution, separating filtrate and filter residue, and washing and drying the filter residue to obtain a carbon powder product; adding a salt solution into the filtrate for fluorine precipitation to obtain a fluorine precipitation solution; and filtering the fluorine precipitation solution, separating filtrate and filter residue, and washing and drying the filter residue to obtain the basic metal fluoride product. According to the method, carbon powder is obtained by filtering after fluorine leaching, and part of fluoride with fluorine ions still remains on the carbon powder.
Disclosure of Invention
The invention aims to provide a method for preparing aluminum fluoride from electrolytic aluminum carbon slag, and aims to solve the technical problems that the existing method for preparing aluminum fluoride from electrolytic aluminum carbon slag does not realize harmless treatment on carbon slag and the production cost of aluminum fluoride is high.
In order to achieve the above purpose, the invention adopts the technical scheme that:
the method for preparing aluminum fluoride by electrolyzing aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag into carbon slag powder, and adding a fluorine leaching agent for fluorine leaching to obtain fluorine leaching slurry;
2) adding a fluorine precipitating agent into the fluorine leaching slurry obtained in the step 1) to precipitate fluorine to obtain fluorine precipitating slurry;
3) and (3) carrying out flotation on the fluorine precipitation slurry obtained in the step 2) to obtain carbon powder and aluminum fluoride.
Further, the fluorine leaching agent in the step 1) is HNO3、H2SO4One or more of them. HNO3Has a concentration of 1 to 3mol.L-1。H2SO4Has a concentration of 1 to 3mol.L-1。
Further, the fluorine leaching agent and the carbon residue powder in the step 1) are prepared into slurry with the mass percentage of 5-15% for fluorine leaching.
Further, the temperature of the fluorine leaching in the step 1) is 40-80 ℃, and the time of the fluorine leaching is 3-8 hours. Stirring is continuously carried out during fluorine leaching.
Further, the carbon slag powder is obtained by grinding the electrolytic aluminum carbon slag in the step 1) and then sieving the ground carbon slag powder through a 100-400-mesh sieve.
Further, the fluorine precipitating agent in the step 2) is Al (OH)3。
Further, the fluorine precipitation temperature in the step 2) is 80-100 ℃, and the fluorine precipitation time is 1-3 hours.
Further, the adding amount of the fluorine precipitation agent in the step 2) is 3-8% of the mass of the fluorine leaching slurry.
Further, the concentration of fluorine ions in the fluorine precipitation slurry in the flotation in the step 3) is less than or equal to 0.01g.L-1。
Further, the flotation agent A in the step 3) is one or more of a flotation agent A, a flotation agent B and a flotation agent C, and is purchased from Henan' an Lixin environmental protection science and technology limited company, the flotation agent B is purchased from Henan province Nuclear force science and technology development limited company, and the flotation agent C is purchased from Shandong Xinlong group bioengineering limited company.
The invention has the beneficial effects that:
the method for preparing the aluminum fluoride from the electrolytic aluminum carbon slag comprises the steps of leaching fluorine in carbon slag powder ground from the electrolytic aluminum carbon slag, precipitating, and then carrying out flotation to obtain carbon powder and aluminum fluoride, wherein the fluorine leaching and the fluorine precipitation can separate the fluorine from the carbon slag powder more thoroughly, the bottom flow is the aluminum fluoride during the flotation, the carbon powder floats on the upper layer, the obtained carbon powder hardly contains the fluorine, and the purer carbon powder can be obtained without secondary treatment, so that the harmless treatment of the carbon slag powder is realized. In addition, the fluorine is leached firstly and then is floated, and the yield of the finally obtained aluminum fluoride can be improved because the carbon residue powder has no residual fluorine. Compared with the existing flotation-fluorine leaching-fluorine precipitation-filtration method, the method for preparing aluminum fluoride from electrolytic aluminum carbon slag can directly obtain aluminum fluoride through one-time flotation, multiple times of flotation or filtration are not needed, the process is simplified, and the cost is reduced.
According to the method for preparing aluminum fluoride from electrolytic aluminum carbon slag, the fluorine leaching agent is added to leach fluorine, so that the fluorine exists in an ionic state, and then the fluorine precipitating agent is added to precipitate the fluorine. The aluminum fluoride is prepared by adopting aluminum nitrate in the prior art because the aluminum nitrate is dissolved in water and then hydrolyzed into nitric acid and aluminum hydroxide, the aluminum nitrate is a dangerous product and has higher price, and the aluminum fluoride obtained by using the aluminum nitrate as a leaching agent and a fluorine precipitation agent is not high in purity. The method can remove a large amount of impurities including soluble impurities and insoluble impurities with lower density by flotation after leaching and precipitating fluorine, and the remaining underflow can obtain aluminum fluoride with higher purity.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 200-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 1mol.L of carbon slag powder in the step 1)-1Preparing ore pulp with the mass fraction of 10% by using the aqueous solution of nitric acid, placing the ore pulp into a reaction tank, stirring the ore pulp for fluorine leaching, wherein the temperature of the fluorine leaching is 60 ℃, the time of the fluorine leaching is 5 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 90 ℃, and adding Al (OH)3Stirring for 2h to precipitate fluorine, and measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process to obtain the fluorine ion concentration in the upper layer liquid in the reaction tank which is less than or equal to 0.01g.L-1And ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 4% of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry in the step 3), wherein the flotation agent is a flotation agent A, and the mass ratio of the flotation agent A to the fluorine precipitation slurry is 0.005: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is crude aluminum fluoride, the flotation process enables the upper layer carbon powder to be separated from the bottom flow aluminum fluoride, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal, so that crude aluminum fluoride is obtained.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 2
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 200-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 2mol.L of carbon slag powder in the step 1)-1Preparing ore pulp with the mass fraction of 5% by using the aqueous solution of nitric acid, placing the ore pulp into a reaction tank, stirring the ore pulp for fluorine leaching, wherein the temperature of the fluorine leaching is 80 ℃, the time of the fluorine leaching is 3 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 80 ℃, and adding Al (OH)3Stirring for 3h to precipitate fluorine, measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process, and measuring the fluorine ion concentration in the upper layer liquid in the reaction tank to be less than or equal to 0.01g.L-1And ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 8 percent of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry obtained in the step 3), wherein the flotation agent is a flotation agent B, and the mass ratio of the flotation agent B to the fluorine precipitation slurry is 0.01: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 3
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 100-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 3mol.L of carbon slag powder in the step 1)-1Preparing into aqueous solution of sulfuric acidAnd (3) placing the ore pulp with the mass fraction of 15% into a reaction tank, stirring to carry out fluorine leaching, wherein the temperature of the fluorine leaching is 40 ℃, the time of the fluorine leaching is 8 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 100 ℃, and adding Al (OH)3Stirring for 1h to precipitate fluorine, measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process, and measuring the fluorine ion concentration in the upper layer liquid in the reaction tank to be less than or equal to 0.01g.L-1And (3) ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 3 percent of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry in the step 3), wherein the flotation agent is a flotation agent C, and the mass ratio of the flotation agent C to the fluorine precipitation slurry is 0.008: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 4
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 400-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 3mol.L of carbon slag powder in the step 1)-1Preparing 12% ore pulp by using the nitric acid aqueous solution, placing the ore pulp into a reaction tank, stirring the ore pulp for fluorine leaching, wherein the temperature of the fluorine leaching is 50 ℃, the time of the fluorine leaching is 7 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 85 ℃, and adding Al (OH)3Stirring for 2h to precipitate fluorine, and measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process to obtain the fluorine ion concentration in the upper layer liquid in the reaction tank which is less than or equal to 0.01g.L-1When the fluorine precipitation is finished, the fluorine precipitation slurry is obtained, and the adding amount of Al (OH)3 is the fluorine leaching amount5 percent of the mass of the slurry.
4) Carrying out flotation on the fluorine precipitation slurry obtained in the step 3), wherein the flotation agent is a flotation agent A, and the mass ratio of the flotation agent A to the fluorine precipitation slurry is 0.015: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 5
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 300-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 2mol.L of carbon slag powder in the step 1)-1Preparing the sulfuric acid aqueous solution into ore pulp with the mass fraction of 8%, placing the ore pulp into a reaction tank, stirring the ore pulp for fluorine leaching, wherein the temperature of the fluorine leaching is 70 ℃, the time of the fluorine leaching is 4 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 95 ℃, and adding Al (OH)3Stirring for 1h to precipitate fluorine, measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process, and measuring the fluorine ion concentration in the upper layer liquid in the reaction tank to be less than or equal to 0.01g.L-1And ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 6 percent of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry in the step 3), wherein the flotation agent is a flotation agent A, and the mass ratio of the flotation agent A to the fluorine precipitation slurry is 0.02: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 6
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 400-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 2.5mol.L into the carbon slag powder in the step 1)-1Preparing ore pulp with the mass fraction of 6% by using the aqueous solution of nitric acid, placing the ore pulp into a reaction tank, stirring the ore pulp for fluorine leaching, wherein the temperature of the fluorine leaching is 50 ℃, the time of the fluorine leaching is 6 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 90 ℃, and adding Al (OH)3Stirring for 2h to precipitate fluorine, and measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process to obtain the fluorine ion concentration in the upper layer liquid in the reaction tank which is less than or equal to 0.01g.L-1And ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 8 percent of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry obtained in the step 3), wherein the flotation agent is a flotation agent B, and the mass ratio of the flotation agent B to the fluorine precipitation slurry is 0.01: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 7
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 100-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 2mol.L of carbon slag powder in the step 1)-1Preparing the nitric acid aqueous solution into ore pulp with the mass fraction of 13 percent, and placing the ore pulp into a reaction tankAnd (4) stirring to leach fluorine, wherein the temperature of the fluorine leaching is 80 ℃, the time of the fluorine leaching is 4 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 80 ℃, and adding Al (OH)3Stirring for 2h to precipitate fluorine, and measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process to obtain the fluorine ion concentration in the upper layer liquid in the reaction tank which is less than or equal to 0.01g.L-1And ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 7 percent of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry obtained in the step 3), wherein the flotation agent is a flotation agent A, and the mass ratio of the flotation agent A to the fluorine precipitation slurry is 0.015: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Example 8
The method for preparing aluminum fluoride from electrolytic aluminum carbon slag comprises the following steps:
1) grinding electrolytic aluminum carbon slag by using a Raymond mill, then sieving by using a 300-mesh sieve, and removing impurity iron by magnetic separation to obtain carbon slag powder.
2) Adding 1mol.L of carbon slag powder in the step 1)-1Preparing ore pulp with the mass fraction of 14% by using the nitric acid aqueous solution, placing the ore pulp into a reaction tank, stirring the ore pulp for fluorine leaching, wherein the temperature of the fluorine leaching is 60 ℃, the time of the fluorine leaching is 3 hours, and obtaining fluorine leaching serous fluid after the completion.
3) Heating the fluorine leaching slurry in the step 2) to 100 ℃, and adding Al (OH)3Stirring for 1h to precipitate fluorine, measuring the fluorine ion concentration in the reaction tank by using a fluorine ion tester in the fluorine precipitation process, and measuring the fluorine ion concentration in the upper layer liquid in the reaction tank to be less than or equal to 0.01g.L-1And ending fluorine precipitation to obtain fluorine precipitation slurry, wherein the adding amount of Al (OH)3 is 4% of the mass of the fluorine leaching slurry.
4) Carrying out flotation on the fluorine precipitation slurry obtained in the step 3), wherein the flotation agent is a flotation agent A, and the mass ratio of the flotation agent A to the fluorine precipitation slurry is 0.018: 100, in the flotation process, the upper layer is carbon powder, the bottom flow is a crude aluminum fluoride product, the flotation process separates the upper layer carbon powder from the crude aluminum fluoride product, and then the bottom flow aluminum fluoride enters sodium removal equipment for sodium removal to obtain the crude aluminum fluoride product.
5) And (3) dehydrating and drying the crude aluminum fluoride product in the step 4) by using a dehydrator to obtain aluminum fluoride, and dehydrating and drying the carbon powder in the step 4) by using the dehydrator to obtain dried carbon powder.
Test examples
1. The contents of the respective elements in the aluminum fluoride obtained in examples 1 to 8 were measured by an atomic absorption spectrometer, and the measurement results are shown in table 1.
TABLE 1 content of each element in aluminum fluoride obtained in examples 1 to 8
As can be seen from Table 1, the content of F is more than 58%, the content of Al is less than 29%, the standard content of F in wet-process aluminum fluoride is more than 58%, and the standard content of Al is less than 29%.
2. The fluorine content in the obtained carbon powder was measured, and the measurement results are shown in table 2.
TABLE 2 fluorine content in carbon powders obtained in examples 1-8
As can be seen from Table 2, the carbon powders obtained in examples 1 to 8 of the present invention have a low fluorine content and can be directly recycled.
Claims (10)
1. The method for preparing aluminum fluoride by electrolyzing aluminum carbon slag is characterized by comprising the following steps:
1) grinding electrolytic aluminum carbon slag into carbon slag powder, and adding a fluorine leaching agent for fluorine leaching to obtain fluorine leaching slurry;
2) adding a fluorine precipitating agent into the fluorine leaching slurry obtained in the step 1) to precipitate fluorine to obtain fluorine precipitating slurry;
3) and (3) carrying out flotation on the fluorine precipitation slurry obtained in the step 2) to obtain carbon powder and aluminum fluoride.
2. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1, wherein the fluorine leaching agent in the step 1) is HNO3、H2SO4One or two of them.
3. The method for preparing aluminum fluoride by electrolyzing aluminum carbon slag according to claim 2, wherein the HNO in step 1)3Has a concentration of 1 to 3mol.L-1Said H is2SO4Has a concentration of 1 to 3mol.L-1。
4. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1 or 2, wherein the fluorine leaching agent and the carbon slag powder in the step 1) are prepared into slurry with the mass percentage of 5-15% for fluorine leaching.
5. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1, wherein the temperature of the fluorine leaching in the step 1) is 40-80 ℃, and the time of the fluorine leaching is 3-8 h.
6. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1, wherein the carbon slag powder is obtained by grinding the electrolytic aluminum carbon slag in step 1) and sieving the ground electrolytic aluminum carbon slag with a 100-400-mesh sieve.
7. The method for preparing aluminum fluoride from electrolytic aluminum carbon residue as claimed in claim 1, wherein the fluorine precipitation agent in step 2) is Al (OH)3。
8. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1 or 7, wherein the fluorine precipitation temperature in the step 2) is 80-100 ℃, and the fluorine precipitation time is 1-3 h.
9. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1 or 7, wherein the fluorine precipitation agent is added in the step 2) in an amount of 3-8% by mass of the fluorine leaching slurry.
10. The method for preparing aluminum fluoride from electrolytic aluminum carbon slag according to claim 1, wherein the concentration of fluorine ions in the fluorine precipitating slurry during the flotation in the step 3) is less than or equal to 0.01g.L-1。
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| CN114314626A (en) * | 2022-01-19 | 2022-04-12 | 湖南绿脉环保科技股份有限公司 | Method for reducing sodium content in fluorine-containing raw material |
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| CN114314626A (en) * | 2022-01-19 | 2022-04-12 | 湖南绿脉环保科技股份有限公司 | Method for reducing sodium content in fluorine-containing raw material |
| CN114314626B (en) * | 2022-01-19 | 2024-01-26 | 湖南绿脉环保科技股份有限公司 | Method for reducing sodium content in fluorine-containing raw material |
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