CN114031099A - Acidification roasting method for efficiently treating aluminum electrolysis solid waste - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/32—Thermal decomposition of sulfates including complex sulfates, e.g. alums
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/06—Sulfates; Sulfites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
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Abstract
An acidification roasting method for efficiently treating aluminum electrolysis solid waste belongs to the technical field of aluminum electrolysis solid waste resource treatment. The method is characterized in that the specific treatment process comprises the steps of uniformly mixing the aluminum electrolysis solid waste and alumina in proportion, carrying out acidification roasting, and finally carrying out wet water immersion treatment. The method takes the aluminum electrolysis solid waste as a raw material, mixes a certain amount of aluminum oxide, and carries out sulfating roasting-water leaching treatment, so that valuable elements are fully and efficiently converted into sulfate solution, and meanwhile, the aluminum oxide solid is separated and recycled. The method has the advantages that the aluminum electrolysis solid waste is directly utilized, the aluminum oxide is added, so that the fluoride is more fully acidified and roasted, and finally the aluminum electrolysis solid waste is harmless, valuable elements, aluminum oxide, fluorine resources, lithium potassium resources and the like in the aluminum electrolysis solid waste can be effectively recovered, so that the method changes waste into valuable things, has a simple process, and is easy for industrial implementation.
Description
Technical Field
The invention belongs to the technical field of aluminum electrolysis solid waste recycling treatment, and particularly relates to an acidification roasting method for efficiently treating aluminum electrolysis solid waste.
Background
In recent years, the electrolytic aluminum industry in China has developed rapidly. Along with the increase of the yield of the electrolytic aluminum, the yield of fluoride-containing solid waste residues such as aluminum electrolysis anode covering materials and the like is also rapidly increased in the solid waste generated in the electrolysis process except waste cathode carbon blocks such as waste aluminum electrolytes and electrolytic bath furnace bottom sediment. At present, the solid waste generated by the electrolytic aluminum industry in China is about 25 ten thousand tons, and is accumulated and stockpiled with more than 200 ten thousand tons. Under the prior art, most electrolytic aluminum plants adopt an open-air stacking or direct soil landfill method to treat electrolytic aluminum solid waste, not only occupy a large amount of land, but also the contained soluble fluoride not only pollutes the atmosphere, but also flows into rivers along with rainwater and permeates underground polluted soil and underground water, thereby bringing great harm to the environment. The recycling of the aluminum electrolysis solid waste is of great significance to the comprehensive coordination and sustainable development of the aluminum industry in China.
There have been some studies on recycling of solid waste in aluminum electrolysis processes. Patent CN102079534B2 provides a method for producing cryolite from electrolytic aluminum fluorine-containing waste residue, mixing the electrolytic aluminum fluorine-containing waste residue with concentrated sulfuric acid, roasting at 150-450 ℃, and reacting the obtained solid sodium sulfate, aluminum sulfate and hydrofluoric acid to obtain high-purity cryolite. Patents CN105293536A and CN109179457A disclose a method for extracting lithium from electrolytic aluminum waste residue, which comprises mixing and roasting the electrolytic aluminum waste residue with concentrated sulfuric acid, then soaking in water, adding calcium oxide, and then adding saturated sodium carbonate solution to obtain lithium carbonate product. In the prior art, the cryolite or the lithium carbonate is prepared by taking the electrolytic aluminum waste residue and concentrated sulfuric acid as raw materials aiming at the electrolytic aluminum waste residue, so that resources in the electrolytic aluminum waste residue are recovered to a certain extent, but the conversion rate of fluoride in the acidification roasting process is not mentioned.
Disclosure of Invention
The invention provides an acidification roasting method capable of efficiently treating aluminum electrolysis solid waste aiming at the resource treatment of the aluminum electrolysis cell solid waste, and valuable element salt solution, fluorine and alumina are respectively recovered from the acidification roasting method, so that the comprehensive utilization rate of resources is improved.
The adopted specific technical scheme is as follows:
an acidification roasting method for efficiently treating aluminum electrolysis solid waste comprises the specific treatment process of uniformly mixing the aluminum electrolysis solid waste and alumina in proportion, carrying out acidification roasting, and finally carrying out wet water immersion treatment.
The aluminum electrolysis solid waste comprises waste solid aluminum electrolyte (the fluoride content is more than or equal to 90%), aluminum electrolysis cell bottom sediment (the fluoride and the aluminum oxide respectively account for about 50%) and aluminum electrolysis anode covering material (the fluoride accounts for about 60% and the aluminum oxide accounts for about 35%).
Before carrying out acidizing roasting, crushing, ball-milling and screening the aluminum electrolysis solid waste to enable the particle size of the aluminum electrolysis solid waste to be smaller than 200 meshes, and obtaining a granular material.
The added alumina needs to be calcined at high temperature to be converted into alpha-alumina.
And mixing the obtained granular material and alumina according to the mass ratio of 2: 1-1: 2 to obtain uniformly mixed granular material.
Mixing the uniformly mixed granular material with concentrated sulfuric acid with the concentration of 98%, wherein the mass ratio of the granular material to the concentrated sulfuric acid is 1: (1-5) placing the crucible into a roasting device, and roasting for 1-4 hours at the temperature of 150-300 ℃ and at the stirring speed of 200-600 r/min; and (3) absorbing hydrogen fluoride gas generated by reaction by using aluminum hydroxide, sodium hydroxide or calcium hydroxide in the roasting process, and calculating the fluorine conversion rate in the roasting process.
The fluorine conversion is defined as the percentage of fluorine converted to hydrogen fluoride in the calcination process to the total amount of fluorine in the feedstock and is calculated by the equation:
fluorine conversion (fluorine converted to hydrogen fluoride/total amount of fluorine in raw material) × 100%
And the wet water immersion treatment is to add a certain amount of deionized water into the roasted product, and stir and react for 0.5-2 h at room temperature. And filtering and separating the mixed solution to separate a salt solution containing valuable elements and a solid precipitate, and washing and drying the solid precipitate.
The salt solution containing valuable elements comprises sodium sulfate, aluminum sulfate, potassium sulfate and lithium sulfate; the resulting solid precipitated as alumina.
The invention has the following beneficial effects:
according to the method, the aluminum oxide is added to carry out the acidification roasting and water leaching technologies on the aluminum electrolysis solid waste, so that valuable elements, aluminum oxide and fluorine resources in the aluminum electrolysis solid waste can be effectively recovered, waste can be changed into valuable, and the pollution to the environment caused by long-term accumulation and storage of the aluminum electrolysis solid waste is avoided; the method has the advantages of simple process, convenient operation, low production cost, no secondary pollution in the production process and accordance with the requirements of green chemical industry; meanwhile, the alumina in the method can be recycled for multiple times; hydrofluoric acid produced in the process can be used as an additional product.
In the case of no adding alumina, fluorine and aluminum form aluminum fluoride, and the aluminum fluoride can not completely react with sulfuric acid to generate hydrogen fluoride to be discharged (about only 80 percent of fluorine is discharged in the form of hydrogen fluoride), but after adding alumina, the aluminum fluoride and the sulfuric acid are promoted to react to further generate hydrogen fluoride to be discharged, so that the roasting reaction is more thorough and efficient.
Drawings
FIG. 1 is a flow chart of the method for efficiently treating aluminum electrolysis solid waste of the present invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying fig. 1, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Comparative example 1
An acidification roasting method for efficiently treating aluminum electrolysis solid waste comprises the following specific operations:
taking 20g of pure cryolite, and reserving the cryolite in a particle form of less than 200 meshes; uniformly mixing the aluminum oxide powder and aluminum oxide in a mass ratio of 1: 0; preparing sulfuric acid with a concentration of 98%: mixing the uniformly mixed material and concentrated sulfuric acid in a mass ratio of 1:5, adding the mixture into a crucible, placing the crucible into a roasting device, and roasting the mixture for 4 hours at the temperature of 300 ℃ at a stirring speed of 500 r/min; absorbing hydrogen fluoride gas generated by reaction with aluminum hydroxide in the roasting process; after the roasting reaction is finished and cooled, adding 400ml of deionized water into the roasted product, stirring and reacting for 0.5h at room temperature, and filtering to obtain filtrate and filter residue; washing and drying the filter residue; the obtained filtrate is a sulfate solution containing sodium sulfate and aluminum sulfate, and the main component of the filter residue is aluminum fluoride. The fluorine conversion during calcination was calculated to be 78.9%.
Example 1
An acidification roasting method for efficiently treating aluminum electrolysis solid waste comprises the following specific operations:
taking 20g of pure cryolite, and reserving the cryolite in a particle form of less than 200 meshes; uniformly mixing the aluminum oxide powder and aluminum oxide in a mass ratio of 1: 1; preparing sulfuric acid with a concentration of 98%: mixing the uniformly mixed material and concentrated sulfuric acid in a mass ratio of 1:4, adding the mixture into a crucible, placing the crucible into a roasting device, and roasting the mixture for 2 hours at the temperature of 250 ℃ at a stirring speed of 500 r/min; absorbing hydrogen fluoride gas generated by reaction with aluminum hydroxide in the roasting process; after the roasting reaction is finished and cooled, adding 400ml of deionized water into the roasted product, stirring and reacting for 1h at room temperature, and filtering to obtain filtrate and filter residue; washing and drying the filter residue; the obtained filtrate is a sulfate solution containing sodium sulfate and aluminum sulfate, and the main component of the filter residue is alumina. The fluorine conversion during calcination was calculated to be 99.9%.
The raw materials of the comparative example and the example are pure cryolite. In the case of no addition of alumina as described in comparative example 1, the cryolite was not completely converted, so the residue remaining was aluminum fluoride. After the addition of a certain amount of alumina acid for the conversion to hydrogen fluoride as described in example 1, the cryolite was almost completely converted to hydrogen fluoride and only the added alumina was present in the residue, indicating that the addition of alumina has a promoting effect on the conversion of fluoride during the acid roasting process, while the added alumina can be recycled.
Example 2
An acidification roasting method for efficiently treating aluminum electrolysis solid waste comprises the following specific operations:
taking 20g of waste solid aluminum electrolyte, and crushing, ball-milling and screening the waste solid aluminum electrolyte to obtain particles smaller than 200 meshes for later use; uniformly mixing the aluminum oxide powder and aluminum oxide in a mass ratio of 2: 1; preparing sulfuric acid with a concentration of 98%: mixing the uniformly mixed material and concentrated sulfuric acid in a mass ratio of 1:1, adding the mixture into a crucible, placing the crucible into a roasting device, and roasting the mixture for 1 hour at the temperature of 150 ℃ at a stirring speed of 500 r/min; aluminum hydroxide and hydrogen fluoride gas generated by adsorption reaction are used in the roasting process; after the roasting reaction is finished and cooled, adding 400ml of deionized water into the roasted product, stirring and reacting for 1h at room temperature, and filtering to obtain filtrate and filter residue; washing and drying the filter residue; the obtained filtrate is sulfate solution containing valuable elements such as sodium sulfate, aluminum sulfate, potassium sulfate, lithium sulfate and the like, and the filter residue is solid aluminum fluoride and cryolite. The fluorine conversion during calcination was calculated to be 50.7%.
Example 3
An acidification roasting method for efficiently treating aluminum electrolysis solid waste comprises the following specific operations:
taking 20g of waste solid aluminum electrolyte, and crushing, ball-milling and screening the waste solid aluminum electrolyte to obtain particles smaller than 200 meshes for later use; uniformly mixing the aluminum oxide powder and aluminum oxide in a mass ratio of 1: 1; preparing sulfuric acid with a concentration of 98%: mixing the uniformly mixed material and concentrated sulfuric acid in a mass ratio of 1:3, adding the mixture into a crucible, placing the crucible into a roasting device, and roasting the mixture for 2 hours at the temperature of 250 ℃ at a stirring speed of 500 r/min; aluminum hydroxide and hydrogen fluoride gas generated by adsorption reaction are used in the roasting process; after the roasting reaction is finished and cooled, adding 400ml of deionized water into the roasted product, stirring and reacting for 1h at room temperature, and filtering to obtain filtrate and filter residue; washing and drying the filter residue; the obtained filtrate is sulfate solution containing valuable elements such as sodium sulfate, aluminum sulfate, potassium sulfate, lithium sulfate and the like, and the filter residue is solid alumina. The fluorine conversion during calcination was calculated to be 99.0%.
Example 4
An acidification roasting method for efficiently treating aluminum electrolysis solid waste comprises the following specific operations:
taking 20g of solid matters precipitated at the bottom of an aluminum electrolysis cell (the content of alumina in the raw materials is about 50 percent, and the part of alumina has the same action with the added alumina), crushing, ball-milling and screening to enable the solid matters to be in a particle form smaller than 200 meshes for standby; uniformly mixing the aluminum oxide powder and aluminum oxide in a mass ratio of 1: 0; preparing sulfuric acid with a concentration of 98%: mixing the uniformly mixed material and concentrated sulfuric acid in a mass ratio of 1:4, adding the mixture into a crucible, placing the crucible into a roasting device, and roasting the mixture for 2 hours at the temperature of 300 ℃ at a stirring speed of 600 r/min; aluminum hydroxide and hydrogen fluoride gas generated by adsorption reaction are used in the roasting process; after the roasting reaction is finished and cooled, adding 400ml of deionized water into the roasted product, stirring and reacting for 0.5h at room temperature, and filtering to obtain filtrate and filter residue; washing and drying the filter residue; the obtained filtrate is sulfate solution containing valuable elements such as sodium sulfate, aluminum sulfate, potassium sulfate, lithium sulfate and the like, and the filter residue is solid alumina. The fluorine conversion during calcination was calculated to be 98.7%.
Claims (7)
1. An acidification roasting method for efficiently treating aluminum electrolysis solid waste is characterized in that the method comprises the steps of uniformly mixing the aluminum electrolysis solid waste and alumina in proportion, carrying out acidification roasting, and carrying out wet water immersion treatment; the aluminum electrolysis solid waste comprises waste solid aluminum electrolyte, aluminum electrolysis cell bottom sediment and aluminum electrolysis anode covering material; the alumina is alpha-alumina.
2. The acid roasting method for efficiently treating the aluminum electrolysis solid waste according to claim 1, wherein before the acid roasting, the aluminum electrolysis solid waste is crushed, ball-milled and sieved to ensure that the particle size of the aluminum electrolysis solid waste is less than 200 meshes, so as to obtain a granular material.
3. The acid roasting method for efficiently treating the aluminum electrolysis solid waste is characterized in that the obtained granular material and alumina are mixed according to the mass ratio of 2: 1-1: 2 to obtain uniformly mixed granular material.
4. The acid roasting method for efficiently treating the aluminum electrolysis solid waste according to claim 3, characterized in that the uniformly mixed granular material is mixed with concentrated sulfuric acid with the concentration of 98%, and the mass ratio of the granular material to the concentrated sulfuric acid is 1: (1-5) placing the crucible into a roasting device, and roasting for 1-4 hours at the temperature of 150-300 ℃ and at the stirring speed of 200-600 r/min; and (3) absorbing hydrogen fluoride gas generated by reaction by using aluminum hydroxide, sodium hydroxide or calcium hydroxide in the roasting process, and calculating the fluorine conversion rate in the roasting process.
5. The acidification roasting method for efficiently treating the aluminum electrolysis solid waste according to claim 1, wherein the wet water immersion treatment is to add deionized water into a roasted product, and stir and react for 0.5-2 h at room temperature.
6. The acidification roasting method for efficiently treating the aluminum electrolysis solid waste according to claim 5, characterized in that after the stirring reaction is finished, filtration and separation are carried out to separate out salt solution containing valuable elements and solid precipitate, and the solid precipitate is washed and dried.
7. The acid roasting method for efficiently treating the aluminum electrolysis solid waste according to claim 6, wherein the obtained valuable element-containing salt solution comprises sodium sulfate, aluminum sulfate, potassium sulfate and lithium sulfate; the resulting solid precipitated as alumina.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114229874A (en) * | 2022-01-25 | 2022-03-25 | 东北大学 | Method for preparing nano alumina |
| CN116081658A (en) * | 2023-02-14 | 2023-05-09 | 安徽鑫纪源科技有限公司 | Purification method for preparing industrial grade lithium carbonate from electrolytic waste residues |
| CN116477650A (en) * | 2023-05-15 | 2023-07-25 | 中南大学 | Method for recovering cryolite with low molecular ratio by underacid roasting of aluminum electrolyte waste residues |
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| CN116081658A (en) * | 2023-02-14 | 2023-05-09 | 安徽鑫纪源科技有限公司 | Purification method for preparing industrial grade lithium carbonate from electrolytic waste residues |
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| CN116477650A (en) * | 2023-05-15 | 2023-07-25 | 中南大学 | Method for recovering cryolite with low molecular ratio by underacid roasting of aluminum electrolyte waste residues |
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