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CN113981232A - Method for directly leaching and recovering lithium element in aluminum electrolyte waste residue by using aluminum sulfate - Google Patents

Method for directly leaching and recovering lithium element in aluminum electrolyte waste residue by using aluminum sulfate Download PDF

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Publication number
CN113981232A
CN113981232A CN202111323230.8A CN202111323230A CN113981232A CN 113981232 A CN113981232 A CN 113981232A CN 202111323230 A CN202111323230 A CN 202111323230A CN 113981232 A CN113981232 A CN 113981232A
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aluminum
waste residue
lithium
filtrate
aluminum sulfate
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旷戈
郑芳妍
刘粤
姜昀
李延鹤
刘慧勇
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Xinyu Guoxing Lithium Industry Co ltd
Fuzhou University
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Xinyu Guoxing Lithium Industry Co ltd
Fuzhou University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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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  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a method for directly leaching and recovering lithium element aluminum sulfate in aluminum electrolyte waste residue, which comprises the following steps: (1) grinding and screening the lithium-containing aluminum electrolyte waste residue, mixing the waste residue with aluminum sulfate and water for reaction, and filtering to obtain filtrate A and filter residue B; (2) adding sodium carbonate into the filtrate A for reaction, and filtering to obtain filtrate C and filter residue D; (3) adding water into the filter residue D, and introducing CO2Filtering to obtain filtrate E and filter residue F; (4) carrying out thermal decomposition, filtration and drying on the filtrate E to obtain lithium carbonate; (5) and (3) evaporating and concentrating the filtrate C to obtain a byproduct sodium sulfate, and recycling the mother liquor obtained by evaporation and concentration to the step (2). (6) And (4) reacting the filter residue F with sulfuric acid to obtain aluminum sulfate, and recycling the aluminum sulfate to the step (1). The method effectively utilizes lithium in the aluminum electrolyte waste residue, has low cost and simple steps, and does not use strong lithium in the lithium leaching processThe acid is beneficial to environmental protection and subsequent impurity removal, and also can effectively recycle resources.

Description

Method for directly leaching and recovering lithium element in aluminum electrolyte waste residue by using aluminum sulfate
Technical Field
The invention belongs to the technical field of lithium recovery, and belongs to the field of aluminum sulfate direct leaching method for recovering aluminum electrolyte waste residues.
Background
Lithium resources have a very high value in the fields of batteries, ceramics, aluminum smelting industry and the like. With the increase of the consumption number of mobile devices such as mobile phones and computers, the lithium ion batteries have a larger market. China is also one of the countries with abundant lithium resources, and the lithium resources in China account for about 13% of the reserves of the lithium resources in the world. Lithium resources in China are mainly divided into lepidolite, spodumene and salt lake brine. The consumption of lithium resources in the world is also increasing year by year, and therefore the demand for lithium carbonate is also increasing year by year.
Since the raw material of the electrolytic aluminum contains a certain amount of lithium oxide and lithium fluoride as one of the additives of the aluminum electrolyte, lithium is enriched during the process of electrolyzing the aluminum. Therefore, the electrolytic aluminum waste residue contains 1 to 7% of lithium. With the increase of the capacity of the aluminum electrolysis plant, the amount of the surplus industrial electrolyte per year is also increasing, for example, the surplus electrolyte per year can reach 2800t in the aluminum electrolysis plant which produces 20 ten thousand tons per year, and thus a large amount of solid waste is produced each year. Lithium-containing aluminum electrolyte waste residue can not be effectively treated, so that site resources of a factory are occupied. Because the waste lithium-containing aluminum electrolyte slag is generated in the electrolytic process, the waste lithium-containing aluminum electrolyte generated in the production process needs to be taken out from the electrolytic cell, and then new additives or supplementary electrolyte is added to adjust the electrolyte components in the electrolytic cell, so that the cost is increased, and the economic loss is indirectly caused. The aluminum electrolyte waste residue contains a large amount of fluorine, and is a dangerous waste. Therefore, the aluminum electrolyte waste residue causes great pollution to the environment.
In the prior art, CN105293536A discloses a method for extracting lithium from electrolytic aluminum waste residues. The method comprises the steps of reacting electrolytic aluminum waste residue with concentrated sulfuric acid, adding water for leaching, and then obtaining lithium carbonate through alkaline hydrolysis reaction, causticization reaction and carbonization reaction. The method uses concentrated sulfuric acid for high-temperature roasting, and has high requirements on equipment. CN105925819A discloses a method for comprehensively recovering lithium element in aluminum electrolyte by using an acid roasting leaching method. Mixing the aluminum electrolyte with acid salt, then carrying out acid roasting, adding water to adjust the pH value, then filtering, and then adding carbonate to finally obtain the lithium carbonate. The roasting temperature of the method can reach 800 ℃ at most, and the method has extremely high requirements on equipment. CN 108569711A discloses a method for extracting lithium salt from waste of aluminum electrolysis high-lithium electrolyte to prepare lithium carbonate. Preparing lithium sulfate solution from electrolyte waste, filtering, removing impurities from filtrate, depositing lithium, filtering for the second time to obtain crude lithium carbonate, washing with water, and drying to obtain the finished lithium carbonate product. The method uses dilute sulfuric acid to react, is easy to react with other fluorides in electrolyte, is high in fluorine content in the prepared lithium sulfate solution, is not beneficial to environmental protection, and is too high in cost due to the fact that an EDTA complexing agent is used in the impurity removal process. CN 105349786A discloses a comprehensive recycling method for lithium-containing aluminum electrolyte. The method is that the lithium-containing aluminum electrolyte is mixed with water, the pH value is adjusted to be less than 2 by using inorganic acid, and then aluminum salt is added to obtain the cryolite. The method uses an acid leaching route, is not beneficial to environmental protection, uses cation exchange resin for impurity removal, and has high cost.
Disclosure of Invention
The invention relates to a method for directly leaching and extracting lithium element in aluminum electrolyte waste residue by using aluminum sulfate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for directly leaching and recovering lithium aluminum sulfate in aluminum electrolyte waste residue is characterized by comprising the following steps:
1) grinding the aluminum electrolyte waste residue, mixing the ground aluminum electrolyte waste residue with aluminum sulfate and water according to a certain proportion for reaction, and filtering to obtain a filtrate A and a filter residue B, wherein the filtrate A is a sulfate solution, and fluorine-containing lithium salt in the electrolyte waste residue is converted into aluminum fluoride to enter the filter residue B;
2) adding sodium carbonate into the filtrate A obtained in the step 1) for reaction, and filtering to obtain a filtrate C and a filter residue D, wherein the filtrate C is a sodium sulfate solution, and the filter residue D is lithium carbonate and aluminum hydroxide;
3) adding water into the filter residue D obtained in the step 2) to prepare slurry, and then introducing CO2Carrying out carbonization reaction, and filtering to obtain a filtrate E and a filter residue F, wherein the filtrate E is a lithium bicarbonate solution, and the filter residue F is aluminum hydroxide;
4) carrying out thermal decomposition on the filtrate E obtained in the step 3), and filtering and drying to obtain lithium carbonate.
In the step 1), the reaction temperature is 30-90 ℃, the pH value ranges from 2.5 to 3.5, and the reaction time is 1-5 h;
in the step 2), the reaction temperature is 30-100 ℃, and the reaction time is 1-3 h;
the solid-to-liquid ratio of the filter residue D to water in the step 3) is 1: 2-10,
step 3), the carbonization reaction pressure is 0-1.0 Mpa, the time is 0.5-5 h, and the temperature is less than or equal to 40 ℃;
step 4), the thermal decomposition temperature is 70-100 ℃;
concentrating the filtrate C obtained in the step 2) by evaporation to obtain a byproduct sodium sulfate.
The chemical reaction equation related to the invention is as follows:
step 1
2Na2LiAlF6+Al2(SO4)3=2Li2SO4+4AlF3+2Na2SO4
Step 2
Al2(SO4)3+3Na2CO3+3H2O=2Al(OH)3+3Na2SO4+3CO2
Li2SO4+Na2CO3=Li2CO3+Na2SO4
Step 3
Li2CO3+CO2+H2O=2LiHCO3
Step 4
2LiHCO3=Li2CO3+H2O+CO2
The invention provides a method for extracting lithium from lithium-containing aluminum electrolyte waste residue. Has the following advantages:
(1) the method directly uses the aluminum sulfate to leach the lithium in the electrolytic aluminum waste residue, is more favorable for environmental protection, and has low leaching temperature and low requirement on equipment. And the leaching rate of lithium can reach 99%.
(2) In the invention, the aluminum sulfate solution is directly used for leaching lithium without adding acid, and the pH range of the solution is 2.5-3.5, and the aluminum sulfate solution is not hydrolyzed in the pH range, so that the water and ion state is kept in the solution, and F ions are not changed into HF to volatilize. And the aluminum ion has very strong capability of combining with the F ion, and the aluminum ion in the aluminum sulfate is combined with the F ion to generate aluminum fluoride precipitate. So that F in the aluminum electrolyte waste slag can be remained in the reaction slag. Is beneficial to environmental protection and subsequent impurity removal and recovery of lithium carbonate.
(3) The invention provides a method with simpler step and lower requirement on equipment for treating the aluminum electrolyte waste residue. And the production cost is also lower.
Drawings
FIG. 1 is a process flow chart of a direct leaching and recovering method of aluminum sulfate of lithium element in aluminum electrolyte waste residue.
Detailed description of the preferred embodiments
Example 1
The aluminum electrolyte waste residue is crushed to 75 meshes, and then aluminum sulfate and water are added to prepare slurry. Wherein Li in the aluminum electrolyte waste residue+With Al in aluminium sulphate3+The molar ratio of (1: 1), the solid-to-liquid ratio of 1:3, and the pH value of 3. The reaction was carried out at 40 ℃ for 3 h. Filtering to obtain a filtrate A; sodium carbonate was added to the filtrate A to adjust the pH to 8. Reacting for 1h at 60 ℃, and filtering to obtain filter residue D and filtrate C; mixing the filter residue D and water in a solid-to-liquid ratio of 1:2 to prepare slurry, and reacting for 0.5h at 0.5Mpa and 30 ℃ to obtain a filtrate E;and carrying out pyrolysis reaction on the filtrate E at the temperature of 80 ℃ to obtain lithium carbonate, wherein the total lithium yield in the aluminum electrolyte is 99.3%.
Example 2
The aluminum electrolyte waste residue is crushed to 120 meshes, and then aluminum sulfate and water are added to prepare slurry. Wherein Li in the aluminum electrolyte waste residue+With Al in aluminium sulphate3+The molar ratio of (1: 2), the solid-to-liquid ratio of 1:5 and the pH value of 2.5. The reaction was carried out at 40 ℃ for 3 h. Filtering to obtain a filtrate A; sodium carbonate was added to the filtrate A to adjust the pH to 7. Reacting for 1h at 80 ℃, and filtering to obtain filter residue D and filtrate C; mixing the filter residue D and water in a solid-to-liquid ratio of 1:3 to prepare slurry, and reacting for 1h at the temperature of 20 ℃ under 0.5Mpa to obtain filtrate E; and carrying out pyrolysis reaction on the filtrate E at the temperature of 90 ℃ to obtain lithium carbonate, wherein the total lithium yield in the aluminum electrolyte is 99.5%. .
Example 3
The aluminum electrolyte waste residue is crushed to 200 meshes, and then aluminum sulfate and water are added to prepare slurry. Wherein Li in the aluminum electrolyte waste residue+With Al in aluminium sulphate3+The molar ratio of (1: 2.5), the solid-to-liquid ratio of 1:2 and the pH value of 3. The reaction was carried out at 60 ℃ for 2 h. Filtering to obtain a filtrate A; sodium carbonate was added to the filtrate A to adjust the pH to 9. Reacting at 70 deg.C for 1h, filtering to obtain residue D and filtrate C, mixing residue D and water at a solid-to-liquid ratio of 1:4 to obtain slurry, and reacting at 0.5Mpa and 30 deg.C for 0.5h to obtain filtrate E; and carrying out pyrolysis reaction on the filtrate E at the temperature of 90 ℃ to obtain lithium carbonate, wherein the total lithium yield in the aluminum electrolyte is 99.25%.
Example 4
The aluminum electrolyte waste residue is crushed to 200 meshes, and then aluminum sulfate and water are added to prepare slurry. Wherein Li in the aluminum electrolyte waste residue+With Al in aluminium sulphate3+The molar ratio of (1: 4), the solid-to-liquid ratio of 1:5 and the pH value of 4.3. The reaction was carried out at 50 ℃ for 4 h. Filtering to obtain a filtrate A; sodium carbonate was added to the filtrate A to adjust the pH to 8. Reacting at 90 deg.C for 1h, filtering to obtain residue D and filtrate C, mixing residue D and water at a solid-to-liquid ratio of 1:4 to obtain slurry, and reacting at 30 deg.C under 0.5Mpa for 0.5h to obtain filtrate E; and carrying out pyrolysis reaction on the filtrate E at the temperature of 85 ℃ to obtain lithium carbonate, wherein the total lithium yield in the aluminum electrolyte is 99.15%.
Example 5
The aluminum electrolyte waste residue is crushed to 300 meshes, and then aluminum sulfate and water are added to prepare slurry. Wherein Li in the aluminum electrolyte waste residue+With Al in aluminium sulphate3+The molar ratio of (1: 3), the solid-to-liquid ratio of 1:5 and the pH value of 3.2. The reaction was carried out at 70 ℃ for 4 h. Filtering to obtain a filtrate A; sodium carbonate was added to the filtrate A to adjust the pH to 10. Reacting at 90 deg.C for 2h, filtering to obtain residue D and filtrate C, mixing residue D and water at a solid-to-liquid ratio of 1:5 to obtain slurry, and reacting at 0.5Mpa and 20 deg.C for 0.5h to obtain filtrate E; and carrying out pyrolysis reaction on the filtrate E at 100 ℃ to obtain lithium carbonate, wherein the total lithium yield in the aluminum electrolyte is 99.55%.
Example 6
The aluminum electrolyte waste residue is crushed to 400 meshes, and then aluminum sulfate and water are added to prepare slurry. Wherein Li in the aluminum electrolyte waste residue+With Al in aluminium sulphate3+The molar ratio of (1: 4), the solid-to-liquid ratio of 1:5 and the pH value of 3.3. The reaction was carried out at 65 ℃ for 5 h. Filtering to obtain a filtrate A; sodium carbonate was added to the filtrate A to adjust the pH to 10. Reacting at 80 deg.C for 3h, filtering to obtain residue D and filtrate C, mixing residue D and water at a solid-to-liquid ratio of 1:6 to obtain slurry, and reacting at 30 deg.C under 0.5Mpa for 0.5h to obtain filtrate E; and carrying out pyrolysis reaction on the filtrate E at the temperature of 90 ℃ to obtain lithium carbonate, wherein the total lithium yield in the aluminum electrolyte is 99.05%.
The above embodiments are illustrative of the present invention, but the present invention is not limited to the above embodiments, and any changes, modifications, substitutions, combinations, and simplifications made without departing from the scope of the present invention shall be considered as equivalent replacements within the scope of the present invention.

Claims (10)

1.一种铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：具体包括如下步骤：1. the aluminum sulfate direct leaching recovery method of lithium element in aluminum electrolyte waste residue is characterized in that: specifically comprise the steps: (1)将铝电解质废渣粉碎研磨，与硫酸铝、水混合进行反应，得到滤液A和滤渣B；(1) the aluminum electrolyte waste residue is pulverized and ground, mixed with aluminum sulfate, water and reacted to obtain filtrate A and filter residue B; (2)步骤(1)中所得的滤液A为硫酸锂、硫酸钠及硫酸铝的混合硫酸盐溶液，在硫酸盐溶液中加入碳酸钠进行反应，过滤后得到滤液C及滤渣D；(2) filtrate A obtained in step (1) is the mixed sulfate solution of lithium sulfate, sodium sulfate and aluminum sulfate, in sulfate solution, sodium carbonate is added to react, and filtrate C and filter residue D are obtained after filtering; (3)步骤(2)中滤渣D加入水配成浆料，然后通入CO2进行碳化反应，过滤后得到滤液E和滤渣F；(3) in step (2), filter residue D is added with water and made into slurry, then CO is passed into it to carry out carbonization reaction, and filtrate E and filter residue F are obtained after filtration; (4)将步骤(3)中得到的滤液E经过热分解、过滤及干燥后得到碳酸锂。(4) The filtrate E obtained in step (3) is thermally decomposed, filtered and dried to obtain lithium carbonate. 2.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(1)中，铝电解质废渣粉碎研磨至75~400目，铝电解质废渣中Li+与硫酸铝中Al3 +的摩尔比为1:0.5~5，固液比为1:2~15，pH值范围2.5~3.5。2. according to the aluminum sulfate direct leaching recovery method of lithium element in the aluminum electrolyte waste residue described in claim 1, it is characterized in that: in step (1), the aluminium electrolyte waste residue is pulverized and ground to 75～400 orders, and in the aluminium electrolyte waste residue, Li The molar ratio of + to Al 3 + in aluminum sulfate is 1:0.5~5, the solid-liquid ratio is 1:2~15, and the pH value range is 2.5~3.5. 3.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(1)中反应温度为30~90℃，反应时间为1~5h。3. according to the aluminum sulfate direct leaching recovery method of lithium element in the aluminum electrolyte waste residue described in claim 1, it is characterized in that: in step (1), the reaction temperature is 30～90 ℃, and the reaction time is 1～5h. 4.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(2)中加入碳酸钠调节pH为6~12，所获滤渣D为碳酸锂与氢氧化铝混合物。4. according to the aluminum sulfate direct leaching recovery method of lithium element in the aluminum electrolyte waste residue described in claim 1, it is characterized in that: in step (2), adding sodium carbonate to adjust pH is 6～12, and the obtained filter residue D is lithium carbonate mixed with aluminium hydroxide. 5.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(2)中反应温度为30~100℃，反应时间为1~3h。5. according to the aluminum sulfate direct leaching recovery method of lithium element in the aluminum electrolyte waste residue described in claim 1, it is characterized in that: in step (2), the reaction temperature is 30～100 ℃, and the reaction time is 1～3h. 6.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(3)中滤渣D与水的固液比为1:2~10。6. according to the aluminum sulfate direct leaching recovery method of lithium element in the aluminum electrolyte waste residue described in claim 1, it is characterized in that: in step (3), the solid-liquid ratio of filter residue D and water is 1:2～10. 7.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(3)中碳化反应压力0~1.0Mpa，时间为0.5~5h，温度≤40℃。7. according to the aluminum sulfate direct leaching recovery method of lithium element in the aluminum electrolyte waste residue described in claim 1, it is characterized in that: carbonization reaction pressure 0～1.0Mpa in step (3), time is 0.5～5h, temperature≤40 °C. 8.根据权利要求1中所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(4)中热分解温度为70~100℃。8. The aluminum sulfate direct leaching recovery method of lithium element in aluminum electrolyte waste residue according to claim 1, is characterized in that: in step (4), thermal decomposition temperature is 70～100 ℃. 9.根据权利要求1所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(2)中得到的滤液C通过蒸发浓缩得到副产品硫酸钠，蒸发浓缩母液循环回步骤(2)。9. the aluminum sulfate direct leaching recovery method of lithium element in aluminum electrolyte waste residue according to claim 1, is characterized in that: the filtrate C obtained in step (2) obtains by-product sodium sulfate by evaporation concentration, and evaporation concentration mother liquor is circulated back to step (2). 10.根据权利要求1所述的铝电解质废渣中锂元素的硫酸铝直接浸出回收方法，其特征在于：步骤(3)中得到的滤渣F与硫酸反应得到硫酸铝，循环回步骤(1)。10. The aluminum sulfate direct leaching recovery method of lithium element in aluminum electrolyte waste residue according to claim 1 is characterized in that: the filter residue F obtained in step (3) reacts with sulfuric acid to obtain aluminum sulfate, which is recycled back to step (1).
CN202111323230.8A 2021-11-10 2021-11-10 Method for directly leaching and recovering lithium element in aluminum electrolyte waste residue by using aluminum sulfate Pending CN113981232A (en)

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CN115672952A (en) * 2022-10-27 2023-02-03 云南云铝润鑫铝业有限公司 Method for extracting sodium sulfide by using electrolytic aluminum hazardous waste residues
CN115959689A (en) * 2022-12-28 2023-04-14 云南云铝润鑫铝业有限公司 Method for enriching and extracting lithium salt from overhaul residues and carbon residues
CN116334411A (en) * 2023-04-11 2023-06-27 珠海市瑞斐门特科技有限公司 Recovery method for extracting lithium element from aluminum electrolyte slag at low temperature in multiple stages
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