CN116219204A - Method for circularly extracting lithium from lepidolite and lithium carbonate prepared by method - Google Patents

Method for circularly extracting lithium from lepidolite and lithium carbonate prepared by method Download PDF

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Publication number
CN116219204A
CN116219204A CN202211734747.0A CN202211734747A CN116219204A CN 116219204 A CN116219204 A CN 116219204A CN 202211734747 A CN202211734747 A CN 202211734747A CN 116219204 A CN116219204 A CN 116219204A
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lithium
sulfate
lepidolite
calcium
calcium oxide
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汪金良
王厚庆
徐木财
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Jiangxi Shanning Technology Co ltd
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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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/06—Sulfating roasting
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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

Abstract

The invention belongs to the technical field of lithium battery material production, and particularly relates to a method for circularly extracting lithium from lepidolite and lithium carbonate prepared by the method. The method adopts a sulfate roasting method to produce lithium products, the used auxiliary materials are calcium sulfate and calcium oxide and/or calcium carbonate, sulfuric acid is adopted to neutralize mother liquor in a precipitation step and/or filtrate in a filtering step after precipitation to a pH value of 5.5-7, mixed sulfate is obtained through evaporation and crystallization, and then the mixed sulfate is used for replacing the calcium sulfate in the auxiliary materials to continuously extract lithium. According to the invention, elements such as sodium and potassium generated in the lepidolite lithium extraction process are fully utilized, sulfate obtained by crystallizing the mother solution for the previous lithium extraction is used as an auxiliary material for the subsequent lithium extraction, so that the whole process has no waste liquid discharge, and is economical and environment-friendly.

Description

Method for circularly extracting lithium from lepidolite and lithium carbonate prepared by method
Technical Field
The invention belongs to the technical field of production of lithium battery materials, and particularly relates to a method for circularly extracting lithium from lepidolite and lithium carbonate prepared by the method.
Background
Lepidolite is one of the important lithium resources, and is the mineral raw material most commonly used for extracting lithium. How to efficiently and economically decompose lepidolite and dissolve out lithium in the lepidolite is a key for preparing various lithium compounds by extracting lithium from lepidolite. At present, various methods for producing lithium salt by taking solid lepidolite as a raw material at home and abroad are divided into two main types, namely a mixed sintering method mainly comprising a lime method, a chloride method and a sulfate method; the other is an autoclave process, which mainly comprises a sulfuric acid process and a liquid-alkali process. The autoclaving method belongs to the field of reinforced metallurgy, has high operation requirements on field equipment and workers, and has potential safety hazards; the limestone method in the mixed sintering method needs limestone with the quantity being 3 times that of lepidolite, so that the energy consumption is extremely high, and the chlorination method has serious corrosion to equipment, so that the method is not beneficial to environmental protection; the sulfate process is the most mainstream process at present, and basically lithium carbonate is produced through the process of roasting-leaching-impurity removal-precipitation-washing-filtration, but mainly used auxiliary materials are potassium sulfate, sodium sulfate, calcium oxide and the like, and the cost is high. Therefore, it is necessary to develop a lithium extraction technology with high efficiency, environmental protection and low energy consumption.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is the defects of low lithium recovery rate, poor economical efficiency and poor environmental protection of the existing lithium extraction process by the sulfate roasting method, and further provides a novel economic and environmental protection lepidolite cyclic lithium extraction method capable of remarkably improving the comprehensive recovery rate of lithium.
The invention aims at realizing the following technical scheme:
according to a first aspect of the embodiments of the present invention, the present invention provides a method for cyclic lithium extraction from lepidolite, comprising the steps of:
mixing lepidolite and auxiliary materials to obtain a mixture, and sequentially roasting, leaching, primary filtering, primary filtrate impurity removal, precipitation and secondary filtering the mixture to obtain a secondary filtering solid, namely a lithium product;
the auxiliary materials are calcium sulfate, calcium oxide and/or calcium carbonate;
and neutralizing mother liquor in the precipitation step and/or secondary filtrate in the secondary filtration step by sulfuric acid until the pH value is 5.5-7, evaporating and crystallizing to obtain mixed sulfate, and using the mixed sulfate to replace calcium sulfate in the auxiliary material to continuously extract lithium.
In the embodiment of the invention, the mass ratio of the lepidolite to the calcium sulfate to the calcium oxide is 18:4-10:1.5-6 based on dry weight.
In the embodiment of the invention, the calcium sulfate is solid waste calcium sulfate generated in a process of producing lithium hydroxide by a lime method or a hydrofluoric acid smelting plant, and the mass percentage of the calcium sulfate in the solid waste calcium sulfate is not less than 50%.
In an embodiment of the present invention, the calcium oxide is derived from solid waste calcium oxide or industrial calcium oxide, and the mass percentage of calcium oxide in the solid waste calcium oxide is not less than 70%.
In the embodiment of the invention, when the auxiliary material adopts calcium sulfate, the roasting temperature in the roasting step is 950-1100 ℃ and the roasting time is 20-80 min.
In an embodiment of the present invention, the total dry weight of sodium sulfate, potassium sulfate, and lithium sulfate in the mixed sulfate is not less than 25%.
In the embodiment of the invention, the mass ratio of the lepidolite to the mixed sulfate to the calcium oxide is 18:7-12:1.5-6 based on dry weight.
In the embodiment of the invention, when the mixed sulfate is adopted as the auxiliary material, the roasting temperature in the roasting step is 880-1000 ℃ and the roasting time is 20-80 min.
In an embodiment of the present invention, the lithium product is at least one of lithium carbonate, lithium phosphate, and lithium oxalate.
According to a second aspect of the embodiment of the invention, the invention also provides lithium carbonate prepared by the above lepidolite cyclic lithium extraction method, wherein the mass percentage of the lithium carbonate is more than 99%.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. according to the lepidolite cyclic lithium extraction method provided by the embodiment of the invention, a sulfate roasting method is adopted to produce a lithium product, wherein the used auxiliary materials are calcium sulfate, calcium oxide and/or calcium carbonate, sulfuric acid is adopted to neutralize mother liquor in a precipitation step and/or filtrate in a filtering step after precipitation to a pH value of 5.5-7, evaporation crystallization is carried out to obtain mixed sulfate, and the mixed sulfate is recycled to the lithium extraction process to replace the calcium sulfate in the auxiliary materials for continuous lithium extraction. According to the lithium extraction method disclosed by the invention, sodium, potassium and other elements generated in the lepidolite lithium extraction process are fully utilized, the mother solution of the previous lithium extraction is crystallized, and the obtained sulfate can be used as an auxiliary material for the subsequent lithium extraction, so that the whole process is free from waste liquid discharge, and is economical and environment-friendly.
2. According to the lepidolite cyclic lithium extraction method provided by the embodiment of the invention, the used auxiliary materials are calcium sulfate, calcium oxide and/or calcium carbonate, the calcium sulfate is slightly soluble, and calcium, potassium, sodium and lithium are in a non-same main group relationship, so that the leaching rate of lithium is prevented from being reduced due to the leaching of positive ions potassium and sodium in the leaching process, the leaching rate of lithium is higher, the melting point of lithium ore can be improved by the calcium oxide and/or the calcium carbonate, the lithium ore is calcined at a higher temperature, the reaction is ensured to be more sufficient, the leaching rate of lithium is greatly improved, the glassy state in the calcining process can be avoided, the calcium carbonate can be decomposed to generate carbon dioxide in the calcining process, the filter residues are more loose, and the subsequent efficient operation of the processes of leaching, washing, filtering and the like is facilitated.
3. According to the lepidolite cyclic lithium extraction method provided by the embodiment of the invention, solid waste calcium sulfate (gypsum) generated in the process of smelting hydrofluoric acid by using chemical plants and fluorite is used as an auxiliary material, so that the conversion and utilization of solid waste are realized, the cost of extracting lithium ores is reduced, the gypsum (namely calcium sulfate crystal water) begins to lose crystal water when the temperature is more than 100 ℃, and at the moment, the gypsum is combined with fluorine in adjacent lepidolite to form hydrogen fluoride to volatilize, and the fluorine removal difficulty in the subsequent leaching solution is reduced; the crystal water is slowly released and has sufficient reaction time with fluorine in the lepidolite, in addition, gypsum and the lepidolite are in a tightly connected state after being mixed, and can react among the interiors of particles, so that a very good defluorination effect is achieved, and the prepared lithium product has better quality and longer service life after defluorination.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
In the examples and comparative examples of the present invention, the desulfurization gypsum used was obtained from the desulfurization process of a power plant, 2 molecules of water was contained in 1 molecule of desulfurization gypsum, and the quicklime used was purchased from a lime plant, and the lepidolite ore used was composed as shown in table 1.
TABLE 1 lepidolite ore composition
Composition of the components SiO 2 Al 2 O 3 K 2 O Na 2 O CaO MgO Fe 2 O 3 Li 2 O MnO
Content wt.% 67.86 17.13 4.25 5.21 0.66 0.04 1.08 2.35 0.23
Example 1
The lepidolite cyclic lithium extraction method provided by the embodiment comprises the following steps:
step S1, dry weight m (lepidolite): m (calcium sulfate): m (calcium oxide) =10:4:1, mixing 666.70g of lepidolite ore, 266.68g of desulfurized gypsum (containing 97.25% of calcium sulfate) and 66.67g of calcium oxide into 1000g of mixed raw materials, grinding the raw materials to about 200 meshes, placing the raw materials in a roasting furnace at 1020 ℃ for roasting for 80min, cooling, grinding the clinker, leaching with 1000mL of water for 30min, filtering, adjusting the pH value of the filtrate to be 5.5 by sulfuric acid, adjusting the solution to be neutral by sodium hydroxide, heating to 98 ℃ for precipitating by sodium carbonate (the excess coefficient is 1-1.18), filtering, and washing the precipitate by water to obtain lithium carbonate (I-1).
The mother liquor after precipitation in this step, the filtrate after filtration, and the water after washing were recovered together, neutralized to ph=7 with sulfuric acid, and evaporated to crystallize to obtain a mixed salt (dry weight 211.7 g).
And S2, mixing the mixed salt obtained in the step S1 with 470g of dry mica and 47g of calcium oxide, grinding, placing in a roasting furnace at 1000 ℃ for roasting for 20min, cooling, grinding clinker, stirring and leaching with 700mL of water for 30min, filtering, adding sodium hydroxide into filtrate to adjust pH to neutral for removing impurities, heating to 98 ℃, precipitating with sodium carbonate, filtering, and washing the precipitate with water to obtain lithium carbonate (I-2).
The mother solution after precipitation, the filtrate after filtration and the water after washing in the step are recovered together, neutralized to pH=7 by sulfuric acid, and the mixed salt obtained by evaporation and crystallization is returned to the ingredients for recycling to prepare lithium carbonate.
Example 2
Step S1, dry weight m (lepidolite): m (calcium sulfate): m (calcium oxide) =10:5:2, mixing 588.2g of lepidolite ore, 294.1g of desulfurized gypsum (containing 96.35wt.% of calcium sulfate) and 127.7g of quicklime (containing 97.8wt.% of calcium oxide) into 1000g of mixed raw materials, grinding the mixed raw materials to about 200 meshes, placing the mixed raw materials in a roasting furnace at 1080 ℃ for roasting for 40min, cooling, grinding the clinker, leaching the clinker with 1000mL of water for 30min, filtering the mixture, regulating the pH value of the filtrate with sulfuric acid to be 5.5, regulating the solution with sodium hydroxide to be neutral for removing impurities, heating the filtrate to 98 ℃, precipitating the filtrate with sodium carbonate (with an excess coefficient of 1-1.18), filtering the precipitate, and washing the precipitate with water to obtain lithium carbonate (II-1).
The mother liquor after precipitation in this step, the filtrate after filtration, and the water after washing were recovered together, neutralized to ph=5.5 with sulfuric acid, and evaporated to crystallize to obtain a mixed salt (dry weight 219.2 g).
And S2, mixing the mixed salt obtained in the step S1 with 480g of dry mica and 42g of calcium oxide, grinding, placing in a roasting furnace at 950 ℃ for roasting for 40min, cooling, grinding clinker, stirring and leaching with 700mL of water for 30min, filtering, adding sodium hydroxide into filtrate to adjust pH to be neutral, heating to 98 ℃, precipitating with sodium carbonate, filtering, and washing the precipitate with water to obtain lithium carbonate (II-2).
The mother solution after precipitation, the filtrate after filtration and the water after washing in the step are recovered together, neutralized to pH=7 by sulfuric acid, and the mixed salt obtained by evaporation and crystallization is returned to the ingredients for recycling to prepare lithium carbonate.
Example 3
Step S1, dry weight m (lepidolite): m (calcium sulfate): m (calcium oxide) =20:9:5, mixing 588.2g of lepidolite ore, 264.7g of desulfurized gypsum (containing 95.45wt.% of calcium sulfate) and 147.1g of quicklime (containing 97.8wt.% of calcium oxide) into 1000g of mixed raw materials, grinding to about 200 meshes, placing the raw materials in a roasting furnace at 1100 ℃ for roasting for 40min, cooling, grinding clinker, leaching with 1000mL of water for 30min, filtering, adjusting the pH value of the filtrate with sulfuric acid to be=5.5, adjusting the solution with sodium hydroxide to be neutral for removing impurities, heating to 98 ℃, precipitating with sodium carbonate (with an excess coefficient of 1-1.2), filtering, and washing the precipitate with water to obtain lithium carbonate (III-1).
The mother liquor after precipitation in this step, the filtrate after filtration, and the water after washing were recovered together, neutralized to ph=6 with sulfuric acid, and evaporated to crystallize to obtain a mixed salt (dry weight 216.5 g).
And S2, mixing the mixed salt obtained in the step S1 with 470g of dry mica and 47g of calcium oxide, grinding, placing in a roasting furnace at 950 ℃ for roasting for 40min, cooling, grinding clinker, stirring and leaching with 700mL of water for 30min, filtering, adding sodium hydroxide into filtrate to adjust pH to be neutral, heating to 98 ℃, precipitating with sodium carbonate, filtering, and washing the precipitate with water to obtain lithium (III-2) carbonate.
The mother solution after precipitation, the filtrate after filtration and the water after washing in the step are recovered together, neutralized to pH=7 by sulfuric acid, and the mixed salt obtained by evaporation and crystallization is returned to the ingredients for recycling to prepare lithium carbonate.
Example 4
Step S1, dry weight m (lepidolite): m (calcium sulfate): m (calcium carbonate) =18:7:6, mixing 580g of lepidolite ore, 226g of calcium sulfate and 193.5g of calcium carbonate into 1000g of mixed raw materials, grinding to about 200 meshes, placing the mixed raw materials in a 950 ℃ roasting furnace for roasting for 60min, grinding clinker after cooling, stirring and leaching with 1000mL of water for 20min, filtering, adjusting pH value of filtrate to be 5.5 by sulfuric acid, adjusting solution to be neutral by sodium hydroxide, adding 50kg of calcium hydroxide into the liquid to react for 4h, filtering, evaporating and concentrating the filtrate to obtain lithium hydroxide monohydrate IV-1.
The residue precipitated in this step was neutralized to ph=7 with sulfuric acid, and the crystal water was dried to obtain a mixed salt (dry weight 1129.45 g).
And S2, mixing the mixed salt obtained in the step S1 with 1889.2g of 1129.45g of dry mica and 188.9g of calcium carbonate, grinding, roasting in a roasting furnace at 880 ℃ for 40min, cooling, grinding clinker, stirring and leaching with 700mL of water for 20min, filtering, adding sodium hydroxide into filtrate to adjust pH to neutral, heating to 98 ℃ and precipitating with sodium carbonate (with an excess coefficient of 1-1.2), filtering, and washing the precipitate with water to obtain lithium carbonate IV-2.
The mother solution after precipitation, the filtrate after filtration and the water after washing in the step are recovered together, neutralized to pH=7 by sulfuric acid, and the mixed salt obtained by evaporation and crystallization is returned to the ingredients for recycling to prepare lithium carbonate.
Comparative example 1
The other contents were the same as in example 2 except for the following.
Lithium carbonate DI-1 was prepared in the same manner as in step S1 of example 2, and lithium carbonate DI-2 was prepared in the same manner as in step S2 of example 2, using an equal amount of sodium sulfate instead of calcium sulfate.
Test examples
The purity and lithium recovery rate of the lithium carbonate products produced in examples 1 to 3 and comparative example 1 were tested, wherein the lithium recovery rate=the amount of lithium in lithium carbonate/the amount of lithium in lepidolite×100%.
The results are shown in Table 2.
TABLE 2 purity and lithium recovery of lithium carbonate products
Figure BDA0004033256510000061
Figure BDA0004033256510000071
As can be seen from Table 2, the lithium carbonate content (purity) in the lithium carbonate products prepared in examples 1 to 3 is above 99wt.%, all reach the industrial zero-order standard, which means that the invention utilizes the byproduct mixed sulfate to replace calcium sulfate, and also can prepare high-quality lithium carbonate products, and the recovery rate of lithium in lepidolite is higher than 83.5%, thereby realizing the efficient extraction of lithium element in lepidolite, and simultaneously greatly reducing the consumption of calcium sulfate, and the whole process has no waste liquid emission and good environmental protection and economy.
The components of the mixed salts obtained in examples 1 to 3 were analyzed, and the results are shown in Table 3.
TABLE 3 composition of Mixed salt
Figure BDA0004033256510000072
From table 4, the mixed salt formed by evaporation and crystallization is sulfate, and sodium salt occupies most proportion, so that mixed sulfate is fully utilized to form auxiliary material closed loop in the whole lithium extraction process, and lithium in the salt also enters a circulation system for simultaneous recovery, thereby improving the comprehensive recovery rate of lithium.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.

Claims (10)

1. A lepidolite cyclic lithium extraction method comprises the following steps:
mixing lepidolite and auxiliary materials to obtain a mixture, and sequentially roasting, leaching, primary filtering, primary filtrate impurity removal, precipitation and secondary filtering the mixture to obtain a secondary filtering solid, namely a lithium product; it is characterized in that the method comprises the steps of,
the auxiliary materials are calcium sulfate, calcium oxide and/or calcium carbonate;
and neutralizing mother liquor in the precipitation step and/or secondary filtrate in the secondary filtration step by sulfuric acid until the pH value is 5.5-7, evaporating and crystallizing to obtain mixed sulfate, and using the mixed sulfate to replace calcium sulfate in the auxiliary material to continuously extract lithium.
2. The method for circularly extracting lithium from lepidolite according to claim 1, wherein the mass ratio of lepidolite to calcium sulfate to calcium oxide is 18:4-10:1.5-6 based on dry weight.
3. The lepidolite cyclic lithium extraction method according to claim 1 or 2, wherein the calcium sulfate is solid waste calcium sulfate generated in a process of producing lithium hydroxide by a lime method or a hydrofluoric acid smelting plant, and the mass percentage of the calcium sulfate in the solid waste calcium sulfate is not less than 50%.
4. The lepidolite cyclic lithium extraction method according to claim 1 or 2, wherein the calcium oxide is derived from solid waste calcium oxide or industrial calcium oxide, and the mass percentage of calcium oxide in the solid waste calcium oxide is not less than 70%.
5. The method for circularly extracting lithium from lepidolite according to claim 1, wherein when the auxiliary material is calcium sulfate, the roasting temperature in the roasting step is 950-1100 ℃ and the roasting time is 20-80 min.
6. The method for circularly extracting lithium from lepidolite according to claim 1, wherein the total dry weight of sodium sulfate, potassium sulfate and lithium sulfate in the mixed sulfate is not less than 25%.
7. The method for circularly extracting lithium from lepidolite according to claim 6, wherein the mass ratio of lepidolite to mixed sulfate to calcium oxide is 18:7-12:1.5-6 based on dry weight.
8. The method for circularly extracting lithium from lepidolite according to claim 1, 6 or 7, wherein when the mixed sulfate is adopted as the auxiliary material, the roasting temperature in the roasting step is 880-1000 ℃ and the roasting time is 20-80 min.
9. The method for circularly extracting lithium from lepidolite according to claim 1, wherein the lithium product is at least one of lithium carbonate, lithium phosphate and lithium oxalate.
10. A lithium carbonate prepared by the lepidolite cyclic lithium extraction method according to any one of claims 1 to 9, wherein the mass percentage of the lithium carbonate is more than 99%.
CN202211734747.0A 2022-12-31 2022-12-31 Method for circularly extracting lithium from lepidolite and lithium carbonate prepared by method Pending CN116219204A (en)

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