CN110835679A - Method for preparing granular spodumene by granulating fine powder spodumene - Google Patents
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/242—Binding; Briquetting ; Granulating with binders
- C22B1/243—Binding; Briquetting ; Granulating with binders inorganic
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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
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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
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for preparing granular spodumene by granulating fine powder spodumene, which comprises the following steps: (1) drying the fine spodumene powder until the water content is 1% -3%; (2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag, a sodium silicate solution and water, the mass of the calcium slag is 4% -6% of that of the fine-powder spodumene, the mass of the sodium silicate solution is 1% -3% of that of the fine-powder spodumene, and the mass of the water is 1% -3% of that of the fine-powder spodumene; (3) and granulating and screening the mixture to obtain a finished product of the granular spodumene. The fine powder spodumene is granulated to prepare the particle spodumene by the method, so that various problems in actual production are solved, and the yield of lithium salt is increased; after the fine powder spodumene is granulated to prepare the particle spodumene, the crystal form conversion rate is provided, and the lithium yield is obviously improved; the calcium slag is added, so that the secondary recovery of lithium in the calcium slag is realized, the lithium salt yield is further improved, and the pollution of solid waste discharge to the environment is reduced.
Description
Technical Field
The invention relates to the technical field of lithium salt production, in particular to a method for preparing granular spodumene by utilizing fine powder spodumene granulation.
Background
With the development of new energy sources of lithium batteries, the demand of lithium salts is increasing. The production process of lithium salt can be divided into salt lake brine extraction and ore extraction according to different raw material sources. The salt lake brine extraction process is mainly adopted in the south and American areas abroad, the spodumene ore extraction process is mainly adopted in other areas including China, and the extraction of lithium from the ore accounts for most of the total lithium salt yield. The spodumene comprises particle spodumene and fine powder spodumene according to different ore dressing processes, and the fine powder spodumene (200-mesh screen underflow is more than or equal to 65 percent) accounts for the vast majority of the total spodumene, so that the process for extracting lithium salt from the fine powder spodumene is mainly adopted.
Because the fine-powder spodumene has large water content and small particle size, the problem of feeding blockage is easy to occur in the actual production, so that the fine-powder spodumene is wasted, the yield of lithium salt is influenced, and the blockage easily causes environmental pollution; and because the particle size of the fine-powder spodumene is small, the fine-powder spodumene is melted at a higher roasting temperature, the roasting temperature of the fine-powder spodumene is generally controlled to be 800-900 ℃, however, the optimal transformation temperature of the spodumene is 1000 ℃, that is, at 1000 ℃, the crystal transformation rate of the spodumene can reach the highest, the lower roasting temperature causes the crystal transformation rate of the fine-powder spodumene to be low, the lithium yield is seriously influenced, and great economic loss is brought to production enterprises.
In the process of preparing lithium salt from spodumene ore, calcium slag is generated in the purification and concentration processes, the traditional method for treating the calcium slag is directly thrown away as solid waste after agitation washing, but the calcium slag contains lithium, so the direct throwing of the calcium slag pollutes the environment and causes economic loss. Therefore, it is very necessary to reuse the calcium slag and improve the recovery rate of lithium.
In patent application No. 200710085901.5 entitled method for producing lithium from spodumene concentrate, although a method for producing lithium salt by granulation is disclosed, there is no disclosure on how to improve the yield of lithium and on how to secondarily recover calcium slag, which is a solid waste in a lithium salt production system. At present, no research related to the significant improvement of lithium yield and secondary lithium recovery is found in the lithium salt production method.
Disclosure of Invention
In view of the above prior art, it is an object of the present invention to provide a process for preparing granular spodumene by granulation of fine spodumene powder. The fine powder spodumene is granulated to prepare the particle spodumene, so that the problems of easy blockage, environmental pollution and the like in actual production are solved, and the yield of lithium salt is improved; after the fine powder spodumene is granulated to prepare the particle spodumene, the problem that the crystal form conversion rate is influenced due to low roasting temperature is solved, so that the yield of the lithium is obviously improved; the solid waste-calcium slag in the lithium salt production system is added into the ingredients of the adhesive, so that the secondary recovery of lithium in the calcium slag is realized, the lithium salt yield is further improved, and the environmental pollution caused by the discharge of the solid waste is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, there is provided a process for the preparation of particulate spodumene by granulation of finely divided spodumene comprising the steps of:
(1) drying the fine spodumene powder until the water content is 1% -3%;
(2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag, a sodium silicate solution and water, the mass of the calcium slag is 4% -6% of that of the fine-powder spodumene, the mass of the sodium silicate solution is 1% -3% of that of the fine-powder spodumene, and the mass of the water is 2% -4% of that of the fine-powder spodumene;
(3) and granulating and screening the mixture to obtain a finished product of the granular spodumene.
Preferably, in the step (1), the drying of the fine spodumene is carried out in a paddle dryer.
Preferably, in the step (1), the fine spodumene with a 200-mesh screen underflow of more than or equal to 65% is adopted as the fine spodumene.
Preferably, in the step (2), the calcium slag is generated after purification and concentration processes in the lithium salt preparation process. The main component of the calcium slag is calcium sulfate, and the water content of the calcium slag is 20-25%.
Preferably, the calcium slag comprises the following main components in percentage by weight: ca2+25.34％，Mg2+14.92％,Al3+5.83％，SO4 2-8.21％,CO3 2-6.27％，Li2O is less than 2 percent.
Preferably, in the step (3), extrusion granulation is adopted for the granulation.
Preferably, the extrusion type granulation adopts a roll extrusion type granulator to extrude the mixture into cuboids with the same size, and the cuboids are crushed into blocks by a crusher, wherein the extrusion pressure of the roll extrusion type granulator is 8-12 MPa.
Preferably, the screening is to screen the blocks through a rolling screen, wherein the grain diameter of qualified products is 2-3mm, and unqualified products are returned to a granulator for continuous extrusion granulation.
In a second aspect of the invention, there is provided a particulate spodumene prepared by the above process.
In a third aspect of the invention, there is provided the use of the above particulate spodumene for the preparation of a battery grade lithium salt.
The invention has the beneficial effects that:
1. the invention prepares the particle spodumene by granulating the fine powder spodumene, solves the problems of easy blockage, environmental pollution and the like in the actual production, and simultaneously improves the yield of lithium salt; after the fine powder spodumene is granulated to prepare the particle spodumene, the roasting at the temperature of 1000 ℃ can be realized, so that the problem that the crystal form conversion rate is influenced due to low roasting temperature is solved, the lithium yield is obviously improved, and great economic benefit is brought.
2. The invention adds the adhesive when the fine powder spodumene is granulated, on one hand, the addition of the adhesive is convenient for granulation, and on the other hand, the solid waste-calcium slag in the lithium salt production system is added in the ingredients of the adhesive, thereby not only realizing the secondary recovery of lithium in the calcium slag, further improving the yield of lithium salt, but also reducing the pollution of the solid waste discharge to the environment.
3. The invention greatly improves the yield of lithium, on one hand, after the calcium slag is added, the lithium in the calcium slag is recycled for the second time, so that the yield of lithium is improved, and on the other hand, the calcium slag and the sodium silicate solution with proper dosage are added to jointly cooperate and promote the yield of lithium in the process of preparing lithium salt from the spodumene particles.
4. The process for preparing the particle spodumene by the method has the advantages of simple operation, low cost, obvious economic benefit and suitability for industrial popularization, and the yield of lithium salt is obviously improved.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As introduced in the background art, the conventional spodumene crystal form has low conversion rate, and secondary recovery of calcium slag cannot be realized, so that the yield of lithium salt is low.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention were all commercially available materials that are conventional in the art and are commercially available.
Example 1: preparation of particulate spodumene
The method comprises the following steps: (1) drying the fine spodumene powder in a paddle dryer until the water content is 1% -3%;
(2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag, a sodium silicate solution and water, the mass of the calcium slag is 4% of that of the fine-powder spodumene, the mass of the sodium silicate solution is 1% of that of the fine-powder spodumene, and the mass of the water is 1% of that of the fine-powder spodumene;
(3) granulating the mixture in a roll-type granulator, extruding the mixture into cuboids with the same size, and crushing the cuboids into blocks by a crusher, wherein the extrusion pressure of the roll-type granulator is 8-12 MPa; screening the block-shaped body by a rolling sieve to obtain a finished spodumene particle product with the particle size of 2-3 mm.
Example 2: preparation of particulate spodumene
The method comprises the following steps: (1) drying the fine spodumene powder in a paddle dryer until the water content is 1% -3%;
(2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag, a sodium silicate solution and water, the mass of the calcium slag is 6% of that of the fine-powder spodumene, the mass of the sodium silicate solution is 3% of that of the fine-powder spodumene, and the mass of the water is 3% of that of the fine-powder spodumene;
(3) granulating the mixture in a roll-type granulator, extruding the mixture into cuboids with the same size, and crushing the cuboids into blocks by a crusher, wherein the extrusion pressure of the roll-type granulator is 8-12 MPa; screening the block-shaped body by a rolling sieve to obtain a finished spodumene particle product with the particle size of 2-3 mm.
Example 3: preparation of particulate spodumene
The method comprises the following steps: (1) drying the fine spodumene powder in a paddle dryer until the water content is 1% -3%;
(2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag, a sodium silicate solution and water, the mass of the calcium slag is 5% of that of the fine-powder spodumene, the mass of the sodium silicate solution is 2% of that of the fine-powder spodumene, and the mass of the water is 2% of that of the fine-powder spodumene;
(3) granulating the mixture in a roll-type granulator, extruding the mixture into cuboids with the same size, and crushing the cuboids into blocks by a crusher, wherein the extrusion pressure of the roll-type granulator is 8-12 MPa; screening the block-shaped body by a rolling sieve to obtain a finished spodumene particle product with the particle size of 2-3 mm.
Comparative example 1: preparation of particulate spodumene
The method comprises the following steps: (1) drying the fine spodumene powder in a paddle dryer until the water content is 1% -3%;
(2) adding a binding agent into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binding agent is prepared by mixing a sodium silicate solution and water, the sodium silicate solution accounts for 2% of the mass of the fine-powder spodumene, and the water accounts for 2% of the mass of the fine-powder spodumene;
(3) granulating the mixture in a roll-type granulator, extruding the mixture into cuboids with the same size, and crushing the cuboids into blocks by a crusher, wherein the extrusion pressure of the roll-type granulator is 8-12 MPa; screening the block-shaped body by a rolling sieve to obtain a finished spodumene particle product with the particle size of 2-3 mm.
Comparative example 1 compared to example 3, no calcium slag was added.
Comparative example 2: preparation of particulate spodumene
The method comprises the following steps: (1) drying the fine spodumene powder in a paddle dryer until the water content is 1% -3%;
(2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag and water, the calcium slag accounts for 5% of the mass of the fine-powder spodumene, and the water accounts for 2% of the mass of the fine-powder spodumene;
(3) granulating the mixture in a roll-type granulator, extruding the mixture into cuboids with the same size, and crushing the cuboids into blocks by a crusher, wherein the extrusion pressure of the roll-type granulator is 8-12 MPa; screening the block-shaped body by a rolling sieve to obtain a finished spodumene particle product with the particle size of 2-3 mm.
Comparative example 2 in comparison to example 3, no sodium silicate solution was added.
The granular spodumene prepared in examples 1 to 3 of the present invention and comparative examples 1 to 2 and the raw material fine powder spodumene were respectively calcined at 1000 ℃ for 15min to convert α lithium into β lithium, and then the crystal form conversion rate was measured by an atomic absorption analyzer, and the measurement results of the crystal form conversion rate are shown in table 1:
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Fine powder spodumene | |
| Conversion of Crystal form (%) | 93.6 | 93.2 | 94.8 | 88.7 | 88.9 | 84.2 |
As can be seen from the above table, the crystal form conversion rate of the examples 1-3 of the invention is obviously higher than that of the comparative examples 1-2, fine powder spodumene, wherein the crystal form conversion rate of the example 3 is the highest; the lower crystal transformation ratios of comparative examples 1 and 2 than examples 1-3 indicate that removing either the calcium slag or the sodium silicate solution from the binder affects the crystal transformation ratio of the particulate spodumene.
The particulate spodumene obtained in example 3 was subjected to battery-grade lithium salt preparation by the existing sulfuric acid method, and subjected to roasting, acidification, purification, concentration and evaporation, lithium precipitation and other steps to obtain a battery-grade lithium salt, and the components in the battery-grade lithium salt were compared with the national standard, and the results are shown in table 2:
TABLE 2
As can be seen from the above table, Li2CO3The content of the lithium salt is higher than the national standard, and the content of other impurity components is lower than the national standard, so the battery-grade lithium salt prepared from the granular spodumene prepared by the method meets the national standard, and the lithium salt yield is high.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (9)
1. A method for preparing granular spodumene by utilizing fine powder spodumene granulation is characterized by comprising the following steps:
(1) drying the fine spodumene powder until the water content is 1% -3%;
(2) adding a binder into the dried fine-powder spodumene, and uniformly mixing to obtain a mixture, wherein the binder is prepared by mixing calcium slag, a sodium silicate solution and water, the mass of the calcium slag is 4% -6% of that of the fine-powder spodumene, the mass of the sodium silicate solution is 1% -3% of that of the fine-powder spodumene, and the mass of the water is 1% -3% of that of the fine-powder spodumene;
(3) and granulating and screening the mixture to obtain a finished product of the granular spodumene.
2. The method of claim 1, wherein: in the step (1), the fine spodumene powder is dried in a paddle dryer.
3. The method of claim 1, wherein: in the step (1), the fine-powder spodumene with a 200-mesh screen underflow of more than or equal to 65% is adopted as the fine-powder spodumene.
4. The method of claim 1, wherein: in the step (2), the calcium slag is generated after purification and concentration processes in the lithium salt preparation process.
5. The method of claim 1, wherein: in the step (3), extrusion granulation is adopted for granulation.
6. The method of claim 5, wherein: the extrusion type granulation adopts a roll extrusion type granulator to extrude the mixture into cuboids with the same size, and the cuboids are crushed into blocks by a crusher, wherein the extrusion pressure of the roll extrusion type granulator is 8-12 MPa.
7. The method of claim 6, wherein: and in the screening step, the block-shaped bodies are screened by a rolling screen, wherein the grain diameter of qualified products is 2-3mm, and unqualified products are returned to a granulator for continuous extrusion granulation.
8. A particulate spodumene prepared by the process of any one of claims 1 to 7.
9. Use of the particulate spodumene of claim 8 in the preparation of a battery grade lithium salt.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114477241A (en) * | 2022-01-14 | 2022-05-13 | 广东省科学院资源利用与稀土开发研究所 | Method for extracting lithium from spodumene |
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Cited By (1)
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| CN114477241A (en) * | 2022-01-14 | 2022-05-13 | 广东省科学院资源利用与稀土开发研究所 | Method for extracting lithium from spodumene |
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