CN115432721A - Process for preparing lithium hydroxide - Google Patents
Process for preparing lithium hydroxide Download PDFInfo
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- CN115432721A CN115432721A CN202210800305.5A CN202210800305A CN115432721A CN 115432721 A CN115432721 A CN 115432721A CN 202210800305 A CN202210800305 A CN 202210800305A CN 115432721 A CN115432721 A CN 115432721A
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- lithium hydroxide
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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
- C01D15/02—Oxides; Hydroxides
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- 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
Abstract
The invention discloses a process for preparing lithium hydroxide, which comprises the following steps: calcining, acidifying, mixing, leaching and removing impurities from the spodumene to obtain a lithium sulfate solution; refining the lithium sulfate solution; causticizing by mixed alkali; freezing and crystallizing; primary evaporation and concentration; evaporating and concentrating for the second time, and drying in vacuum. The negative pressure evaporation of the invention avoids the contact between the lithium hydroxide and the air, and simultaneously, the vacuum negative pressure drying process is adopted, because the boiling point of the water under the negative pressure condition is lower, the drying effect of the vacuum dryer under the same drying temperature is better, and the CO in the lithium hydroxide is better 3 2‑ And lower.
Description
Technical Field
The invention relates to the technical field of lithium hydroxide production, in particular to a process for preparing lithium hydroxide.
Background
Lithium hydroxide has wide application in the fields of new energy and new materials, such as battery industry, aluminum industry, lubricating grease, medicine, refrigerant, nuclear industry, photoelectric industry and the like. The industrial-grade lithium hydroxide is mainly used for lithium-based lubricating grease, and the battery-grade lithium hydroxide monohydrate is mainly used in high and new technical fields such as new energy and new materials. The market development of industrial-grade lithium hydroxide is mature, and the demand for acceleration is stable; the high rate of growth in demand for lithium hydroxide relies entirely on the pulling of high nickel ternary materials.
At present, the mainstream production process of the lithium hydroxide monohydrate in China is a lithium sulfate causticization method, sodium hydroxide with the corresponding theoretical quantity is added according to the lithium content in a lithium sulfate solution, sodium sulfate decahydrate is frozen out, the freezing solution is subjected to impurity removal and evaporation to prepare industrial lithium hydroxide monohydrate, and the industrial lithium hydroxide monohydrate is redissolved and evaporated to obtain the battery-grade lithium hydroxide monohydrate.
In recent years, the emphasis of lithium hydroxide research has been on how to further reduce the impurity content and obtain lithium hydroxide with high purity and uniform particles. Lithium hydroxide is one of raw materials of high-nickel ternary materials, the requirement on the quality of the lithium hydroxide is high, and even part of material factories begin to require a lithium salt factory to supply anhydrous micro-powder lithium hydroxide without crystal water (so as to avoid the quality problem caused by dehydration in the process of mixed sintering). The lithium hydroxide can be further processed according to the customization requirements of material factories, and higher requirements are provided for the process technology and production experience of lithium salt factories. The anhydrous lithium hydroxide applied to the cathode material is more easily polluted by carbon dioxide, and the carbonate content is not more than 0.5%. Therefore, in the production of lithium hydroxide, strict process control is required to avoid carbonate content exceeding the standard.
In the published document CN _112811447 a-a method for preparing battery-grade lithium hydroxide monohydrate, the process flow is complicated, and calcium removal is performed by using sodium oxalate, including subsequent impurity removal by using citric acid or EDTA as an additive, which may cause accumulation of organic matters in a production system, and is not environment-friendly and easily causes pollution.
In another published document CN _106629787 \ "b-battery-grade lithium hydroxide preparation method, the lithium hydroxide freezing solution is evaporated and concentrated, the lithium hydroxide is obtained by solid-liquid separation, and the crude lithium hydroxide is leached, which increases the risk of contacting the lithium hydroxide with carbon dioxide in the air, and changes the CO in the lithium hydroxide 3 2- Content, causing instability of the results.
Disclosure of Invention
In order to solve the problems, the invention discloses a process for preparing lithium hydroxide, which can effectively reduce CO in the lithium hydroxide 3 2- The content of the lithium hydroxide is reduced, so that the lithium hydroxide is prevented from reacting with carbon dioxide in the air to generate lithium carbonate, the side reaction is reduced, and the performance of the ternary material is improved.
The technical scheme of the invention is as follows: a process for preparing lithium hydroxide comprising the steps of:
s1: calcining, acidifying, mixing, leaching and removing impurities from the spodumene to obtain a lithium sulfate solution;
s2: and (3) refining the lithium sulfate solution: adjusting the pH value of the lithium sulfate solution to 11-12, filtering, removing COD from the filtrate, and then removing impurities such as Ca, mg and B to obtain a lithium sulfate refined solution;
s3: causticizing with mixed alkali: adding solid sodium hydroxide into the lithium sulfate refined solution obtained in the step S2, and mixing and stirring to obtain mixed alkali liquor;
s4: freezing and crystallizing: freezing the mixed alkali liquor obtained in the step S3 to-15-0 ℃, and then performing centrifugal separation to obtain a freezing liquid and sodium sulfate decahydrate solid;
s5: primary evaporation and concentration: performing primary negative pressure evaporation concentration on the centrifugal refrigerating fluid obtained in the step S4, performing centrifugal separation on the concentrated solution to obtain a crude product of lithium hydroxide, and performing evaporation concentration to obtain negative pressure evaporation with the vacuum degree of minus 0.06MPa to minus 0.04 MPa;
s6: secondary evaporation concentration and vacuum drying: dissolving the crude lithium hydroxide with pure water, introducing the dissolved solution into a secondary evaporation crystallization system, performing centrifugal separation on the separated crystal slurry to obtain battery-grade lithium hydroxide monohydrate, performing vacuum high-temperature drying to obtain anhydrous lithium hydroxide, and performing evaporation concentration to obtain negative pressure evaporation with the vacuum degree ranging from-0.06 MPa to-0.04 MPa.
Further, in the step S1, the concentration of lithium sulfate is 35 to 45g/L.
Further, in step S2, ca is less than 5ppm, mg is less than 5ppm, and B is less than 5ppm in the refined lithium sulfate solution.
Further, in step S3, naOH and Li in the lithium sulfate refining solution are added 2 The molar ratio of O is controlled to be 2.2.
Further, in step S4, the freezing process is one of continuous freezing, secondary freezing or secondary continuous freezing, the crystallization temperature is controlled to be-15-0 ℃, and SO in the freezing liquid 4 2- ＜30g/L of Li in sodium sulfate decahydrate 2 O＜0.5%。
Further, in step S6, the vacuum drying temperature is controlled to be 160-190 ℃, the drying time is 1-4h, and the evaporation and drying process is beneficial to controlling CO 3 2- Said battery grade lithium hydroxide monohydrate CO 3 2- Less than 0.35%, the water content of anhydrous lithium hydroxide is less than 1%, and CO 3 2- ＜0.5%。
A process for preparing lithium hydroxide can also be used to prepare anhydrous or monohydrate lithium hydroxide.
The invention has the advantages that: 1. the centrifugal refrigerating fluid is subjected to negative pressure evaporation concentration for one time, and the concentrated solution is subjected to centrifugal separation to obtain a crude lithium hydroxide product, so that the contact probability of the lithium hydroxide and carbon dioxide in the air can be effectively reduced, and the CO in the lithium hydroxide can be better controlled 3 2- The content of the lithium hydroxide prevents the lithium hydroxide from reacting with carbon dioxide in the air to generate lithium carbonate, reduces the occurrence of side reaction and improves the performance of the ternary material.
2. The negative pressure evaporation of the invention avoids the contact between the lithium hydroxide and the air, and simultaneously, the vacuum negative pressure drying process is adopted, because the boiling point of the water under the negative pressure condition is lower, the drying effect of the vacuum dryer under the same drying temperature is better, and the CO in the lithium hydroxide is better 3 2- And lower.
Detailed Description
For the purpose of promoting an understanding of the present invention, the following detailed description of the embodiments of the present invention is provided for the purpose of illustrating the invention and is not to be construed as limiting the scope of the present invention.
Example 1
A process for preparing lithium hydroxide comprises the following specific steps:
calcining, acidifying, mixing, leaching and removing impurities of the spodumene to obtain a lithium sulfate solution, wherein the existing process is still adopted, and the produced lithium sulfate solution is directly used for a new process; and (3) refining the lithium sulfate solution: harvesting Li at 2m 2 Adding 4.2kg NaOH into lithium sulfate solution with O content of 35g/L, adjusting pH to 11, adding 8.3kg sodium carbonate, stirring, heating to 70 deg.C, and passing throughFiltering, and removing COD, ca, mg and B from the filtrate to obtain the refined lithium sulfate solution. The content of Ca in the lithium sulfate refined solution was 3ppm, mg was 1ppm, and B was 3ppm; causticizing with mixed alkali: d, carrying out Li harvest on 1.9m obtained in the step S2 2 Feeding the lithium sulfate refined solution with the O content of 35g/L into a mixed alkali preparation tank, adding 212kg of solid sodium hydroxide, mixing and stirring to obtain mixed alkali solution; wherein, naOH and total Li in lithium sulfate refining solution are added 2 The molar ratio of O is controlled to be 2.4; freezing and crystallizing: performing continuous freezing crystallization and centrifugal separation on the mixed alkali liquor obtained in the step S3 twice, controlling the freezing crystallization temperature at-5 ℃ to obtain secondary centrifugal freezing liquid and sodium sulfate decahydrate solid; primary evaporation and concentration: carrying out primary evaporation concentration on the secondary centrifugal refrigerating fluid obtained in the step S4, wherein the evaporation concentration is negative pressure evaporation at the vacuum degree of-0.054 MPa, and the concentrated solution is subjected to centrifugal separation to obtain a crude product of lithium hydroxide; secondary evaporation concentration and vacuum drying: dissolving the crude lithium hydroxide with pure water, introducing the dissolved solution into a secondary evaporation crystallization system, evaporating and concentrating to evaporate at negative pressure of-0.054 MPa of vacuum degree, separating out crystal slurry, performing centrifugal separation to obtain battery-grade lithium hydroxide monohydrate, and performing vacuum drying at 160 ℃ for 1.5h to obtain anhydrous lithium hydroxide.
Example 2
A process for preparing lithium hydroxide comprises the following specific steps:
calcining, acidifying, mixing, leaching and removing impurities from the spodumene to obtain a lithium sulfate solution, wherein the existing process is still adopted, and the produced lithium sulfate solution is directly used for a new process; and (3) lithium sulfate solution refining: harvesting Li at 2m 2 Adding 4.5kg of NaOH into a lithium sulfate solution with the O content of 38g/L, adjusting the pH value to 12, adding 8.7kg of sodium carbonate, stirring, heating to 70 ℃, filtering, and removing COD, ca, mg and B from the filtrate to obtain a lithium sulfate refined solution; causticizing by using mixed alkali: li harvesting 2m from step S2 2 Feeding the lithium sulfate refined solution with the O content of 36g/L into a mixed alkali preparation tank, adding 230kg of solid sodium hydroxide, mixing and stirring to obtain mixed alkali liquor; wherein, naOH and total Li in lithium sulfate refining solution are added 2 The molar ratio of O is controlled to be 2.6; freezing and crystallizing: performing continuous freezing crystallization and centrifugal separation on the mixed alkali liquor obtained in the step S3 twice, controlling the freezing crystallization temperature to be-10 ℃, and obtaining secondary centrifugal freezing liquid and sodium sulfate decahydrate solid; concentration by one evaporationShrinking: carrying out primary evaporation concentration on the secondary centrifugal refrigerating fluid obtained in the step S4, wherein the evaporation concentration is negative pressure evaporation at the vacuum degree of-0.058 MPa, and the concentrated solution is subjected to centrifugal separation to obtain a crude product of lithium hydroxide; secondary evaporation concentration and vacuum drying: dissolving the crude lithium hydroxide with pure water, introducing the dissolved solution into a secondary evaporation crystallization system, evaporating and concentrating to evaporate at negative pressure of-0.058 MPa of vacuum degree, separating crystal slurry, performing centrifugal separation to obtain battery-grade lithium hydroxide monohydrate, and performing vacuum drying at 175 ℃ for 1.5h to obtain anhydrous lithium hydroxide.
Example 3
A process for preparing lithium hydroxide comprises the following specific steps:
calcining, acidifying, mixing, leaching and removing impurities from the spodumene to obtain a lithium sulfate solution, wherein the existing process is still adopted, and the produced lithium sulfate solution is directly used for a new process; and (3) lithium sulfate solution refining: harvesting Li at 2m 2 Adding 4.6kg of NaOH into a lithium sulfate solution with the O content of 42g/L, adjusting the pH value to 12, adding 8.4kg of sodium carbonate, stirring, heating to 70 ℃, filtering, and removing COD, ca, mg and B from the filtrate to obtain a lithium sulfate refined solution; causticizing with mixed alkali: d, carrying out Li harvest on 1.9m obtained in the step S2 2 Feeding the lithium sulfate refined solution with the O content of 41g/L into a mixed alkali preparation tank, adding 290kg of solid sodium hydroxide, mixing and stirring to obtain mixed alkali solution; wherein, naOH and total Li in lithium sulfate refining solution are added 2 The molar ratio of O is controlled to be 2.8; freezing and crystallizing: performing continuous freezing crystallization and centrifugal separation on the mixed alkali liquor obtained in the step S3 for two times, controlling the freezing crystallization temperature at-15 ℃, and obtaining secondary centrifugal freezing liquid and sodium sulfate decahydrate solid; primary evaporation and concentration: carrying out primary evaporation concentration on the secondary centrifugal refrigerating fluid obtained in the step S4, wherein the evaporation concentration is negative pressure evaporation at the vacuum degree of-0.06 MPa, and the concentrated solution is subjected to centrifugal separation to obtain a crude product of lithium hydroxide; secondary evaporation concentration and vacuum drying: dissolving crude lithium hydroxide with pure water, introducing the solution into a secondary evaporative crystallization system, evaporating and concentrating to evaporate at negative pressure of-0.06 MPa, separating out crystal slurry, centrifuging to obtain battery-grade lithium hydroxide monohydrate, and vacuum drying at 180 deg.C for 2 hr to obtain anhydrous lithium hydroxide
The lithium hydroxide obtained in examples 1 to 3 was sampled, analyzed and tested, and the sample components were as follows:
the results show that the lithium hydroxide obtained by the preparation method has high main content, uniform particle size distribution and good quality, and the method adopts negative pressure evaporation concentration and simultaneously uses a vacuum drying process to effectively control the content of impurities in the lithium hydroxide and improve the quality of the lithium hydroxide. The process optimization can cut off the carbonization phenomenon of the materials in the drying process from the source, and is beneficial to the control of the product quality.
Claims (6)
1. A process for preparing lithium hydroxide, comprising the steps of:
s1: calcining, acidifying, mixing, leaching and removing impurities from the spodumene to obtain a lithium sulfate solution;
s2: and (3) lithium sulfate solution refining: adjusting the pH value of the lithium sulfate solution to 11-12, filtering, removing COD from the filtrate, and removing impurities such as Ca, mg and B to obtain a lithium sulfate refined solution;
s3: causticizing by using mixed alkali: adding solid sodium hydroxide into the lithium sulfate refined solution obtained in the step S2, and mixing and stirring to obtain mixed alkali liquor;
s4: freezing and crystallizing: freezing the mixed alkali liquor obtained in the step S3 to-15-0 ℃, and then performing centrifugal separation to obtain a freezing liquid and sodium sulfate decahydrate solid;
s5: primary evaporation and concentration: performing primary negative pressure evaporation concentration on the centrifugal refrigerating fluid obtained in the step S4, performing centrifugal separation on the concentrated solution to obtain a crude product of lithium hydroxide, wherein the evaporation concentration is negative pressure evaporation with the vacuum degree of-0.06 MPa to-0.04 MPa;
s6: secondary evaporation concentration and vacuum drying: dissolving the crude lithium hydroxide with pure water, introducing the dissolved solution into a secondary evaporation crystallization system, centrifugally separating the precipitated crystal slurry to obtain battery-grade lithium hydroxide monohydrate, drying at high temperature in vacuum to obtain anhydrous lithium hydroxide, and concentrating the anhydrous lithium hydroxide into negative pressure evaporation with the vacuum degree of-0.06 MPa to-0.04 MPa.
2. The process of claim 1, wherein: in the step S1, the concentration of lithium sulfate is 35 to 45g/L.
3. The process of claim 1, wherein: in the step S2, ca in the lithium sulfate refined solution is less than 5ppm, mg is less than 5ppm, and B is less than 5ppm.
4. The process of claim 1, wherein: in the step S3, naOH and Li in the lithium sulfate refining solution are added 2 The molar ratio of O is controlled to be 2.2.
5. The process of claim 1, wherein: in the step S4, the freezing process is one of continuous freezing, secondary freezing or secondary continuous freezing, the crystallization temperature is controlled to be-15-0 ℃, and SO in freezing liquid is 4 2- Less than 30g/L of Li in sodium sulfate decahydrate 2 O＜0.5%。
6. A process for preparing lithium hydroxide according to claim 1, wherein: in the step S6, the vacuum drying temperature is controlled to be 160-190 ℃, the drying time is 1-4h, and the evaporation and drying process is beneficial to controlling CO 3 2- Said battery grade lithium hydroxide monohydrate CO 3 2- Less than 0.35%, the water content of anhydrous lithium hydroxide is less than 1%, and CO 3 2- ＜0.5%。
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