CN112939035A - Preparation method of lithium hydroxide monohydrate - Google Patents
Preparation method of lithium hydroxide monohydrate Download PDFInfo
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- CN112939035A CN112939035A CN202110371774.5A CN202110371774A CN112939035A CN 112939035 A CN112939035 A CN 112939035A CN 202110371774 A CN202110371774 A CN 202110371774A CN 112939035 A CN112939035 A CN 112939035A
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- lithium hydroxide
- hydroxide monohydrate
- mvr evaporator
- lithium
- stirring
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- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 title claims abstract description 33
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 title claims abstract description 33
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 132
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000001556 precipitation Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 9
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000001376 precipitating effect Effects 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000001704 evaporation Methods 0.000 claims description 24
- 230000008020 evaporation Effects 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000010413 mother solution Substances 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 8
- 230000008025 crystallization Effects 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000009993 causticizing Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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 provides a preparation method of lithium hydroxide monohydrate, which comprises the following steps: s1, adding calcium hydroxide and crude lithium carbonate into a size mixing tank, adding water, and uniformly stirring; s2, heating and stirring, and reacting at constant temperature; s3, naturally cooling in a precipitation tank, precipitating, and filtering to obtain a lithium hydroxide primary solution; s4, removing impurities from the lithium hydroxide primary liquid through a precision filter; s5, concentrating by an MVR evaporator 1 to enable the concentration of lithium hydroxide to reach 70-80 g/L; s6, passing through a precision filter and an iron remover, entering an MVR evaporator 2, and concentrating until the solid content of lithium hydroxide is 30-40%; s7, cooling, crystallizing and separating; and S8, drying to obtain the battery-grade lithium hydroxide monohydrate. The preparation method of the lithium hydroxide monohydrate can obtain the battery-grade lithium hydroxide monohydrate through one-time crystallization, has the industrial production energy consumption which is greatly lower than that of other existing preparation methods, and has great economic benefits.
Description
Technical Field
The invention relates to the field of new energy materials, in particular to a preparation method of lithium hydroxide monohydrate.
Background
Today, with rapid development of science and technology, countries in the world face the problems of resource scarcity, energy shortage, environmental pollution and the like which threaten the sustainable and healthy development of human civilization. In the face of increasingly worsened environments, the use of petroleum-based energy sources is greatly reduced, and the development of novel renewable energy sources has become common human consensus. Because the lithium battery has the characteristics of higher energy ratio, lower self-discharge rate, stronger high and low temperature adaptability, longer cycle life and the like, the lithium battery becomes an energy storage battery with the greatest development prospect at present. Lithium hydroxide is widely used in lithium batteries as one of important lithium salts. Under the new trend of advocating green and environmental protection, solving the energy crisis and improving the resource utilization rate, the method has important value on the research of the extraction and processing technology of the lithium resource.
Lithium hydroxide is widely used in lithium grease, an electrolyte for an alkaline storage battery, and the like. With the requirements of new energy automobiles on endurance, power and the like, higher requirements are put forward on the energy density, the charge and discharge performance and the like of the lithium ion battery. High energy density materials such as NCM811, NCM622, and NCA are becoming the mainstream of battery positive electrode materials in the future. At present, lithium hydroxide is mainly used as a lithium source for synthesizing ternary positive electrodes NCM811, NCM622, NCA and partial lithium iron phosphate (LFP) products, and with the rapid development of new energy industries, the gap of the demand of battery-grade lithium hydroxide is further expanded.
The current processes for preparing lithium hydroxide mainly comprise a lithium carbonate causticization method, an ionic membrane electrolysis method, an aluminate precipitation method, a calcination method and the like. Among them, the causticizing method of lithium carbonate is the main method for producing lithium hydroxide at present. The lithium carbonate causticization method is to prepare lithium hydroxide by using lime milk and lithium carbonate, specifically to obtain a lithium hydroxide solution by using the difference of the solubility of the lithium hydroxide and the solubility of the calcium carbonate, and then prepare the lithium hydroxide by a crystallization mode; but because the preparation process needs to be performed with multiple times of crystallization, resource waste and cost increase are caused.
How to process the battery-grade lithium hydroxide monohydrate by a simple process and reduce the production energy consumption thereof is a technical problem to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a preparation method of lithium hydroxide monohydrate, which has simple process and low energy consumption.
The invention aims to realize the technical scheme that the preparation method of the lithium hydroxide monohydrate comprises the following steps:
s1, adding calcium hydroxide and crude lithium carbonate into a size mixing tank, adding water, and uniformly stirring;
s2, transferring the uniform mixture obtained in the step S1 into a reaction kettle, heating and stirring, and reacting for 1 hour at constant temperature after the temperature reaches 100 ℃;
s3, transferring the reaction product obtained in the step S2 to a precipitation tank, naturally cooling in the precipitation tank, precipitating for 2 hours, and filtering to obtain a lithium hydroxide primary solution;
s4, further removing impurities from the lithium hydroxide primary liquid obtained in the step S3 through a precision filter;
s5, concentrating the liquid with the impurities removed in the step S4 by an MVR evaporator 1 to ensure that the concentration of lithium hydroxide reaches 70-80 g/L;
s6, the solution obtained in the step S5 enters an MVR evaporator 2 after passing through a precision filter and an iron remover, and is concentrated until the solid content of lithium hydroxide is 30-40%;
s7, cooling, crystallizing and separating the solution obtained in the step S6, leaching the solution by using steam condensate water from an MVR evaporator to obtain a lithium hydroxide monohydrate wet product and a mother solution, and returning the mother solution to S5 for circulation;
s8, drying the isolate obtained in the step S7 at-0.07 to-0.08 MPa at 50 to 60 ℃ for 2 to 3 hours to obtain the battery-grade lithium hydroxide monohydrate.
Further, the molar ratio of the calcium hydroxide to the lithium carbonate in the step S1 is 1.2: 1, the water addition amount is that the concentration of the lithium hydroxide after the reaction is 18-22 g/L.
Further, the stirring parameter in the step S1 is 100-120 rpm, and the time is 5-10 min.
Further, in the step S5, the pressure of the MVR evaporator 1 is-0.040 to-0.050 MPa, the evaporation temperature is 80 to 90 ℃, and the evaporation time is 2 to 4 hours.
Further, in the step S6, the pressure of the MVR evaporator 2 is-0.040 to-0.050 MPa, the evaporation temperature is 80 to 90 ℃, and the evaporation time is 1 to 2 hours.
Further, the crystal is cooled and crystallized in the step S7, the stirring speed is 40-80 r/min, the stirring time is 1h, the cooling temperature is 40-50 ℃, and then centrifugal separation is carried out.
The preparation method of the lithium hydroxide monohydrate can obtain the battery-grade lithium hydroxide monohydrate through one-time crystallization, has the industrial production energy consumption which is greatly lower than that of other existing preparation methods, and has great economic benefits.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of lithium hydroxide monohydrate comprises the following steps:
s1, putting a primary product of 120kg of calcium hydroxide and 100kg of lithium carbonate into a stirring cylinder, adding water to ensure that the concentration of the reacted lithium hydroxide is 18g/L, and uniformly stirring at the stirring speed of 100 revolutions per minute for 5 min;
s2, transferring the uniform mixture obtained in the step S1 into a reaction kettle, and preserving heat for 1h at 100 ℃ for reaction;
s3, transferring the reaction product obtained in the step S2 to a precipitation tank, naturally cooling in the precipitation tank, precipitating for 2 hours, and filtering to obtain a lithium hydroxide primary solution;
s4, further removing impurities from the lithium hydroxide primary liquid obtained in the step S3 through a precision filter;
s5, passing the liquid with the impurities removed in the step S4 through an MVR evaporator 1 to enable the concentration of lithium hydroxide to reach 70 g/L; the pressure of the MVR evaporator 1 is-0.04 MPa, the evaporation temperature is 80 ℃, and the evaporation time is 4 h;
s6, filtering the solution obtained in the step S5, and enabling the filtrate to pass through an MVR evaporator 2 to enable the solid content of lithium hydroxide to be 30%; the pressure of the MVR evaporator 2 is-0.04 MPa, the evaporation temperature is 80 ℃, and the evaporation time is 2 h;
s7, carrying out crystallization separation on the solution obtained in the step S6; stirring at 40 rpm for 1 hr at 40 deg.C, and centrifuging;
s8, drying the isolate obtained in the step S7 at-0.07 MPa and 50 ℃ for 3h to obtain 56.84kg of battery-grade lithium hydroxide monohydrate.
Example 2
A preparation method of lithium hydroxide monohydrate comprises the following steps:
s1, putting a primary product of 120kg of calcium hydroxide and 100kg of lithium carbonate into a stirring cylinder, adding water to ensure that the concentration of the reacted lithium hydroxide is 20g/L, and uniformly stirring at the stirring speed of 120 revolutions per minute for 8 minutes;
s2, transferring the uniform mixture obtained in the step S1 into a reaction kettle, and preserving heat for 1h at 100 ℃ for reaction;
s3, transferring the reaction product obtained in the step S2 to a precipitation tank, naturally cooling in the precipitation tank, precipitating for 2 hours, and filtering to obtain a lithium hydroxide primary solution;
s4, further removing impurities from the lithium hydroxide primary liquid obtained in the step S3 through a precision filter;
s5, passing the liquid with the impurities removed in the step S4 through an MVR evaporator 1 to enable the concentration of lithium hydroxide to reach 75 g/L; the pressure of the MVR evaporator 1 is-0.05 MPa, the evaporation temperature is 90 ℃, and the evaporation time is 2 h;
s6, filtering and removing iron from the solution obtained in the step S5, and enabling the filtrate to pass through an MVR evaporator 2 to enable the solid content of lithium hydroxide to be 40%; the pressure of the MVR evaporator 2 is-0.04 MPa, the evaporation temperature is 90 ℃, and the evaporation time is 1 h;
s7, carrying out crystallization separation on the solution obtained in the step S6; stirring at 80 r/min for 1 hr at 50 deg.c, and centrifuging;
s8, drying the isolate obtained in the step S7 at-0.08 MPa and 60 ℃ for 2h to obtain 64.25kg of battery-grade lithium hydroxide monohydrate.
Example 3
A preparation method of lithium hydroxide monohydrate comprises the following steps:
s1, putting a primary product of 120kg of calcium hydroxide and 100kg of lithium carbonate into a stirring cylinder, adding water to ensure that the concentration of the reacted lithium hydroxide is 19g/L, and uniformly stirring at the stirring speed of 110 revolutions per minute for 10 min;
s2, transferring the uniform mixture obtained in the step S1 into a reaction kettle, and preserving heat for 1h at 100 ℃ for reaction;
s3, transferring the reaction product obtained in the step S2 to a precipitation tank, naturally cooling in the precipitation tank, precipitating for 2 hours, and filtering to obtain a lithium hydroxide primary solution;
s4, further removing impurities from the lithium hydroxide primary liquid obtained in the step S3 through a precision filter;
s5, passing the liquid with the impurities removed in the step S4 through an MVR evaporator 1 to enable the concentration of lithium hydroxide to reach 80 g/L; the pressure of the MVR evaporator 1 is-0.04 MPa, the evaporation temperature is 85 ℃, and the evaporation time is 3 h;
s6, filtering the solution obtained in the step S5, and enabling the filtrate to pass through an MVR evaporator 2 to enable the solid content of lithium hydroxide to be 35%; the pressure of the MVR evaporator 2 is-0.05 MPa, the evaporation temperature is 85 ℃, and the evaporation time is 1.5 h;
s7, carrying out crystallization separation on the solution obtained in the step S6; stirring at 60 r/min for 1 hr at 45 deg.c, and centrifuging;
s8, drying the isolate obtained in the step S7 at-0.07 MPa and 55 ℃ for 2.5h to obtain 60.27kg of battery-grade lithium hydroxide monohydrate.
Example 4
A preparation method of lithium hydroxide monohydrate comprises the following steps:
s1, putting a primary product of 120kg of calcium hydroxide and 100kg of lithium carbonate into a stirring cylinder, adding water to ensure that the concentration of the reacted lithium hydroxide is 18.5g/L, and uniformly stirring at the stirring speed of 100 revolutions per minute for 6 min;
s2, transferring the uniform mixture obtained in the step S1 into a reaction kettle, and preserving heat for 1h at 100 ℃ for reaction;
s3, transferring the reaction product obtained in the step S2 to a precipitation tank, naturally cooling in the precipitation tank, precipitating for 2 hours, and filtering to obtain a lithium hydroxide primary solution;
s4, further removing impurities from the lithium hydroxide primary liquid obtained in the step S3 through a precision filter;
s5, passing the liquid with the impurities removed in the step S4 through an MVR evaporator 1 to enable the concentration of lithium hydroxide to reach 72 g/L; the pressure of the MVR evaporator 1 is-0.048 MPa, the evaporation temperature is 85 ℃, and the evaporation time is 3 h;
s6, filtering the solution obtained in the step S5, and enabling the filtrate to pass through an MVR evaporator 2 to enable the solid content of lithium hydroxide to be 38%; the pressure of the MVR evaporator 2 is-0.049 MPa, the evaporation temperature is 82 ℃, and the evaporation time is 1.5 h;
s7, carrying out crystallization separation on the solution obtained in the step S6; stirring at 70 r/min for 1 hr at 45 deg.c, and centrifuging;
s8, drying the isolate obtained in the step S7 at-0.08 MPa and 50 ℃ for 2.5h to obtain 62.4kg of battery-grade lithium hydroxide monohydrate.
The lithium hydroxide monohydrate prepared by the method is detected, and the detection result is as follows:
therefore, the performance index of the lithium hydroxide monohydrate prepared by the method meets the standard of battery-grade lithium hydroxide monohydrate.
The large production data prove that the energy consumption for preparing the lithium hydroxide monohydrate is as follows:
therefore, the preparation method of the invention has the advantages of short production time, low energy consumption, great superiority to other preparation methods and great economic benefit.
It should be understood that the examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that any changes and modifications to the present invention may occur to those skilled in the art after reading the present teachings, and such equivalents are also intended to be limited by the appended claims.
Claims (6)
1. A preparation method of lithium hydroxide monohydrate is characterized by comprising the following steps:
s1, adding calcium hydroxide and crude lithium carbonate into a size mixing tank, adding water, and uniformly stirring;
s2, transferring the uniform mixture obtained in the step S1 into a reaction kettle, heating and stirring, and reacting for 1 hour at constant temperature after the temperature reaches 100 ℃;
s3, transferring the reaction product obtained in the step S2 to a precipitation tank, naturally cooling in the precipitation tank, precipitating for 2 hours, and filtering to obtain a lithium hydroxide primary solution;
s4, further removing impurities from the lithium hydroxide primary liquid obtained in the step S3 through a precision filter;
s5, concentrating the liquid with the impurities removed in the step S4 by an MVR evaporator 1 to ensure that the concentration of lithium hydroxide reaches 70-80 g/L;
s6, the solution obtained in the step S5 enters an MVR evaporator 2 after passing through a precision filter and an iron remover, and is concentrated until the solid content of lithium hydroxide is 30-40%;
s7, cooling, crystallizing and separating the solution obtained in the step S6, leaching the solution by using steam condensate water from an MVR evaporator to obtain a lithium hydroxide monohydrate wet product and a mother solution, and returning the mother solution to S5 for circulation;
s8, drying the isolate obtained in the step S7 at-0.07 to-0.08 MPa at 50 to 60 ℃ for 2 to 3 hours to obtain the battery-grade lithium hydroxide monohydrate.
2. The method for preparing lithium hydroxide monohydrate according to claim 1, wherein the molar ratio of calcium hydroxide to lithium carbonate in step S1 is 1.2: 1, the water addition amount is that the concentration of the lithium hydroxide after the reaction is 18-22 g/L.
3. The method as claimed in claim 1, wherein the stirring parameter in step S1 is 100-120 rpm, and the time is 5-10 min.
4. The method for preparing lithium hydroxide monohydrate according to claim 1, wherein the pressure of the MVR evaporator 1 in the step S5 is-0.040-0.050 MPa, the evaporation temperature is 80-90 ℃, and the evaporation time is 2-4 h.
5. The method for preparing lithium hydroxide monohydrate according to claim 1, wherein in step S6, the pressure of the MVR evaporator 2 is-0.040 to-0.050 MPa, the evaporation temperature is 80 to 90 ℃, and the evaporation time is 1 to 2 hours.
6. The method for preparing lithium hydroxide monohydrate according to any one of claims 1 to 5, wherein the step S7 is performed by cooling and crystallizing at a stirring speed of 40 to 80 rpm for 1 hour at a cooling temperature of 40 to 50 ℃, and then performing centrifugal separation.
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| WO2024089394A1 (en) * | 2022-10-27 | 2024-05-02 | Research By British Lithium Ltd | Production of battery grade chemicals |
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