CN116514144A - Method for preparing battery-grade lithium fluoride from industrial-grade lithium carbonate - Google Patents
Method for preparing battery-grade lithium fluoride from industrial-grade lithium carbonate Download PDFInfo
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- CN116514144A CN116514144A CN202310568063.6A CN202310568063A CN116514144A CN 116514144 A CN116514144 A CN 116514144A CN 202310568063 A CN202310568063 A CN 202310568063A CN 116514144 A CN116514144 A CN 116514144A
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- grade lithium
- lithium fluoride
- lithium
- lithium carbonate
- fluoride
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- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 title claims abstract description 114
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 37
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 14
- 238000005342 ion exchange Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 9
- 150000001768 cations Chemical class 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000003957 anion exchange resin Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052744 lithium Inorganic materials 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- 229910052749 magnesium Inorganic materials 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000009466 transformation Effects 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
- C01D15/04—Halides
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium batteries, and particularly relates to a method for preparing battery-grade lithium fluoride from industrial-grade lithium carbonate. The invention takes industrial grade lithium carbonate with more impurities as raw material and reacts with hydrofluoric acid to prepare the battery grade lithium fluoride product. Compared with the prior art, the method has the advantages of short flow, easy operation, low energy consumption, low cost, high product purity (purity is less than 99.95 percent), stable quality and product yield of not less than 90 percent.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a method for preparing battery-grade lithium fluoride from industrial-grade lithium carbonate.
Background
At present, with increasing importance of ecological environment protection worldwide, the replacement of traditional fossil energy sources which bring about environmental pollution and greenhouse effect by utilizing new green energy sources such as solar energy, wind energy, electric energy and the like is an important means focused by the current energy source transformation. Electric energy is one of the most widely used green energy sources at present. Battery technology is the key to the efficient use of electrical energy that enters production and life. With the rapid development of battery technology, the green energy technology represented by lithium batteries is continuously changing the daily life of people, and the production of lithium hexafluorophosphate as electrolyte in lithium batteries is a bottleneck for limiting the industrial development of lithium battery technology.
The main raw material for producing the electrolyte lithium hexafluorophosphate is battery grade lithium fluoride (LiF content is more than or equal to 99.95%). Most of the research on lithium batteries is focused on the preparation of electrode materials and the research on battery systems, while the development of electrolyte material production technologies is relatively less, especially the production of battery grade lithium fluoride is currently carried out, and metal ions and impurities in the production process seriously affect the product quality of the battery grade lithium fluoride. In the direct synthesis method mentioned in the literature [ J ] inorganic salt industry, 2011,43 (5): 15 ], the requirement on the lithium carbonate raw material is high, the purity of the lithium carbonate must reach the electronic grade, and the cost is high. The direct synthesis, extraction and metathesis processes described in the literature of "Small Lin Jianer, tapu and Fu, gaozhi Lang. High degree of resolution metal fves, japan, hei Cheng 4-042602[ P.1992-02-13 ], all require subsequent purification of lithium fluoride. The preparation of high purity lithium fluoride [ J ]. Tianjin technology, 2012 (6): 3 by purification of industrial lithium carbonate is described in documents Yu Baoqing, zhao Qingyun, sun Xinhua, where treatment of lithium bicarbonate pretreatment solution with complexing agents is mentioned, in which method the impurity ions in the lithium bicarbonate pretreatment solution are treated by means of resin adsorption.
In addition, the demand for lithium batteries has shown a sharply increased development trend in recent years, and the capacity of the current battery-grade lithium fluoride production process cannot meet the market demand.
Disclosure of Invention
In order to solve the problems, the invention provides a process method for preparing battery grade lithium fluoride from industrial grade lithium carbonate.
The technical scheme of the invention is as follows:
a method for preparing high-purity lithium fluoride from industrial lithium carbonate comprises the following steps:
(1) Carbonization reaction: technical grade lithium carbonate (L)iCO 3 The content is more than or equal to 99.0 percent) and ultrapure water are added into a reaction kettle to form lithium carbonate suspension, carbon dioxide gas is introduced, and lithium bicarbonate clarified liquid is obtained after complete reaction;
(2) And (3) filtering: passing the clarified lithium bicarbonate solution obtained in the step (1) through a filter to obtain clarified lithium bicarbonate pretreatment solution, and returning the solid obtained by filtering to the step (1) for use as unreacted complete lithium carbonate;
(3) Ion exchange: introducing the lithium bicarbonate pretreatment solution obtained in the step (2) into an ion exchange system, and removing metal cations such as calcium, magnesium and the like in the lithium bicarbonate pretreatment solution to obtain a refined lithium bicarbonate solution;
(4) And (3) synthesis: introducing the refined lithium bicarbonate solution obtained in the step (3) into a synthesis reaction kettle, adding hydrofluoric acid for reaction, and obtaining a lithium fluoride suspension after the reaction is finished;
(5) And (3) filtering and washing: filtering the lithium fluoride suspension in the step (4), and washing with ultrapure water to obtain a battery-grade lithium fluoride wet material, wherein the filtrate is returned to the step (4) for synthesizing lithium fluoride;
(6) Drying and cooling: and (3) carrying out vacuum drying on the wet lithium fluoride material of the battery grade generated in the step (5), and obtaining the lithium fluoride of the battery grade after cooling.
Further, in the step (1), the mass fraction of lithium carbonate in the lithium carbonate suspension is 20-40%, and the carbon dioxide introducing speed is 5-20 m 3 And/h, the reaction temperature is 20-40 ℃, and the reaction time is 0.5-3.5 h.
In the step (2), the filter element is made of PP, PTFE, titanium or SUS316L, and the aperture is 0.2-15 mu m.
Further, in the step (3), the ion exchange system contains one or two of diatomite, weak alkaline anion exchange resin and weak acid cation exchange resin, and the space velocity of the material is 1.0-3.0 h -1 。
Further, in the step (4), the reaction temperature is 20-45 ℃ and the reaction time is 1-6 h.
Further, in the step (5), the pore diameter of the filter cloth used for filtration is 20 to 200 meshes, and the filter cloth is washed with ultrapure water at 60 to 80 ℃.
Further, in the step (6), vacuum drying is adopted, and the vacuum degree is-15 kPa to-110 kPa; the drying temperature is 150-220 ℃; the drying time is 2-10 h.
The invention has the beneficial effects that:
according to the technical scheme, the technical grade lithium carbonate with more impurities is used as a raw material, and the technical method is used for reacting with hydrofluoric acid to prepare the battery grade lithium fluoride product. The raw material adopted by the invention is industrial grade lithium carbonate, so that the production cost of battery grade lithium fluoride can be reduced; removing impurities by ion exchange on the lithium bicarbonate pretreatment solution to ensure the purity of the product; the existing direct synthesis method, extraction method and double decomposition preparation can not directly obtain high-purity lithium fluoride, and subsequent purification of the lithium fluoride is required. Compared with the prior art, the method has the advantages of short flow, easy operation, low energy consumption, low cost, high product purity (the purity is not less than 99.95 percent), stable quality and product yield of not less than 90 percent.
Drawings
FIG. 1 is a flow chart of the production process of the invention.
Detailed Description
The production process of the present invention is further illustrated by the following specific examples.
Example 1
1kg of technical grade lithium carbonate is added into a stirrer of 2.5kg of deionized water at normal temperature, and the stirring speed is 250r/min. Introducing carbon dioxide into the suspension for 5m 3 Introducing carbon dioxide for 60min, controlling the temperature at 30 ℃, reacting for 3.5h, gradually clarifying the suspension, introducing the solution into a micro-filter, selecting a 1 mu m PP filter core for the filter aperture, and removing undissolved lithium carbonate raw materials; the obtained filtrate is introduced into an ion exchange system, and the airspeed is 2h -1 Further removing cations such as calcium and magnesium in the solution to obtain a purer refined lithium bicarbonate solution, wherein the content of the cations such as calcium and magnesium after ion exchange is 0.1ppm; introducing the obtained refined lithium bicarbonate solution into a synthesis reaction kettle, adding 1.4kg of hydrofluoric acid with the mass fraction of 40% for reaction, and controlling the reaction temperatureReacting at 40 ℃ for 3 hours to obtain lithium fluoride suspension; filtering the lithium fluoride suspension, wherein the pore diameter of a filter cloth is 60 meshes, and washing the lithium fluoride suspension with ultrapure water at 80 ℃ for 3 times to obtain a battery-grade lithium fluoride wet material; and (3) carrying out vacuum drying on the battery grade lithium fluoride wet material under the vacuum degree of-110 kPa, and drying for 10 hours at 150 ℃, and cooling to obtain 653g of battery grade lithium fluoride, wherein the yield is 93.55%. Analyzed and detected, metal ion K, na, ca, fe<0.1ppm、Ni<0.05ppm。
Example 2
1kg of technical grade lithium carbonate is added into a stirrer of 3kg of deionized water at normal temperature, and the stirring speed is 250r/min. Introducing carbon dioxide into the suspension for 10m 3 Introducing carbon dioxide for 60min, controlling the temperature at 20 ℃, reacting for 0.5h, gradually clarifying the suspension, introducing the solution into a micro-filter, selecting a 15 mu m PTFE filter core for the filter aperture, and removing undissolved lithium carbonate raw materials; the obtained filtrate is introduced into an ion exchange system, and the airspeed is 1h -1 Further removing cations such as calcium and magnesium in the solution to obtain a purer refined lithium bicarbonate solution, wherein the content of the cations such as calcium and magnesium after ion exchange is 0.1ppm; introducing the obtained refined lithium bicarbonate solution into a synthesis reaction kettle, adding 1.12kg of hydrofluoric acid with the mass fraction of 50% for reaction, controlling the reaction temperature to be 45 ℃, and reacting for 1h to obtain a lithium fluoride suspension; filtering the lithium fluoride suspension, wherein the pore diameter of a filter cloth is 20 meshes, and washing the filter cloth with ultrapure water at 70 ℃ for 3 times to obtain a battery-grade lithium fluoride wet material; and (3) carrying out vacuum drying on the wet lithium fluoride material at the vacuum degree of-15 kPa, and drying for 2 hours at 220 ℃, and cooling to obtain 662g of the battery grade lithium fluoride, wherein the yield is 94.25%. Analyzed and detected, metal ion K, na, ca, fe<0.1ppm、Ni<0.05ppm。
Example 3
1kg of technical grade lithium carbonate is added into a stirrer of 5kg of deionized water at normal temperature, and the stirring speed is 250r/min. Introducing carbon dioxide into the suspension for 20m 3 Introducing carbon dioxide for 60min, controlling the temperature at 40deg.C, reacting for 3 hr, clarifying the suspension, introducing the solution into microfilter, and filtering with 0.2 μm pore diameterA titanium filter element for removing undissolved lithium carbonate raw material; the obtained filtrate is introduced into an ion exchange system, and the airspeed is 3.0h -1 Further removing cations such as calcium and magnesium in the solution to obtain a purer refined lithium bicarbonate solution, wherein the content of the cations such as calcium and magnesium after ion exchange is 0.1ppm; introducing the obtained refined lithium bicarbonate solution into a synthesis reaction kettle, adding 1.25kg of 45% hydrofluoric acid for reaction, controlling the reaction temperature to be 20 ℃, and reacting for 6 hours to obtain a lithium fluoride suspension; filtering the lithium fluoride suspension, wherein the aperture of a filter cloth is 200 meshes, and washing the lithium fluoride suspension with high-purity water at 60 ℃ for 3 times to obtain a battery-grade lithium fluoride wet material; and carrying out vacuum drying on the wet lithium fluoride material at the vacuum degree of-75 kPa for 6 hours at 180 ℃, and cooling to obtain 692g of lithium fluoride with the high yield of 99.42%. Analyzed and detected, metal ion K, na, ca, fe<0.1ppm、Ni<0.05ppm。
Claims (10)
1. A method for preparing battery grade lithium fluoride from industrial grade lithium carbonate, which is characterized by comprising the following steps:
(1) Carbonization reaction: adding industrial grade lithium carbonate and ultrapure water into a reaction kettle to form lithium carbonate suspension, introducing carbon dioxide gas, and obtaining lithium bicarbonate clear liquid after complete reaction;
(2) And (3) filtering: passing the clarified lithium bicarbonate solution obtained in the step (1) through a filter to obtain clarified lithium bicarbonate pretreatment solution, and returning the solid obtained by filtering to the step (1) for use as unreacted complete lithium carbonate;
(3) Ion exchange: introducing the lithium bicarbonate pretreatment solution obtained in the step (2) into an ion exchange system, and removing metal cations in the lithium bicarbonate pretreatment solution to obtain a refined lithium bicarbonate solution;
(4) And (3) synthesis: introducing the refined lithium bicarbonate solution obtained in the step (3) into a synthesis reaction kettle, adding hydrofluoric acid for reaction, and obtaining a lithium fluoride suspension after the reaction is finished;
(5) And (3) filtering and washing: filtering the lithium fluoride suspension in the step (4), and washing with ultrapure water to obtain a battery-grade lithium fluoride wet material, wherein the filtrate is returned to the step (4) for synthesizing lithium fluoride;
(6) Drying and cooling: and (3) carrying out vacuum drying on the wet lithium fluoride material of the battery grade generated in the step (5), and obtaining the lithium fluoride of the battery grade after cooling.
2. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 1, wherein in the step (1), the mass fraction of lithium carbonate in the lithium carbonate suspension is 20% -40%, and the carbon dioxide introducing speed is 5-20 m 3 And/h, the reaction temperature is 20-40 ℃, and the reaction time is 0.5-3.5 h.
3. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 1 or 2, wherein in the step (2), the filter element is made of PP, PTFE, titanium or SUS316L material, and the pore diameter is 0.2-15 μm.
4. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 1 or 2, wherein in the step (3), the ion exchange system contains one or two of diatomite, weak-base anion exchange resin and weak-acid cation exchange resin, and the space velocity of the material is 1.0-3.0 h -1 。
5. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 3, wherein in the step (3), the ion exchange system contains one or two of diatomite, weak alkaline anion exchange resin and weak acid cation exchange resin, and the space velocity of the material is 1.0-3.0 h -1 。
6. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 1, 2 or 5, wherein in the step (4), the reaction temperature is 20-45 ℃ and the reaction time is 1-6 h.
7. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 3, wherein in the step (4), the reaction temperature is 20-45 ℃ and the reaction time is 1-6 h.
8. The method for preparing battery grade lithium fluoride from industrial grade lithium carbonate according to claim 4, wherein in the step (4), the reaction temperature is 20-45 ℃ and the reaction time is 1-6 h.
9. The method for producing a battery grade lithium fluoride according to claim 1 or 2 or 5 or 7 or 8, wherein in the step (5), the filter cloth used for filtration has a pore size of 20 to 200 mesh and is washed with ultrapure water at 60 to 80 ℃.
10. The method for preparing the battery grade lithium fluoride by using the industrial grade lithium carbonate according to claim 1 or 2 or 5 or 7 or 8, wherein in the step (6), vacuum drying is adopted, and the vacuum degree is between-15 kPa and-110 kPa; the drying temperature is 150-220 ℃; the drying time is 2-10 h.
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