CN112299454A - Method for improving direct yield of battery-grade lithium carbonate prepared from brine - Google Patents
Method for improving direct yield of battery-grade lithium carbonate prepared from brine Download PDFInfo
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- CN112299454A CN112299454A CN202011262415.8A CN202011262415A CN112299454A CN 112299454 A CN112299454 A CN 112299454A CN 202011262415 A CN202011262415 A CN 202011262415A CN 112299454 A CN112299454 A CN 112299454A
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 48
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 48
- 239000012267 brine Substances 0.000 title claims abstract description 34
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 35
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 19
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 6
- 230000000996 additive effect Effects 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 58
- 238000000926 separation method Methods 0.000 claims description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000011777 magnesium Substances 0.000 claims description 11
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 238000004806 packaging method and process Methods 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 5
- 239000000920 calcium hydroxide Substances 0.000 claims description 5
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 5
- 239000002826 coolant Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 5
- 239000001095 magnesium carbonate Substances 0.000 claims description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000011085 pressure filtration Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000010438 granite Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052629 lepidolite Inorganic materials 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 229910052670 petalite Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
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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
- C01D15/08—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine, which specifically comprises the following steps: s1, preparation: preparing brine, a container, an additive and tools which need to be used, checking whether omission exists, and performing next operation after the checking is finished, wherein S2 and stirring treatment are as follows: adding brine and aluminum chloride into a container, uniformly stirring and mixing the mixture by a stirrer for 1-2 hours, and taking precipitate to obtain a first mixed solution. Compared with the prior art, the invention has the beneficial effects that: the invention greatly reduces the loss of lithium ions, reduces the extraction cost, has smaller equipment requirement and simpler and more convenient required equipment, greatly improves the convenience of operation, reduces the labor force, ensures that the direct lithium yield is more than 90 percent, greatly reduces the energy consumption due to lower operation cost, ensures that the purity of the prepared product is higher, and brings great convenience to users.
Description
Technical Field
The invention relates to the technical field of brine utilization, in particular to a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine.
Background
The salt lake usually refers to lake with lake water salt content more than 50 g.L < -1 >, the lake contains a large amount of Cl < - >, SO42 < - >, HCO3 < - >, CO32 < - >, Na < + >, K < + >, Mg < + > and Li < + > ions, the salt content exceeds 24.7 per thousand, and the salt lake is an important raw material for producing various industrial and agricultural products. As the amount of lithium used in conventional application fields is increasing, people are also continuously developing new application fields, and the demand for lithium resources is also increasing. Lithium has attracted attention in the 21 st century as a new energy and strategic resource. The lithium resource of the Chinese salt lake accounts for about 85 percent of the total industrial reserve of the lithium resource, the strong stipulation that the extraction of lithium from the salt lake brine becomes the main direction of research and production of lithium salt, lithium carbonate is a raw material for preparing various lithium compounds, is a product with the largest yield and the widest application in lithium salt products, is widely applied to the industries of chemical industry, metallurgy, ceramics, medicine, refrigeration and the like, can also be used for preparing a catalyst for chemical reaction, is called industrial monosodium glutamate, and lithium does not have a simple substance form in the natural world but mainly exists in granite pegmatite ore beds (spodumene, lepidolite, petalite and the like) and brine and seawater in a compound form. According to published reports, more than 60% of lithium resources are distributed in salt lake brine worldwide, sulfate salt lake brine, particularly magnesium sulfate subtype brine, is the most representative of all boron-containing and lithium-containing salt lakes, and the reserve of the contained lithium resources accounts for about 30% of the total reserve worldwide, but the direct yield of the existing method for preparing battery-grade lithium carbonate from brine is low, so that the loss of lithium is high, the extraction cost is high, and the practicability is greatly reduced.
Disclosure of Invention
The invention aims to provide a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine specifically comprises the following steps:
s1, preparation: preparing brine, a container, an additive and a tool which need to be used, checking whether omission exists or not, and performing the next operation after the inspection is finished;
s2, stirring treatment: adding brine and aluminum chloride into a container, uniformly stirring and mixing the mixture by a stirrer for 1-2 hours, and taking a precipitate to obtain a first mixed solution;
s3, primary magnesium removal: adding sodium carbonate into the obtained mixed solution, stirring the mixed solution by a stirrer for 5 to 10 minutes to obtain a second mixed solution after stirring, and continuously stirring the solution at the temperature of between 50 and 80 ℃ for reacting for 2 to 4 hours;
s4, first filtration and separation: so that the solution obtained in the step S3 is subjected to solid-liquid separation treatment to obtain filter cake magnesium carbonate;
s5, secondary magnesium removal: adding calcium hydroxide into the solution of S4, uniformly stirring and mixing the solution by a stirrer, and reacting the solution at the temperature of between 50 and 80 ℃ for 60 to 120 minutes, wherein the concentration of lithium ions in the solution is between 10 and 13 g/L;
s6, second filtering and separating: carrying out filter pressing separation on the obtained solution in the S5 so as to obtain a filter cake magnesium hydroxide;
s7, evaporation and concentration: evaporating and concentrating the solution obtained in the step S6 by 3-4 times, wherein the concentration of lithium ions after concentration can reach 40-50 g/L;
s8, re-reacting: introducing the solution obtained in the step S8 into a reaction kettle, slowly adding sodium carbonate at the temperature of 80-100 ℃, and stirring for reaction for 30 minutes;
s9, filter pressing separation: carrying out solid-liquid separation on the solution obtained in the step S8, washing the solution for 5-8 times by using deionized water, and fully drying the solution at the temperature of 150 ℃ and 190 ℃ for 20-40 minutes to obtain lithium carbonate with the lithium carbonate content of 88-93%;
s10, cooling: cooling the lithium carbonate obtained in the step S9, wherein a cooling medium is an aqueous solution;
s11, packaging: and packaging the lithium carbonate obtained in the step S10 so as to be convenient for transportation and storage at a later stage.
Preferably, the preparation is carried out in such a way that the articles and containers used are free of dust and are kept clean.
Preferably, the temperature of the lithium carbonate after cooling in S10 is controlled to be 20-45 ℃.
Preferably, the molar ratio of aluminum chloride to lithium in brine in S2 is 2-6: 1.
Preferably, the lithium carbonate should be stored in a dry position.
Compared with the prior art, the invention has the beneficial effects that: the invention greatly reduces the loss of lithium ions, reduces the extraction cost, has smaller equipment requirement and simpler and more convenient required equipment, greatly improves the convenience of operation, reduces the labor force, ensures that the direct lithium yield is more than 90 percent, greatly reduces the energy consumption due to lower operation cost, ensures that the purity of the prepared product is higher, and brings great convenience to users.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, the present invention provides a technical solution: a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine specifically comprises the following steps:
s1, preparation: preparing brine, a container, an additive and tools to be used, checking whether omission exists or not, performing the next operation after the inspection is finished, and ensuring that the used objects and the container do not have dust and are in a clean state during preparation.
S2, stirring treatment: adding brine and aluminum chloride into a container, uniformly stirring and mixing the mixture by a stirrer for 1 hour, and taking out a precipitate to obtain a first mixed solution, wherein the molar ratio of the aluminum chloride to the lithium in the brine is 2:1 in S2.
S3, primary magnesium removal: adding sodium carbonate into the obtained mixed solution, stirring the mixed solution by a stirrer for 5 minutes to obtain a second mixed solution after the stirring is finished, and then continuously stirring the solution at 50 ℃ for reacting for 2 hours.
S4, first filtration and separation: thereby subjecting the solution obtained in S3 to solid-liquid separation treatment to obtain cake magnesium carbonate.
S5, secondary magnesium removal: calcium hydroxide was added to the solution of S4, followed by uniform stirring and mixing treatment with a stirrer, and reaction was carried out at 50 ℃ for 60 minutes, the lithium ion concentration in the solution being 10 g/L.
S6, second filtering and separating: the solution obtained in the step S5 is subjected to pressure filtration separation, so that a filter cake of magnesium hydroxide is obtained.
S7, evaporation and concentration: and (4) evaporating and concentrating the solution obtained in the step (S6) by 3 times, wherein the concentration of lithium ions after concentration can reach 40 g/L.
S8, re-reacting: the solution obtained in S8 was introduced into a reaction kettle, sodium carbonate was slowly added at 80 ℃, and the reaction time was 30 minutes with stirring.
S9, filter pressing separation: and (3) performing solid-liquid separation on the solution obtained in the step (S8), washing the solution with deionized water for 5 times, and fully drying the solution at the temperature of 150 ℃ for 20 minutes to obtain lithium carbonate with the lithium carbonate content of 88%.
S10, cooling: and (4) cooling the lithium carbonate obtained in the step S9, wherein the cooling medium is an aqueous solution, and the temperature of the lithium carbonate after cooling in the step S10 is controlled at 20 ℃.
S11, packaging: and packaging the lithium carbonate obtained by the S10, so that the lithium carbonate can be transported and stored conveniently in the later period, and a dry position is selected for storing the lithium carbonate when the lithium carbonate is stored.
From the above, it was found that the obtained lithium ion loss was large and the direct yield was low.
Example two
Referring to fig. 1, the present invention provides a technical solution: a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine specifically comprises the following steps:
s1, preparation: preparing brine, a container, an additive and tools to be used, checking whether omission exists or not, performing the next operation after the inspection is finished, and ensuring that the used objects and the container do not have dust and are in a clean state during preparation.
S2, stirring treatment: adding brine and aluminum chloride into a container, uniformly stirring and mixing the mixture by a stirrer for 2 hours, and taking out a precipitate to obtain a first mixed solution, wherein the molar ratio of the aluminum chloride to the lithium in the brine is 6:1 in S2.
S3, primary magnesium removal: adding sodium carbonate into the obtained mixed solution, stirring the mixed solution by a stirrer for 10 minutes to obtain a second mixed solution after the stirring is finished, and then continuously stirring the solution at 80 ℃ for reacting for 4 hours.
S4, first filtration and separation: thereby subjecting the solution obtained in S3 to solid-liquid separation treatment to obtain cake magnesium carbonate.
S5, secondary magnesium removal: calcium hydroxide was added to the solution of S4, followed by uniform stirring and mixing treatment with a stirrer, and reaction was carried out at 80 ℃ for 120 minutes, the lithium ion concentration in the solution being 13 g/L.
S6, second filtering and separating: the solution obtained in the step S5 is subjected to pressure filtration separation, so that a filter cake of magnesium hydroxide is obtained.
S7, evaporation and concentration: and (4) evaporating and concentrating the solution obtained in the step (S6) by 4 times, wherein the concentration of lithium ions after concentration can reach 50 g/L.
S8, re-reacting: the solution obtained in S8 was introduced into a reaction kettle, and sodium carbonate was slowly added thereto at 100 ℃ and stirred for 30 minutes.
S9, filter pressing separation: and (3) performing solid-liquid separation on the solution obtained in the step (S8), washing the solution with deionized water for 8 times, and fully drying the solution at 190 ℃ for 40 minutes to obtain lithium carbonate with the lithium carbonate content of 90%.
S10, cooling: and (4) cooling the lithium carbonate obtained in the step S9, wherein the cooling medium is an aqueous solution, and the temperature of the lithium carbonate after cooling in the step S10 is controlled at 45 ℃.
S11, packaging: and packaging the lithium carbonate obtained by the S10, so that the lithium carbonate can be transported and stored conveniently in the later period, and a dry position is selected for storing the lithium carbonate when the lithium carbonate is stored.
From the above, it was found that the obtained lithium ion loss was not insignificant, and the direct yield was not insignificant.
EXAMPLE III
Referring to fig. 1, the present invention provides a technical solution: a method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine specifically comprises the following steps:
s1, preparation: preparing brine, a container, an additive and tools to be used, checking whether omission exists or not, performing the next operation after the inspection is finished, and ensuring that the used objects and the container do not have dust and are in a clean state during preparation.
S2, stirring treatment: adding brine and aluminum chloride into a container, uniformly stirring and mixing the mixture by a stirrer for 1.5 hours, and taking out a precipitate to obtain a first mixed solution, wherein the molar ratio of the aluminum chloride to the lithium in the brine is 4:1 in S2.
S3, primary magnesium removal: adding sodium carbonate into the obtained mixed solution, stirring the mixed solution by a stirrer for 8 minutes to obtain a second mixed solution after the stirring is finished, and then continuously stirring the solution at 75 ℃ for reacting for 3 hours.
S4, first filtration and separation: thereby subjecting the solution obtained in S3 to solid-liquid separation treatment to obtain cake magnesium carbonate.
S5, secondary magnesium removal: calcium hydroxide was added to the solution of S4, followed by uniform mixing with stirring with a stirrer, and reaction was carried out at 60 ℃ for 100 minutes, the lithium ion concentration in the solution being 12 g/L.
S6, second filtering and separating: the solution obtained in the step S5 is subjected to pressure filtration separation, so that a filter cake of magnesium hydroxide is obtained.
S7, evaporation and concentration: and (4) evaporating and concentrating the solution obtained in the step (S6) by 3.5 times, wherein the concentration of lithium ions after concentration can reach 45 g/L.
S8, re-reacting: the solution obtained in S8 was introduced into a reaction kettle, and sodium carbonate was slowly added thereto at 90 ℃ and stirred for 30 minutes.
S9, filter pressing separation: and (3) performing solid-liquid separation on the solution obtained in the step (S8), washing the solution with deionized water for 7 times, and fully drying the solution at the temperature of 170 ℃ for 30 minutes to obtain lithium carbonate with the lithium carbonate content of 93%.
S10, cooling: and (4) cooling the lithium carbonate obtained in the step S9, wherein the cooling medium is an aqueous solution, and the temperature of the lithium carbonate after cooling in the step S10 is controlled at 35 ℃.
S11, packaging: and packaging the lithium carbonate obtained by the S10, so that the lithium carbonate can be transported and stored conveniently in the later period, and a dry position is selected for storing the lithium carbonate when the lithium carbonate is stored.
According to the three embodiments, the embodiment III is the best scheme, the loss of the lithium ions is greatly reduced, the extraction cost is reduced, the equipment requirement is smaller, the required equipment is simpler and more convenient, the convenience of operation is greatly improved, the labor force is reduced, the lithium direct yield is higher than 90%, the operation cost is lower, the energy consumption is greatly reduced, the purity of the prepared product is higher, and great convenience is brought to a user.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for improving the direct recovery rate of battery-grade lithium carbonate prepared from brine is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, preparation: preparing brine, a container, an additive and a tool which need to be used, checking whether omission exists or not, and performing the next operation after the inspection is finished;
s2, stirring treatment: adding brine and aluminum chloride into a container, uniformly stirring and mixing the mixture by a stirrer for 1-2 hours, and taking a precipitate to obtain a first mixed solution;
s3, primary magnesium removal: adding sodium carbonate into the obtained mixed solution, stirring the mixed solution by a stirrer for 5 to 10 minutes to obtain a second mixed solution after stirring, and continuously stirring the solution at the temperature of between 50 and 80 ℃ for reacting for 2 to 4 hours;
s4, first filtration and separation: so that the solution obtained in the step S3 is subjected to solid-liquid separation treatment to obtain filter cake magnesium carbonate;
s5, secondary magnesium removal: adding calcium hydroxide into the solution of S4, uniformly stirring and mixing the solution by a stirrer, and reacting the solution at the temperature of between 50 and 80 ℃ for 60 to 120 minutes, wherein the concentration of lithium ions in the solution is between 10 and 13 g/L;
s6, second filtering and separating: carrying out filter pressing separation on the obtained solution in the S5 so as to obtain a filter cake magnesium hydroxide;
s7, evaporation and concentration: evaporating and concentrating the solution obtained in the step S6 by 3-4 times, wherein the concentration of lithium ions after concentration can reach 40-50 g/L;
s8, re-reacting: introducing the solution obtained in the step S8 into a reaction kettle, slowly adding sodium carbonate at the temperature of 80-100 ℃, and stirring for reaction for 30 minutes;
s9, filter pressing separation: carrying out solid-liquid separation on the solution obtained in the step S8, washing the solution for 5-8 times by using deionized water, and fully drying the solution at the temperature of 150 ℃ and 190 ℃ for 20-40 minutes to obtain lithium carbonate with the lithium carbonate content of 88-93%;
s10, cooling: cooling the lithium carbonate obtained in the step S9, wherein a cooling medium is an aqueous solution;
s11, packaging: and packaging the lithium carbonate obtained in the step S10 so as to be convenient for transportation and storage at a later stage.
2. The method of claim 1, wherein the method comprises the steps of: in preparation, the articles and containers used should be kept clean and free of dust.
3. The method of claim 2, wherein the method comprises the steps of: after cooling in S10, the temperature of lithium carbonate should be controlled at 20-45 ℃.
4. The method of claim 3, wherein the method comprises the steps of: in S2, the molar ratio of the aluminum chloride to the lithium in the brine is 2-6: 1.
5. The method of claim 4, wherein the method comprises the steps of: when the lithium carbonate is stored, a dry position is selected for storage.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8741256B1 (en) * | 2009-04-24 | 2014-06-03 | Simbol Inc. | Preparation of lithium carbonate from lithium chloride containing brines |
| CN105152191A (en) * | 2015-10-28 | 2015-12-16 | 中国科学院青海盐湖研究所 | Method for preparing lithium carbonate through salt lake brine with high ratio of magnesium to lithium |
| CN106517254A (en) * | 2016-05-26 | 2017-03-22 | 广州市睿石天琪能源技术有限公司 | Method for reducing magnesium content in brine |
| CN106629789A (en) * | 2016-09-12 | 2017-05-10 | 中国科学院青海盐湖研究所 | Method for extracting lithium from brine to prepare battery-grade lithium carbonate by ion exchange method |
| CN110182831A (en) * | 2019-05-28 | 2019-08-30 | 昌鑫生态科技(陕西)有限公司 | The technology of salt lake extraction lithium carbonate |
| CN111137909A (en) * | 2020-01-14 | 2020-05-12 | 中南大学 | Method for stepwise recovering lithium and magnesium in salt lake brine |
| CN111484046A (en) * | 2020-03-29 | 2020-08-04 | 衢州学院 | Method for extracting lithium from salt lake brine with high magnesium-lithium ratio |
-
2020
- 2020-11-12 CN CN202011262415.8A patent/CN112299454A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8741256B1 (en) * | 2009-04-24 | 2014-06-03 | Simbol Inc. | Preparation of lithium carbonate from lithium chloride containing brines |
| CN105152191A (en) * | 2015-10-28 | 2015-12-16 | 中国科学院青海盐湖研究所 | Method for preparing lithium carbonate through salt lake brine with high ratio of magnesium to lithium |
| CN106517254A (en) * | 2016-05-26 | 2017-03-22 | 广州市睿石天琪能源技术有限公司 | Method for reducing magnesium content in brine |
| CN106629789A (en) * | 2016-09-12 | 2017-05-10 | 中国科学院青海盐湖研究所 | Method for extracting lithium from brine to prepare battery-grade lithium carbonate by ion exchange method |
| CN110182831A (en) * | 2019-05-28 | 2019-08-30 | 昌鑫生态科技(陕西)有限公司 | The technology of salt lake extraction lithium carbonate |
| CN111137909A (en) * | 2020-01-14 | 2020-05-12 | 中南大学 | Method for stepwise recovering lithium and magnesium in salt lake brine |
| CN111484046A (en) * | 2020-03-29 | 2020-08-04 | 衢州学院 | Method for extracting lithium from salt lake brine with high magnesium-lithium ratio |
Non-Patent Citations (2)
| Title |
|---|
| 李存增等: "从吸附法盐湖卤水提锂溶液中去除钙、镁试验研究", 《湿法冶金》 * |
| 魏昊等: "电池级碳酸锂制备与提纯的研究进展", 《现代化工》 * |
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