CN113735143A - Method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide - Google Patents
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- CN113735143A CN113735143A CN202111134010.0A CN202111134010A CN113735143A CN 113735143 A CN113735143 A CN 113735143A CN 202111134010 A CN202111134010 A CN 202111134010A CN 113735143 A CN113735143 A CN 113735143A
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- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 title claims abstract description 181
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 81
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000010000 carbonizing Methods 0.000 title claims abstract description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012535 impurity Substances 0.000 claims abstract description 25
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 24
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 22
- 238000003763 carbonization Methods 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 14
- 238000001728 nano-filtration Methods 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 159000000002 lithium salts Chemical class 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 229910000032 lithium hydrogen carbonate Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- DVSDBMFJEQPWNO-UHFFFAOYSA-N methyllithium Chemical compound C[Li] DVSDBMFJEQPWNO-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- 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)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide. The method comprises the following steps: step S1: dissolving lithium hydroxide with pure water, and filtering and intercepting insoluble substances through an ultrafiltration membrane to obtain filtrate; step S2: nano-filtering the filtrate to remove impurity ions to obtain a lithium hydroxide refined solution; step S3: introducing carbon dioxide into the lithium hydroxide refined solution to perform carbonization operation, and performing centrifugal separation to obtain a lithium carbonate wet material; step S4: and stirring and washing the lithium carbonate wet material by using pure water, and drying to obtain a high-purity lithium carbonate product. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide has the advantages of simple process, high conversion rate, extremely low product impurities, low requirement on equipment and suitability for mass production, and the prepared high-purity lithium carbonate meets the following requirements: li2CO3≧99.99%，Na≤3ppm，Si≤4ppm，Ca≤4ppm，Fe≤2ppm。
Description
Technical Field
The invention relates to the technical field of chemical production of high-purity lithium carbonate, in particular to a method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide.
Background
The international market supply and demand of the technical-grade lithium carbonate tend to be saturated, the price is greatly reduced due to the reduction of development cost, and the development of high-purity lithium carbonate can increase the added value of products and is beneficial to the extension of lithium product series development and lithium industrial chain. On the other hand, as the application range of lithium products in the high-tech field is continuously expanded, the demand for lithium salt is increasing at home and abroad, and the purity requirement for the products is higher and higher, so that the development of high-added-value high-purity lithium salt products is imperative.
High-purity lithium carbonate is a necessity in the magnetic material industry, the atomic energy industry, the electronic industry, the optical instrument industry and the like. In recent years, high-purity lithium carbonate used as a positive electrode material and an electrolyte material of a lithium ion battery has been receiving increasing attention. In addition, the high-purity lithium carbonate is used as a basic lithium salt, and can also be used for producing high-purity secondary lithium salts such as high-purity lithium chloride, lithium bromide and the like, and further, after metal lithium is produced through electrolysis, a plurality of organic lithium compounds such as butyl lithium, methyl lithium and the like can be derived. The existing preparation methods of high-purity lithium carbonate are mainly divided into two types: direct synthesis and purification of crude lithium carbonate. However, the first method has low carbonization efficiency, low pyrolysis conversion rate, large mother liquor treatment capacity and high processing cost, and the second method has high requirements on raw material purity, high raw material cost, complex flow and high processing cost. However, the method for preparing the high-purity lithium carbonate by directly carbonizing the battery-grade lithium hydroxide as the raw material has the advantages of short process flow, simple operation, high conversion rate, low processing cost, great economic benefit and suitability for mass production in factories compared with other preparation methods.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide comprises the following steps:
step S1 dissolution: putting raw material lithium hydroxide into a container, adding pure water, fully stirring and dissolving, filtering insoluble substances by using an ultrafiltration membrane, and collecting filtrate;
step S2 impurity removal: removing Ca, Si, Fe and SO from the filtrate by a nanofiltration device4 2-Obtaining lithium hydroxide refined liquid by impurity ions;
step S3 carbonization: introducing carbon dioxide into the lithium hydroxide refined solution to perform carbonization operation, controlling the pH value of the solution, and separating by a centrifuge to obtain a lithium carbonate wet material;
step S4 washing and drying: and stirring and washing the lithium carbonate wet material by pure water, and heating and drying to obtain a high-purity lithium carbonate product.
Furthermore, the raw material used in step S1 is battery-grade lithium hydroxide, and the raw material is usually dissolved by adding 4-6 times of pure water.
Furthermore, the impurity content Ca of the solution is controlled to be less than or equal to 0.005g/L, Fe is controlled to be less than or equal to 0.003g/L, Si is controlled to be less than or equal to 0.003g/L, and SO is controlled to be less than or equal to 0.005g/L through nanofiltration operation in the step S24 2-≤0.020g/L。
Further, the carbon dioxide introduced in the step S3 is high-purity carbon dioxide, and the purity is 99.99%.
Further, the reaction end point in the step S3 is generally controlled to have pH =9 to 11, and a higher conversion rate can be achieved.
Further, the carbonization mother liquor obtained by filtering in the step S3 can be recycled and can be used for dissolving the lithium hydroxide in the step S1.
Further, in step S4, the lithium carbonate is usually washed with 1 to 3 times of pure water, so that soluble impurities in the lithium carbonate can be removed.
Further, in the step S4, the drying temperature is controlled to be 160-220 ℃, and the drying time is controlled to be 1-3 hours.
Compared with other high-purity lithium carbonate preparation methods, the method has the following characteristics: the method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide provided by the invention comprises the following steps of S1: dissolving lithium hydroxide with pure water, and filtering and intercepting insoluble substances through an ultrafiltration membrane to obtain filtrate; step S2: nano-filtering the filtrate to remove impurity ions to obtain a lithium hydroxide refined solution; step S3: introducing carbon dioxide into the lithium hydroxide refined solution to perform carbonization operation, and performing centrifugal separation to obtain a lithium carbonate wet material; step S4: and stirring and washing the lithium carbonate wet material by using pure water, and drying to obtain a high-purity lithium carbonate product. The high-purity lithium carbonate prepared by the method meets the following requirements: li2CO3Not less than 99.99 percent, not more than 3ppm of Na, not more than 4ppm of Si, not more than 4ppm of Ca and not more than 2ppm of Fe. The method has the advantages of simple process, high conversion rate, extremely low product impurity, low requirement on equipment and suitability for mass production.
The high-purity lithium carbonate prepared by the invention is mainly used for preparing the anode material of the lithium ion battery and used as the electrolyte raw material. The high-purity lithium carbonate prepared by the method meets the requirement of Li2CO3Not less than 99.99 percent, not more than 3ppm of Na, not more than 4ppm of Si, not more than 4ppm of Ca and not more than 2ppm of Fe; compared with other methods, the method has the reaction stepsThe method has the advantages of low energy consumption, simple process, low impurity content of the product, suitability for mass production and great advantage in production.
The reaction principle of the method is as follows:
LiOH + C02 → Li2C03↓ + H2O
under the reaction condition of excessive carbon dioxide, different products are generated, in order to prevent the generation of a byproduct LiHC03The experimental pH value needs to be strictly controlled.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it should be obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic flow chart of the method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to the invention.
Detailed Description
The following is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements are also considered to be within the scope of the present invention.
Referring to fig. 1, the present invention provides a method for preparing high-purity lithium carbonate by direct carbonization of lithium hydroxide, wherein step S1 includes: putting raw material lithium hydroxide into a container, adding pure water, fully stirring and dissolving, filtering insoluble substances by using an ultrafiltration membrane, and collecting filtrate; step S2 impurity removal: removing Ca, Si, Fe and SO from the filtrate by a nanofiltration device4 2-Obtaining lithium hydroxide refined liquid by impurity ions; step S3 carbonization: introducing carbon dioxide into the lithium hydroxide refined solution to perform carbonization operation, controlling the pH value of the solution, and separating by a centrifuge to obtain a lithium carbonate wet material; step S4 washing and drying: and stirring and washing the lithium carbonate wet material by pure water, and heating and drying to obtain a high-purity lithium carbonate product.
Furthermore, the raw material used in step S1 is battery-grade lithium hydroxide, and the raw material is usually dissolved by adding 4-6 times of pure water.
Furthermore, the impurity content Ca of the solution is controlled to be less than or equal to 0.005g/L, Fe is controlled to be less than or equal to 0.003g/L, Si is controlled to be less than or equal to 0.003g/L, and SO is controlled to be less than or equal to 0.005g/L through nanofiltration operation in the step S24 2-≤0.020g/L。
Further, the carbon dioxide introduced in the step S3 is high-purity carbon dioxide, and the purity is 99.99%.
Further, the reaction end point in the step S3 is generally controlled to have pH =9 to 11, and a higher conversion rate can be achieved.
Further, the carbonization mother liquor obtained by filtering in the step S3 can be recycled and can be used for dissolving the lithium hydroxide in the step S1.
Further, in step S4, the lithium carbonate is usually washed with 1 to 3 times of pure water, so that soluble impurities in the lithium carbonate can be removed.
Further, in the step S4, the drying temperature is controlled to be 160-220 ℃, and the drying time is controlled to be 1-3 hours.
Compared with other high-purity lithium carbonate preparation methods, the method has the following characteristics: the method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide provided by the invention comprises the following steps of S1: dissolving lithium hydroxide with pure water, and filtering and intercepting insoluble substances through an ultrafiltration membrane to obtain filtrate; step S2: nano-filtering the filtrate to remove impurity ions to obtain a lithium hydroxide refined solution; step S3: introducing carbon dioxide into the lithium hydroxide refined solution to perform carbonization operation, and performing centrifugal separation to obtain a lithium carbonate wet material; step S4: and stirring and washing the lithium carbonate wet material by using pure water, and drying to obtain a high-purity lithium carbonate product. The high-purity lithium carbonate prepared by the method meets the following requirements: li2CO3Not less than 99.99 percent, not more than 3ppm of Na, not more than 4ppm of Si, not more than 4ppm of Ca and not more than 2ppm of Fe. The method has the advantages of simple process, high conversion rate, extremely low product impurity, low requirement on equipment and suitability for mass production.
The high-purity lithium carbonate prepared by the invention is mainly used for preparing the anode material of the lithium ion battery and used as the electrolyte raw material. The high-purity lithium carbonate prepared by the method meets the requirement of Li2CO3≧99.99Percent, Na is less than or equal to 3ppm, Si is less than or equal to 4ppm, Ca is less than or equal to 4ppm, and Fe is less than or equal to 2 ppm; compared with other methods, the method has the advantages of less reaction steps, low energy consumption, simple process, low impurity content of the product, suitability for mass production and great advantage in production.
The reaction principle of the method is as follows:
LiOH + C02 → Li2C03↓ + H2O
under the reaction condition of excessive carbon dioxide, different products are generated, in order to prevent the generation of a byproduct LiHC03The experimental pH value needs to be strictly controlled.
Example 1
A method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide comprises the following specific steps:
s1 dissolution: putting 500g of lithium hydroxide into a container, adding 2L of pure water, fully stirring for 30min, filtering out insoluble substances by using an ultrafiltration membrane, and collecting filtrate;
s2 impurity removal: injecting the filtrate obtained in the step S1 into a nanofiltration device to obtain refined lithium hydroxide solution;
s3 carbonization: introducing high-purity carbon dioxide into the lithium hydroxide refined solution obtained in the step S2 to perform carbonization operation, controlling the introduction amount of the carbon dioxide by a pH meter so that the pH of the solution is =9, and performing centrifugal separation by a centrifugal machine to obtain 510g of lithium carbonate;
s4 washing and drying: the mixture was stirred and washed with 500ml of pure water to obtain a wet lithium carbonate, and then the product was dried at 180 ℃ to obtain 460g of high purity lithium carbonate, which was designated as sample 1.
Example 2
A method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide comprises the following specific steps:
s1 dissolution: putting 1000g of lithium hydroxide into a container, adding 5L of pure water, fully stirring for 30min, filtering insoluble substances by using an ultrafiltration membrane, and collecting filtrate;
s2 impurity removal: injecting the filtrate obtained in the step S1 into a nanofiltration device to obtain refined lithium hydroxide solution;
s3 carbonization: introducing high-purity carbon dioxide into the lithium hydroxide refined solution obtained in the step S2 to perform carbonization operation, controlling the introduction amount of the carbon dioxide by a pH meter so that the pH of the solution is =11, and performing centrifugal separation by a centrifugal machine to obtain 1050g of lithium carbonate;
s4 washing and drying: the mixture was stirred and washed with 2L of pure water to obtain a wet lithium carbonate, and the product was dried at 200 ℃ to obtain 915g of high purity lithium carbonate, which was designated as sample 2.
Example 3
A method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide comprises the following specific steps:
s1 dissolution: putting 600g of lithium hydroxide into a container, adding 3.6L of pure water, fully stirring for 30min, filtering out insoluble substances by using an ultrafiltration membrane, and collecting filtrate;
s2 impurity removal: injecting the filtrate obtained in the step S1 into a nanofiltration device to obtain refined lithium hydroxide solution;
s3 carbonization: introducing high-purity carbon dioxide into the lithium hydroxide refined solution obtained in the step S2 to perform carbonization operation, controlling the introduction amount of the carbon dioxide by a pH meter so that the pH of the solution is =10, and performing centrifugal separation by a centrifugal machine to obtain 635g of lithium carbonate;
s4 washing and drying: this was stirred and washed with 1.3L of pure water to give a wet lithium carbonate, and the product was then dried at 210 ℃ to give 560g of high purity lithium carbonate, which was designated as sample 3.
Example 4
A method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide comprises the following specific steps:
s1 dissolution: putting 800g of lithium hydroxide into a container, adding 4L of pure water, fully stirring for 30min, filtering out insoluble substances by using an ultrafiltration membrane, and collecting filtrate;
s2 impurity removal: injecting the filtrate obtained in the step S1 into a nanofiltration device to obtain refined lithium hydroxide solution;
s3 carbonization: introducing high-purity carbon dioxide into the lithium hydroxide refined solution obtained in the step S2 to perform carbonization operation, controlling the introduction amount of the carbon dioxide by a pH meter so that the pH of the solution is =10, and performing centrifugal separation by a centrifugal machine to obtain 830g of lithium carbonate;
s4 washing and drying: the resulting mixture was stirred and washed with 1.7L of pure water to give a wet lithium carbonate, and the product was dried at 170 ℃ to give 740g of high purity lithium carbonate, which was designated as sample 4.
The results of analyzing the components of the samples obtained in examples 1 to 4 are shown in the following table:
| sample numbering | Li2CO3 | Na | Si | Fe | Ca |
| Sample No. 1 | 99.992% | 1.5ppm | 3.2ppm | 1.2ppm | 3ppm |
| Sample No. 2 | 99.995% | 2.0ppm | 3.2ppm | 1.1ppm | 2.9ppm |
| Sample No. 3 | 99.993% | 2.2ppm | 3.0ppm | 0.8ppm | 2.7ppm |
| Sample No. 4 | 99.991% | 2.3ppm | 3.1ppm | 0.7ppm | 3.1ppm |
From the above detection data, it can be known that the high-purity lithium carbonate prepared by the method satisfies the following requirements: li2CO3Not less than 99.99 percent, not more than 3ppm of Na, not more than 4ppm of Si, not more than 4ppm of Ca and not more than 2ppm of Fe. Namely, the preparation of high-purity lithium carbonate by direct carbonization of battery-grade lithium hydroxide has the advantages of short process flow, simple operation, conversion rate of over 90 percent, low processing cost and the like, and has very high economic value.
The above examples only express the specific embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the spirit of the present invention, and these changes and modifications are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. A method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide is characterized by comprising the following steps: the method comprises the following steps:
step S1: putting raw material lithium hydroxide into a container, adding pure water, fully stirring and dissolving, filtering insoluble substances by using an ultrafiltration membrane, and collecting filtrate;
step S2: removing Ca, Si, Fe and SO from the filtrate by a nanofiltration device4 2-Obtaining lithium hydroxide refined solution by impurity ions;
step S3: introducing carbon dioxide into the lithium hydroxide refined solution to perform carbonization operation, controlling the pH value of the solution, and separating by a centrifuge to obtain a lithium carbonate wet material;
step S4: and stirring and washing the lithium carbonate wet material by pure water, and heating and drying to obtain a high-purity lithium carbonate product.
2. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to claim 1, wherein: the raw material used in the step S1 is battery-grade lithium hydroxide, and 4-6 times of pure water is added to the raw material for dissolution.
3. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to claim 2, wherein: in the step S2, the impurity content Ca of the solution is controlled to be less than or equal to 0.005g/L, the impurity content Fe of the solution is controlled to be less than or equal to 0.003g/L, the impurity content Si of the solution is controlled to be less than or equal to 0.003g/L, and the impurity content SO of the solution is controlled to be less than or equal to 0.003g/L4 2-≤0.020g/L。
4. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to claim 3, wherein: the carbon dioxide introduced in the step S3 is high-purity carbon dioxide, and the purity is 99.99%.
5. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to claim 4, wherein: the reaction end point in the step S3 is generally controlled to pH =9 to 11, and a higher conversion rate can be achieved.
6. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to claim 5, wherein: and in the step S4, washing with 1-3 times of pure water.
7. The method for preparing high-purity lithium carbonate by directly carbonizing lithium hydroxide according to claim 6, wherein: in the step S4, the drying temperature is 160-220 ℃, and the drying time is 1-3 h.
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| CN115432723A (en) * | 2022-09-05 | 2022-12-06 | 南京工程学院 | Method for preparing battery-grade lithium carbonate by taking waste residues generated in production of n-butyllithium and sec-butyllithium as raw materials |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115432723A (en) * | 2022-09-05 | 2022-12-06 | 南京工程学院 | Method for preparing battery-grade lithium carbonate by taking waste residues generated in production of n-butyllithium and sec-butyllithium as raw materials |
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