CN111115663B - Nano spherical lithium hydroxide and preparation method thereof - Google Patents
Nano spherical lithium hydroxide and preparation method thereof Download PDFInfo
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- CN111115663B CN111115663B CN202010026536.6A CN202010026536A CN111115663B CN 111115663 B CN111115663 B CN 111115663B CN 202010026536 A CN202010026536 A CN 202010026536A CN 111115663 B CN111115663 B CN 111115663B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a nanometer spherical lithium hydroxide and a preparation method thereof, which are characterized in that: the particle size of the primary particles of the lithium hydroxide nanospheres is 10-600 nm, the particle size of D50 in a laser particle size test is 50-2000 nm, the purity of the lithium hydroxide nanospheres is more than 99.7%, and the balance of 0.01-0.2% of nonpolar organic matters and a proper amount of impurities. The nanosphere is compatible with a certain proportion of a nonpolar organic solvent and an ionic surfactant with a hydrophobic group through a lithium hydroxide solution to form stable water-in-oil, namely a structure that an organic matter wraps a water phase (W/O), so that a solution system forms emulsion liquid beads with nanometer and micron sizes, further, the lithium hydroxide of the liquid beads can be dried and separated out into spherical nanoparticles in a spraying process, in addition, the nonpolar organic matter has a little residue in the drying process, the dispersibility of the lithium hydroxide nanosphere is increased, the hardening of the lithium hydroxide particles is favorably prevented, and the better physical appearance and size of the lithium hydroxide nanosphere are maintained.
Description
Technical Field
The invention belongs to the technical field of electrode raw materials for physical preparation, and particularly relates to nano spherical lithium hydroxide and a preparation method thereof.
Background
In recent years, the rapidly developing new energy industry has driven a dramatic increase in the output of power lithium ion batteries. In the lithium ion battery anode material, lithium hydroxide is selected as one of important lithium sources, and the quality of the lithium hydroxide directly influences the performance of the lithium ion anode material. Therefore, many scientific researchers have made a lot of scientific researches on improving the quality of lithium hydroxide, but most of them are based on the purpose of purifying the components, and relatively few reports are made on the morphology and the size of the lithium hydroxide.
With the continuous improvement of the performance requirement of the lithium ion ternary cathode material, the ternary material is continuously developed towards high nickel. In order to improve the lithium mixing uniformity of the high nickel material, lower the sintering temperature, promote the sintering, etc., the requirements for the quality of lithium sources such as lithium hydroxide, etc. are increasingly high, in addition to the requirements for the composition, the requirements for the size and the shape of particles are also increasingly high.
Disclosure of Invention
The invention aims to solve the technical problem of providing nano spherical lithium hydroxide and a preparation method thereof, and can prepare lithium hydroxide nanospheres with uniform particle size and good dispersibility.
In order to solve the technical problems, the technical scheme of the invention is as follows: designing nano spherical lithium hydroxide, which is characterized in that: the particle size of the primary particles of the lithium hydroxide nanospheres is 10-600 nm, the particle size of D50 in a laser particle size test is 50-2000 nm, the purity of the lithium hydroxide nanospheres is more than 99.7%, and the balance of 0.01-0.2% of polar organic matters and a proper amount of impurities.
Preferably, the polar organic substance is one or a combination of any two or more of methanol, ethanol, propanol, propylene glycol, polyethylene glycol, sulfonated kerosene, diethyl ether and acetone.
The invention also provides a method for preparing the nano spherical lithium hydroxide, which is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a lithium hydroxide solution: completely dissolving lithium hydroxide with the purity of more than 99.7 percent in deionized water to prepare a lithium hydroxide solution;
(2) preparing a lithium hydroxide emulsion: adding a polar organic solvent and an ionic surfactant into the lithium hydroxide solution prepared in the step (1), and uniformly stirring to prepare a lithium hydroxide emulsion, wherein the ionic surfactant is provided with a hydrophobic group, the mass consumption of the ionic surfactant is 0.01-0.2% of that of the deionized water in the step (1), and the mass consumption of the polar organic solvent is 4-25% of that of the deionized water in the step (1);
(3) preparing balls: spray drying the lithium hydroxide emulsion prepared in the step (2) to prepare lithium hydroxide nanospheres, wherein the temperature of spray drying is 100-400 ℃;
(4) and (3) drying: and (4) drying and dehydrating the lithium hydroxide nanospheres prepared in the step (3) at the temperature of 140-400 ℃ to prepare the nano spherical lithium hydroxide particles.
Preferably, the concentration of the lithium hydroxide solution in the step (1) is 0.01-5.4 mol/L.
Preferably, the ionic surfactant used in step (2) is an anionic surfactant or a cationic surfactant.
Preferably, the stirring temperature in the step (2) is 20-50 ℃.
Preferably, the polar organic solvent used in step (2) is one or a combination of any two or more of methanol, ethanol, propanol, propylene glycol, polyethylene glycol, sulfonated kerosene, diethyl ether and acetone.
Preferably, the ionic surfactant used in step (2) is one or a combination of any two or more of sodium dodecyl sulfate, sodium tetradecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate and sodium stearate.
Compared with the prior art, the invention has the beneficial effects that:
1. the lithium hydroxide solution is compatible with a certain proportion of polar organic solvent and the ionic surfactant with hydrophobic groups to form stable water-in-oil, namely a structure that an organic matter wraps a water phase (W/O), so that a solution system forms emulsion liquid beads with nanometer and micron sizes, lithium hydroxide in the liquid beads can be dried and separated out into spherical nano particles in a spraying process, little polar organic matter remains in the drying process, the dispersibility of the lithium hydroxide nanospheres is improved, the hardening of the lithium hydroxide particles is favorably prevented, and the better physical appearance and size of the lithium hydroxide nanospheres are maintained.
2. Because the spray drying mode is adopted to dry the nano and micron emulsion liquid beads dispersed into the W/O structure, the liquid drops can be atomized and dispersed into smaller liquid beads, and the drying into single dispersed balls is facilitated.
3. Because the concentration of the lithium hydroxide solution is selected to be 0.01-5.4 mol/L, the granulation efficiency can be improved and the economical efficiency can be improved on the premise of ensuring the good size of the product.
4. The temperature of spray drying is 100-400 ℃, so that under the condition of preventing bonding among the spherical lithium hydroxide particles, water and partial organic matters can be removed rapidly, and lithium hydroxide is crystallized and precipitated.
5. Because the secondary drying is carried out after the spray drying, on one hand, the crystal water which cannot be removed in the spray drying process is formed into anhydrous lithium hydroxide, the agglomeration performance of the anhydrous lithium hydroxide is reduced, and the formation of single dispersed particles is facilitated; on the other hand, the organic matters which are not completely removed are further removed, which is beneficial to improving the content of the lithium hydroxide, so that the lithium hydroxide can reach the battery grade requirement.
6. The dried lithium hydroxide spherical particles still have 0.01-0.2% of organic matters to wrap the spherical lithium hydroxide, and the organic matters are favorable for preventing the lithium hydroxide particles from hardening and have the effect of dispersing the particles.
7. According to the invention, the size of the prepared ball is controllable through the concentration of the lithium hydroxide solution, and the nano-sphere can reduce the friction among particles, is convenient to disperse, can uniformly mix lithium with ternary materials, provides a better fluxing action, is a promising lithium battery raw material, and is suitable for popularization and application in the industry.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of nanospheres of example 3 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1
This example was prepared by the following steps:
(1) preparing a lithium hydroxide solution: taking 125.7 parts by mass of lithium hydroxide (analytically pure, purity of 99.9%), putting into 1000 parts by mass of deionized water, and fully stirring and dissolving to prepare a lithium hydroxide solution with the concentration of 3 mol/L;
(2) preparing a lithium hydroxide emulsion: adding 40 parts by mass of sulfonated kerosene and 0.20 part by mass of sodium tetradecyl sulfate into the lithium hydroxide solution prepared in the step (1), and uniformly stirring to prepare a lithium hydroxide emulsion;
(3) preparing balls: spraying, pelletizing and drying the lithium hydroxide emulsion prepared in the step (2) at 250 ℃ by using a spray drying device to prepare lithium hydroxide nanospheres;
(4) and (3) drying: and (4) fully drying the lithium hydroxide nanospheres prepared in the step (3) in drying equipment at 220 ℃, and removing organic matters and structural water to prepare the nano spherical lithium hydroxide particles.
Example 2
This example was prepared by the following steps:
(1) preparing a lithium hydroxide solution: taking 41.9 parts by mass of lithium hydroxide (analytically pure, with the purity of 99.9%), putting into 10000 parts by mass of deionized water, and fully stirring and dissolving to prepare a lithium hydroxide solution with the concentration of 0.1 mol/L;
(2) preparing a lithium hydroxide emulsion: adding 2072 parts by mass of propylene glycol into the lithium hydroxide solution prepared in the step (1), adding 0.02 part by mass of sodium dodecyl sulfate, and uniformly stirring to prepare a lithium hydroxide emulsion;
(3) preparing balls: spraying, pelletizing and drying the lithium hydroxide emulsion prepared in the step (2) at 100 ℃ by using a spray drying device to prepare lithium hydroxide nanospheres;
(4) and (3) drying: and (4) fully drying the lithium hydroxide nanospheres prepared in the step (3) in drying equipment at the temperature of 400 ℃, and removing organic matters and structural water to prepare the nano spherical lithium hydroxide particles.
Example 3
This example was prepared by the following steps:
(1) preparing a lithium hydroxide solution: taking 41.9 parts by mass of lithium hydroxide (analytically pure, purity of 99.9%), putting into 1000 parts by mass of deionized water, and fully stirring for dissolving to prepare a lithium hydroxide solution with the concentration of 1 mol/L;
(2) preparing a lithium hydroxide emulsion: adding 127 parts by mass of polyethylene glycol and 0.02 part by mass of sodium dodecyl sulfate into the lithium hydroxide solution prepared in the step (1), and uniformly stirring to prepare a lithium hydroxide emulsion;
(3) preparing balls: spraying, pelletizing and drying the lithium hydroxide emulsion prepared in the step (2) at 400 ℃ by using a spray drying device to prepare lithium hydroxide nanospheres;
(4) and (3) drying: and (4) fully and uniformly stirring the lithium hydroxide nanospheres prepared in the step (3) by a three-dimensional mixer, placing the mixture in drying equipment at 140 ℃ for full drying, and removing organic matters and structural water to prepare the nano spherical lithium hydroxide particles. An electron microscopic scan of the lithium hydroxide particles is shown in figure 1.
Comparative example 1
500g of lithium hydroxide (analytically pure, purity of 99.9%) is taken, 500g of ethanol is taken and placed in a ball mill filled with 1000g of clean 0.2mm zirconia balls, ball milling is carried out until D50 laser granularity is tested to be 831nm, grinding is stopped, ground turbid liquid is taken out and placed in drying equipment for drying at 140 ℃, and lithium hydroxide particles are obtained.
Comparative example 2
500g of lithium hydroxide (analytically pure, the purity is 99.9 percent), 500g of ethanol is put into a ball mill filled with 1000g of clean 0.2mm zirconia balls, the ball milling is carried out until the D50 laser granularity is tested to be 831nm, the grinding is stopped, the ground turbid liquid is taken out, the turbid liquid is put into drying equipment for drying at 140 ℃, 0.02g of sodium dodecyl sulfate is added, the mixture is fully stirred by a three-dimensional mixer and then is put into the drying equipment for fully drying at 200 ℃, and the nano lithium hydroxide particles are obtained.
Test results
1. Laser particle size testing
The test method comprises the following steps: the samples obtained after drying in examples 1 to 3 and comparative examples 1 to 2 and the samples obtained after vacuum packaging and storage for 50 days were tested, 1g of lithium hydroxide was placed in 10g of ethanol in which saturated lithium hydroxide was dissolved (lithium hydroxide could not be dissolved in the ethanol solution again), and after 5min of ultrasonic vibration, the samples were tested by a laser particle size analyzer, and the test results are shown in table 1 below. As can be seen from the particle size distribution, the nano-size in examples 1 to 3 has a wide variable range, and after 50 days of storage, the particle size in the examples is uniform and fine, and is substantially equivalent to the particle size after direct drying, and no hardening exists, while in the comparative examples, the non-spherical or non-spherical coated dispersants have certain hardening agglomeration, which results in coarse particles.
TABLE 1 laser particle size test
2. Lithium hydroxide content test
The test method comprises the following steps: after lithium hydroxide is taken and tested by ICP-MS to obtain the lithium content, and the lithium content is converted into lithium hydroxide, the result is shown in the following table 2, and after certain organic dispersion is added compared with the examples 1-3 and the comparative example 2, the purity is reduced to a certain extent and is still more than 99.7% compared with the comparative example 1, the purity is kept higher, and the purity requirement of battery-grade lithium hydroxide is met.
TABLE 2 lithium hydroxide content
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (7)
1. A nano spherical lithium hydroxide is characterized in that: the particle size of the primary particles of the lithium hydroxide nanospheres is 10-600 nm, the particle size of D50 in a laser particle size test is 50-2000 nm, the purity of the lithium hydroxide nanospheres is more than 99.7%, and the balance of 0.01-0.2% of polar organic matters and a proper amount of impurities.
2. The nanospherical lithium hydroxide of claim 1, wherein: the polar organic matter is one or the combination of more than two of methanol, ethanol, propanol, propylene glycol, polyethylene glycol, sulfonated kerosene, diethyl ether and acetone.
3. A preparation method of nano spherical lithium hydroxide is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a lithium hydroxide solution: completely dissolving lithium hydroxide with the purity of more than 99.7% in deionized water to prepare a lithium hydroxide solution, wherein the concentration of the lithium hydroxide solution is 0.01-5.4 mol/L;
(2) preparing a lithium hydroxide emulsion: adding a polar organic solvent and an ionic surfactant into the lithium hydroxide solution prepared in the step (1), and uniformly stirring to prepare a lithium hydroxide emulsion, wherein the ionic surfactant has a hydrophobic group, the mass consumption of the ionic surfactant is 0.01-0.2% of that of the deionized water in the step (1), and the mass consumption of the polar organic solvent is 4-25% of that of the deionized water in the step (1);
(3) preparing balls: spray drying the lithium hydroxide emulsion prepared in the step (2) to prepare lithium hydroxide nanospheres, wherein the temperature of spray drying is 100-400 ℃;
(4) and (3) drying: and (4) drying and dehydrating the lithium hydroxide nanospheres prepared in the step (3) at the temperature of 140-400 ℃ to prepare the nano spherical lithium hydroxide particles.
4. The method for preparing nano spherical lithium hydroxide according to claim 3, wherein: the ionic surfactant used in the step (2) is an anionic surfactant or a cationic surfactant.
5. The method for preparing nano spherical lithium hydroxide according to claim 3, wherein: the stirring temperature in the step (2) is 20-50 ℃.
6. The method for preparing nano spherical lithium hydroxide according to any one of claims 3 to 5, wherein: the polar organic solvent used in the step (2) is one or the combination of any two of methanol, ethanol, propanol, propylene glycol, polyethylene glycol, sulfonated kerosene, diethyl ether and acetone.
7. The method for preparing nano spherical lithium hydroxide according to any one of claims 3 to 5, wherein: the ionic surfactant used in the step (2) is one or the combination of any two of sodium dodecyl sulfate, sodium tetradecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate and sodium stearate.
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| CN112299452A (en) * | 2020-10-29 | 2021-02-02 | 湖南永杉锂业有限公司 | Coating modified anhydrous lithium hydroxide and preparation method thereof |
| CN112216834B (en) * | 2020-10-29 | 2021-08-03 | 湖南永杉锂业有限公司 | Method for preparing modified anhydrous lithium hydroxide by spray coating |
| CN112939034B (en) * | 2021-03-19 | 2023-08-15 | 江西云威新材料有限公司 | Method for preparing battery-grade anhydrous lithium hydroxide from industrial-grade lithium carbonate |
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