CN114772615A - Production method of heavy rhombohedral boehmite - Google Patents
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- CN114772615A CN114772615A CN202210433539.0A CN202210433539A CN114772615A CN 114772615 A CN114772615 A CN 114772615A CN 202210433539 A CN202210433539 A CN 202210433539A CN 114772615 A CN114772615 A CN 114772615A
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- boehmite
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- rhombohedral
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- 229910001593 boehmite Inorganic materials 0.000 title claims abstract description 43
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 30
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 26
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 22
- 150000004684 trihydrates Chemical class 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 33
- 239000002244 precipitate Substances 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 13
- 238000000967 suction filtration Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 5
- 229910052708 sodium Inorganic materials 0.000 abstract description 5
- 239000011734 sodium Substances 0.000 abstract description 5
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 abstract description 2
- 238000004131 Bayer process Methods 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
- RREGISFBPQOLTM-UHFFFAOYSA-N alumane;trihydrate Chemical compound O.O.O.[AlH3] RREGISFBPQOLTM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Inorganic materials [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Inorganic materials [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
- C01P2006/11—Powder tap density
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to the technical field of heavy rhombohedral boehmite production, and discloses a production method of heavy rhombohedral boehmite, which comprises the following material components: alumina trihydrate, pseudo-boehmite, de-granulated water, seed crystals, a dispersing agent and an acid. According to the production method of heavy rhombic boehmite, the particle morphology of the boehmite prepared by the method is regular rhombus, and the boehmite has the characteristics of regular shape, narrow particle size distribution, high tap density, low sodium content, low iron content and the like, and can be used for coating lithium battery separators, so that the surface density of a coating can be remarkably improved, and the shrinkage rate can be reduced.
Description
Technical Field
The invention relates to the technical field of heavy rhombohedral boehmite production, in particular to a production method of heavy rhombohedral boehmite.
Background
The lithium ion battery has the advantages of high specific energy, high specific power, high conversion rate, long service life, no pollution and the like, and is widely applied to the fields of electric vehicles, power supplies, energy storage, electronics and communication. In order to improve the safety of the lithium battery, a layer of alumina or boehmite needs to be coated on the separator.
However, the conventional boehmite cannot satisfy the requirement because of a large coating shrinkage rate. Therefore, there is a need to control the morphology, particle size and particle size distribution of boehmite to meet the needs of lithium battery separator coatings.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a production method of heavy rhombohedral boehmite, which has the advantages of regular shape, narrow particle size distribution, large tap density, low sodium and low iron and the like, and solves the problems.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a process for the production of heavy rhombohedral boehmite, the material composition of which comprises: alumina trihydrate, pseudo-boehmite, de-granulated water, seed crystals, a dispersing agent and acid;
the production method of the heavy rhombohedral boehmite comprises the following steps: the method comprises the following steps:
1) heating and drying aluminum hydroxide, removing iron, screening, and removing large particles and small particles to obtain alumina trihydrate with proper granularity;
2) mixing and stirring alumina trihydrate, pseudo-boehmite, particle-removed water, seed crystal and a dispersing agent according to a certain proportion;
3) adding acid into the mixture after stirring and mixing to adjust the pH value to be 6-8, and then adding the mixture into a wet ball mill to be ground into slurry with specified granularity;
4) adding the slurry into a reaction kettle, stirring, heating to raise the temperature, raising the pressure to 1.0-2.5 MPa, and keeping the pressure at a certain temperature for 1-4 hours;
5) taking the slurry out, naturally cooling the slurry to room temperature in the air, then putting the slurry into a stirring tank, repeatedly performing suction filtration and washing by using deionized water until filtrate is neutral, and standing to precipitate and separate the filtrate;
6) filtering and separating the slurry after precipitation separation, taking out the precipitate after precipitation separation, and then drying the precipitate;
7) and (3) drying the precipitate by using a dryer, and drying the precipitate at the temperature of 120-280 ℃ for 12 hours to obtain the heavy rhombohedral boehmite with the tap density of more than 0.8g/cm 3.
Preferably, the aluminum hydroxide comprises industrial aluminum hydroxide produced by a sintering method or a Bayer method, and the aluminum hydroxide is subjected to heating drying, iron removal, screening and large particle and small particle removal to obtain alumina trihydrate with moderate particles.
Preferably, the pseudoboehmite comprises various pseudoboehmite produced by a carbonization method and a neutralization method, and the slurry is stirred in the reaction kettle at the rotation speed of 900rpm all the time.
Preferably, the seed crystal comprises one of sulfate, nitrate and chloride of aluminum, magnesium and lithium or a mixture thereof.
Preferably, when the alumina trihydrate, the pseudo-boehmite, the deionized water, the seed crystal and the dispersing agent are mixed, the materials are placed into a container and stirred in the container through a stirrer, the materials are primarily mixed, the mixing property of the materials is improved, and the PH is conveniently detected after the acid is added.
Preferably, the acid comprises sulfuric acid, nitric acid, hydrochloric acid, glacial acetic acid.
When the mixture is added into a wet ball mill and ground into slurry with specified granularity, attention should be paid to keeping the mixture clean in the wet ball mill so as to avoid influencing the quality of the mixture.
(III) advantageous effects
Compared with the prior art, the invention provides a production method of heavy rhombohedral boehmite, which has the following beneficial effects:
according to the production method of the heavy rhombohedral boehmite, the particle morphology of the boehmite prepared by the method is regular rhombohedral, and the boehmite has the characteristics of regular shape, narrow particle size distribution, high tap density, low sodium and low iron and the like, and can be used for coating lithium battery diaphragms, so that the surface density of the coating can be obviously improved, and the shrinkage rate can be reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows: a process for producing heavy rhombohedral boehmite comprising the steps of: the material composition of the heavy rhombohedral boehmite comprises alumina trihydrate, pseudo-boehmite, particle-removed water, seed crystal, a dispersing agent and acid;
the production method of the heavy rhombohedral boehmite comprises the following steps:
1) heating, drying, deironing and screening aluminum hydroxide to remove large particles and small particles to obtain aluminum trihydrate with proper granularity, wherein the aluminum hydroxide comprises industrial aluminum oxide produced by a sintering method or a Bayer process, the aluminum hydroxide is heated, dried, deironing and screened to obtain products of large particles, small particles and smaller particles, and the large particles and the small particles are removed to obtain the smaller particles of the aluminum trihydrate;
2) mixing and stirring alumina trihydrate, pseudo-boehmite, particle-removed water, seed crystals and a dispersing agent according to a certain proportion, wherein the pseudo-boehmite comprises the pseudo-boehmite produced by a carbonization method and a neutralization method, and the seed crystals comprise one or a mixture of sulfate, nitrate and chloride of aluminum, magnesium and lithium;
3) adding acid into the mixture after stirring and mixing to adjust the pH to be 6-8, then adding the mixture into a wet ball mill to be ground into slurry with a specified particle size, putting the materials into a container when mixing alumina trihydrate, pseudo-boehmite, de-particle water, seed crystals and a dispersing agent, stirring the materials in the container through a stirrer, performing primary mixing on the materials, improving the mixing property of the materials, conveniently adding the acid, detecting the pH, and slowly adding the acid into the mixture when adding the acid to avoid overhigh local acidity. When the mixture is added into a wet ball mill and ground into slurry with specified granularity, attention should be paid to keeping the wet ball mill clean so as to avoid influencing the quality of the mixture;
4) adding the slurry into a reaction kettle, stirring, heating to raise the temperature, raising the pressure to 1.0-2.5 MPa, and keeping the temperature for 1-4 hours;
5) and taking the slurry out, naturally cooling the slurry to room temperature in the air, then putting the slurry into a stirring tank, repeatedly performing suction filtration and washing by using deionized water until filtrate is neutral, and standing to precipitate and separate the filtrate.
6) And (4) carrying out suction filtration and separation on the slurry after the precipitation separation, taking out the precipitate after the precipitation separation, and then drying the precipitate. During suction filtration, only the slurry separated by precipitation needs to be pumped out, so that the precipitate is prevented from being pumped out;
7) and (3) drying the precipitate by using a dryer, and drying the precipitate at the temperature of 120-280 ℃ for 12 hours to obtain the heavy rhombohedral boehmite with the tap density of more than 0.8g/cm 3.
Example two: a process for the production of heavy rhombohedral boehmites comprising the steps of: the material composition of the heavy rhombohedral boehmite comprises pseudo-boehmite, particle-removed water, seed crystals, a dispersing agent and acid;
the production method of the heavy rhombohedral boehmite comprises the following steps:
1) heating, drying, deironing and screening aluminum hydroxide, removing large particles and small particles to obtain alumina trihydrate with proper granularity, wherein the aluminum hydroxide comprises industrial alumina produced by a sintering method or a Bayer process, the aluminum hydroxide is heated, dried, deironing and screened to obtain products with large particles, small particles and smaller particles, and the large particles and the small particles are removed to obtain the alumina trihydrate with the smaller particles;
2) mixing and stirring alumina trihydrate, pseudo-boehmite, particle-removed water, seed crystals and a dispersing agent according to a certain proportion, wherein the pseudo-boehmite comprises the pseudo-boehmite produced by a carbonization method and a neutralization method, and the seed crystals comprise one or a mixture of sulfate, nitrate and chloride of aluminum, magnesium and lithium;
3) adding acid into the mixture after stirring and mixing to adjust the pH to be 10-11, then adding the mixture into a wet ball mill to be ground into slurry with a specified particle size, putting the materials into a container when mixing alumina trihydrate, pseudo-boehmite, de-particle water, seed crystals and a dispersing agent, stirring the materials in the container through a stirrer, performing primary mixing on the materials, improving the mixing property of the materials, conveniently adding the acid, and then detecting the pH. The acid includes sulfuric acid, nitric acid, hydrochloric acid, and glacial acetic acid, and is added slowly to avoid excessive local acidity. When the mixture is added into a wet ball mill and ground into slurry with specified granularity, attention should be paid to keeping the wet ball mill clean to avoid influencing the quality of the mixture;
4) adding the slurry into a reaction kettle, stirring, heating to raise the temperature, raising the pressure to 1.0-2.5 MPa, and keeping the temperature for 1-4 hours;
5) and (3) naturally cooling the slurry to room temperature in the air, then putting the slurry into a stirring tank, repeatedly performing suction filtration and washing by using deionized water until filtrate is neutral, and standing to precipitate and separate the filtrate. When the slurry is washed, repeatedly washing the slurry by using deionized water in a suction filtration mode, and detecting the pH value of the filtrate by using pH meter paper after washing to make the filtrate neutral;
6) and (4) carrying out suction filtration and separation on the slurry after the precipitation separation, taking out the precipitate after the precipitation separation, and then drying the precipitate. When the slurry is extracted by precipitation separation and suction filtration, the slurry is extracted only by precipitation separation, so that the precipitate is prevented from being extracted;
7) and (3) drying the precipitate by using a dryer, and drying the precipitate at the temperature of 120-280 ℃ for 12 hours to obtain the heavy rhombohedral boehmite with the tap density of more than 0.8g/cm 3.
Example three: a process for producing heavy rhombohedral boehmite comprising the steps of: the material composition of the heavy rhombohedral boehmite comprises pseudo-boehmite, particle-removed water, seed crystals, a dispersing agent and acid;
the production method of the heavy rhombohedral boehmite comprises the following steps:
1) heating, drying, deironing and screening aluminum hydroxide, removing large particles and small particles to obtain alumina trihydrate with proper granularity, wherein the aluminum hydroxide comprises industrial alumina produced by a sintering method or a Bayer process, the aluminum hydroxide is heated, dried, deironing and screened to obtain products with large particles, small particles and smaller particles, and the large particles and the small particles are removed to obtain the alumina trihydrate with the smaller particles;
2) mixing and stirring alumina trihydrate, pseudo-boehmite, particle-removed water, seed crystals and a dispersing agent according to a certain proportion, wherein the pseudo-boehmite comprises pseudo-boehmite produced by a carbonization method and a neutralization method, and when slurry is stirred in a reaction kettle, a stirrer always stirs at the rotating speed of 200 rpm. The seed crystal comprises one or a mixture of aluminum sulfate, magnesium sulfate, lithium sulfate, nitrate and chloride;
3) after the PH of the mixture after the stirring and mixing was adjusted to 6 to 8 by adding an acid, the mixture was ground in a wet ball mill to a slurry having a predetermined particle size, and when alumina trihydrate, pseudo-boehmite, departiculate water, seed crystal and dispersant were mixed, these materials were put in a container and stirred in the container by a stirrer to perform primary mixing of these materials. The acid includes sulfuric acid, nitric acid, hydrochloric acid, and glacial acetic acid. When the mixture is added into a wet ball mill and ground into slurry with specified granularity, attention should be paid to keeping the wet ball mill clean so as to avoid influencing the quality of the mixture;
4) adding the slurry into a reaction kettle, stirring, heating to raise the temperature, raising the pressure to 1.0-2.5 MPa, and keeping the pressure at a certain temperature for 0.5 hour;
5) taking the slurry out, naturally cooling the slurry to room temperature in the air, then putting the slurry into a stirring tank, repeatedly performing suction filtration and washing by using deionized water until filtrate is neutral, standing the filtrate to precipitate and separate the precipitate, repeatedly cleaning the slurry by using a suction filtration mode when the slurry is washed, and detecting the pH value of the filtrate by using a pH test paper after washing to make the filtrate neutral;
6) filtering and separating the slurry after precipitation separation, taking out the precipitate after precipitation separation, and then drying the precipitate;
7) and (3) drying the precipitate by using a dryer, and drying the precipitate at the temperature of 120-280 ℃ for 12 hours to obtain the heavy rhombohedral boehmite with the tap density of more than 0.8g/cm 3.
And (4) judging the standard: in the first embodiment, the mixture is added with acid to adjust the pH value of 6-8, and the slurry is added into a reaction kettle to be stirred, heated and heated to keep the mixture at a certain temperature for 1-4 hours, so that the mixture has the characteristics of regular shape, narrow particle size distribution, high tap density, low sodium and low iron.
The invention has the beneficial effects that: according to the production method of heavy rhombic boehmite, the particle morphology of the boehmite prepared by the method is regular rhombus, and the boehmite has the characteristics of regular shape, narrow particle size distribution, high tap density, low sodium content, low iron content and the like, and can be used for coating lithium battery separators, so that the surface density of a coating can be remarkably improved, and the shrinkage rate can be reduced.
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 (6)
1. A production method of heavy rhombohedral boehmite is characterized in that: the material composition of the heavy rhombohedral boehmite comprises: alumina trihydrate, pseudo-boehmite, de-granulated water, seed crystals, a dispersing agent and acid;
the production method of the heavy rhombohedral boehmite comprises the following steps:
1) heating and drying aluminum hydroxide, removing iron, screening, and removing large particles and small particles to obtain alumina trihydrate with proper granularity;
2) mixing and stirring alumina trihydrate, pseudo-boehmite, particle-removed water, seed crystal and a dispersing agent according to a certain proportion;
3) adding acid into the mixture after stirring and mixing to adjust the pH value to be 6-8, and then adding the mixture into a wet ball mill to be ground into slurry with specified granularity;
4) adding the slurry into a reaction kettle, stirring, heating to raise the temperature, raising the pressure to 1.0-2.5 MPa, and keeping the pressure at a certain temperature for 1-4 hours;
5) taking the slurry out, naturally cooling the slurry to room temperature in the air, then putting the slurry into a stirring tank, repeatedly performing suction filtration and washing by using deionized water until the filtrate is neutral, and standing to precipitate and separate the filtrate;
6) carrying out suction filtration separation on the slurry after the precipitation separation, taking out the precipitate after the precipitation separation, and then drying the precipitate;
7) and (3) drying the precipitate by using a dryer, and drying the precipitate at the temperature of 120-280 ℃ for 12 hours to obtain the heavy rhombohedral boehmite with the tap density of more than 0.8g/cm 3.
2. A process for the production of heavy rhombohedral boehmite according to claim 1, characterized in that: the aluminum hydroxide comprises various aluminum hydroxides produced by a sintering method or a Bayer method, the aluminum hydroxide is heated, dried, deironized and screened to obtain products with large particles, small particles and smaller particles, and the large particles and the small particles are removed to obtain alumina trihydrate with moderate particles.
3. A process for the production of heavy rhombohedral boehmite according to claim 1, characterized in that: the pseudoboehmite comprises various pseudoboehmite produced by a carbonization method and a neutralization method.
4. A process for the production of heavy rhombohedral boehmite according to claim 1, characterized in that: the seed crystal comprises one of sulfate, nitrate and chloride of aluminum, magnesium and lithium or a mixture thereof.
5. A process for the production of heavy rhombohedral boehmite according to claim 1, characterized in that: when the alumina trihydrate, the pseudo-boehmite, the deionized water, the seed crystal and the dispersing agent are mixed, the materials are placed into a container, the materials are stirred by a stirrer and are subjected to primary mixing, the mixing performance of the materials is improved, and the PH is detected after the acid is added conveniently.
6. A process for the production of heavy rhombohedral boehmite according to claim 1, characterized in that: the acid includes sulfuric acid, nitric acid, hydrochloric acid, and glacial acetic acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115353133A (en) * | 2022-09-02 | 2022-11-18 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
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| CN115353133A (en) * | 2022-09-02 | 2022-11-18 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
| CN115353133B (en) * | 2022-09-02 | 2023-12-26 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
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