CN107285352A - The preparation method and applications of nano aluminium oxide - Google Patents
The preparation method and applications of nano aluminium oxide Download PDFInfo
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- CN107285352A CN107285352A CN201710441962.4A CN201710441962A CN107285352A CN 107285352 A CN107285352 A CN 107285352A CN 201710441962 A CN201710441962 A CN 201710441962A CN 107285352 A CN107285352 A CN 107285352A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000001694 spray drying Methods 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000010304 firing Methods 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims description 15
- 238000000967 suction filtration Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 4
- 239000003349 gelling agent Substances 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 9
- 238000012545 processing Methods 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 abstract 3
- 239000000047 product Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 12
- 238000005245 sintering Methods 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
-
- C—CHEMISTRY; METALLURGY
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Cell Separators (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to aluminum oxide preparing technical field, more particularly to a kind of preparation method of nano aluminium oxide.The preparation method at least comprises the following steps：Step S01, by aluminium hydroxide carry out cleaning removal of impurities processing；Step S02, suspension is made in the obtained aluminium hydroxides of step S01, then carries out spray drying treatment, firing is handled in 1100 DEG C~1200 DEG C；Or, the obtained aluminium hydroxides of step S01 are heated, then by ball-milling treatment.This preparation method technique is simple, and the reaction time is short, and technique is controllable, size tunable, product purity be up to 99.9% and more than, obtained nano aluminium oxide particle diameter reaches D50 ＜ 800nm levels.The nano aluminium oxide that this method is prepared can be used in lithium ion battery ceramic diaphragm.
Description
Technical Field
The invention relates to the technical field of preparation of aluminum oxide, in particular to a preparation method and application of nano aluminum oxide.
Background
With the continuous development of social industry, in recent years, the problems of environmental pollution, non-renewable energy shortage and the like in some large cities and heavy industrial cities are not remarkable, so that the development of green energy and the reasonable application of resources become important development directions.
The aluminum-air battery is a new energy battery with high energy density, and has the specific structure that aluminum alloy is used as a battery cathode, sodium hydroxide solution is used as electrolyte, oxygen is used as a battery anode, oxygen in the air is taken in during operation, and the aluminum alloy cathode is continuously consumed and generates Al (OH) during battery discharge3. In addition, fuel cells are made using hydrogen, a source of hydrogen in the aluminum metal industry which has a high commercial valueThe hydrogen route, which is also a process route with the formation of aluminum hydroxide as a by-product. In principle, aluminum hydroxide can be pyrolyzed to aluminum oxide, which can be used as a coating layer of a lithium battery separator to provide insulation, thermal insulation, and high temperature resistance. Thus, chemical treatment processes can be used to convert aluminum hydroxide to high purity alumina.
The prior methods for preparing high-purity aluminum oxide include a neutralization precipitation method, a hydrothermal synthesis method, a hydrolysis reaction of active aluminum powder, an inorganic aluminum salt sol-gel method and the like. The neutralization precipitation method comprises the steps of dissolving aluminum hydroxide into concentrated sulfuric acid, adding water for dilution, neutralizing with ammonia water, controlling the neutralization speed, stirring strongly at 40 ℃, adding an additive when the pH is 2, filtering with activated carbon, adding the additive into filtrate, neutralizing until the pH is 4.5, obtaining an aluminum hydroxide colloid, and then calcining, wherein the process is relatively complex; the temperature of the hydrothermal synthesis method can only reach about 400 ℃ generally, and the lowest temperature for converting aluminum hydroxide into aluminum oxide needs 450 ℃ or above, so that the cost is high on one hand, and certain dangerousness is realized on the other hand; the activity and granularity of the active aluminum powder to the aluminum powder need to be sprayed by overheating the molten metal to 200-300 ℃ in a quenching atomization device (the cooling rate is 105-107K/s) to obtain the active aluminum powder with the average granularity of 5-10 um, and the experimental conditions are strict.
Disclosure of Invention
Aiming at the problems of high requirements on raw materials, complex preparation process, high cost and the like in the method for preparing high-purity alumina in the prior art, the preparation method and the application of the nano-alumina are provided.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of nano alumina at least comprises the following steps:
step S01, cleaning and impurity removing the aluminum hydroxide;
step S02, preparing the aluminum hydroxide obtained in the step S01 into suspension, then carrying out spray drying treatment, and then carrying out firing treatment at 1100-1200 ℃; or,
and (4) heating the aluminum hydroxide obtained in the step (S01), and then performing ball milling treatment.
The preparation method of the nano-alumina provided by the invention has the advantages of simple process, short reaction time, controllable process and controllable particle size, the purity of the product is up to 99.9% or more, and the particle size of the obtained nano-alumina reaches the level that D50 is less than 800 nm.
The nano-alumina prepared by the preparation method of the nano-alumina can be used in a ceramic diaphragm of a lithium ion battery, and the nano-alumina is coated on the surface of the ceramic diaphragm, so that the performance of the ceramic diaphragm can be improved, and the recycling of aluminum resources can be optimized.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of nano aluminum oxide.
The preparation method of the nano alumina at least comprises the following steps:
step S01, cleaning and impurity removing the aluminum hydroxide;
step S02, preparing the aluminum hydroxide obtained in the step S01 into suspension, then carrying out spray drying treatment, and then carrying out firing treatment at 1100-1200 ℃; or,
and (4) heating the aluminum hydroxide obtained in the step (S01), and then performing ball milling treatment.
In a preferred embodiment, the aluminum hydroxide raw material is a product aluminum hydroxide obtained after the aluminum-air battery discharges or a byproduct aluminum hydroxide generated by the aluminum metal hydrogen production, and the discharge product or the hydrogen production product of the aluminum-air battery is used as the raw material, so that the recovery and utilization rate of aluminum resources can be effectively improved.
Preferably, the step of cleaning and impurity removing the aluminum hydroxide comprises adding a strongly acidic inorganic acid solution, such as a nitric acid solution and a hydrochloric acid solution, into the aluminum hydroxide, adjusting the pH value to 5.0-6.0, removing impurities in the aluminum hydroxide, performing suction filtration, and performing suction filtration repeatedly with distilled water to obtain an aluminum hydroxide precipitate.
In order to enable the suction filtration effect to be better, suction filtration is preferably carried out for 3-5 times.
Through the cleaning and impurity removing treatment in the step S01, impurities and oil stains contained in the aluminum hydroxide can be removed, and the negative influence on the purity of the aluminum oxide in the following process is avoided.
Step S02 is two parallel processing modes, no matter spray drying and then firing processing or sectional heating processing and then ball milling processing, the purity of the product is as high as 99.9% and above, and the grain diameter of the obtained nano alumina reaches the level of D50 less than 800 nm.
Preferably, the solid content of the suspension is 40-50%, and at the solid content, the spray particles are uniform and fine, so that the specific surface area of the particles obtained by spray drying is large and the particles are convenient to fire.
Preferably, in the spray drying treatment, the tower inlet temperature of the spray dryer is 550-650 ℃, and the tower outlet temperature of the spray dryer is 110-150 ℃. In the spray drying process, a peristaltic pump is adopted to send the aluminum hydroxide suspension raw material into a tower, the flow is controlled to be 120-160 mL/min, the flow is larger than 160mL/min, drying is not delayed, the obtained particles are mutually adhered, granulation is not uniform, and when the flow is smaller than 120mL/min, equipment waste and energy consumption are caused.
Preferably, the aluminum hydroxide after the spray drying treatment is placed at 1100-1200 ℃ for firing treatment, and the firing treatment time is 1-2 h.
Preferably, the firing treatment is carried out using a muffle furnace.
Preferably, the heating treatment comprises the steps of firstly treating the aluminum hydroxide obtained in the step S01 at 110-200 ℃ for 1-2 h, cooling, then transferring to 600-800 ℃ for firing for 1-2 h, cooling, and then firing at 1100-1200 ℃ for 1-2 h. The aluminum hydroxide is firstly converted into gamma-alumina and then converted into alpha-alumina by the regulation and control of the sectional heating.
Preferably, the heating treatment is carried out using a muffle furnace.
Preferably, in the ball milling treatment, the ball milling rotating speed is controlled to be 200 r/min-400 r/min, and the ball milling time is controlled to be 1-3 h. The high-energy ball mill is adopted to refine the grain diameter of the alumina after the sectional heating treatment, so that the adhesion between grains is avoided.
According to the embodiment of the invention, the aluminum air battery or the aluminum metal hydrogen production reaction byproduct aluminum hydroxide is converted into the available nano-grade aluminum oxide in two ways, the process is simple, the reaction time is short, the process is controllable, the particle size is controllable, the product purity is as high as 99.9% or more, the particle size of the obtained nano-aluminum oxide reaches the level that D50 is less than 800nm, and the preparation method effectively improves the recycling of the aluminum air battery reaction product and the aluminum metal hydrogen production byproduct.
Correspondingly, the invention further provides an application of the nano alumina besides the preparation method of the nano alumina.
In one embodiment, the nano-alumina prepared by the method is used in a ceramic separator of a lithium ion battery.
The specific application method comprises the following steps: mixing the nano alumina with a gelling agent and a solvent to obtain nano alumina slurry, and coating the nano alumina slurry on the surface of the ceramic diaphragm.
Preferably, the gelling agent is polyvinylidene fluoride; the solvent is N-methyl pyrrolidone; the nano-alumina, the gel and the solvent are mixed according to the mass ratio of (4-6) to (90-94) to (1-2).
Preferably, the viscosity of the nano alumina slurry is 180-220 mpa.s.
In order to better illustrate the preparation method of nano alumina provided by the embodiment of the present invention, the following further illustrates the preparation method by the embodiment.
Example 1
(1) Adding 20g of aluminum hydroxide waste liquor generated by the aluminum-air battery into a nitric acid solution, and detecting by using pH test paper until the pH of the solution is 5;
(2) after the pH is qualified, carrying out suction filtration and cleaning for 5 times to obtain 7.56g of aluminum hydroxide;
(3) preparing a product obtained by suction filtration into a suspension with the solid content of 45%, putting the suspension into a spray drying tower, controlling the flow rate to be 150mL/min, controlling the temperature of the suspension entering the tower to be 550 ℃ and the temperature of the suspension leaving the tower to be 110 ℃, performing spray drying treatment, cooling the obtained aluminum hydroxide, sintering the aluminum hydroxide at 1100 ℃ for 2 hours after cooling to obtain 6.9g of high-purity aluminum oxide, and calculating to ensure that the recovery rate reaches 91.3%.
Example 2
(1) Adding 100g of aluminum hydroxide waste liquor generated by the aluminum-air battery into a nitric acid solution, adding water, and detecting by using pH test paper until the pH of the solution is 6;
(2) after the pH is qualified, carrying out suction filtration and cleaning for 8 times to obtain 53.1 aluminum hydroxide;
(3) preparing a product obtained by suction filtration into a suspension with the solid content of 45%, putting the suspension into a spray drying tower, controlling the tower entering temperature to be 650 ℃ and the tower exiting temperature to be 140 ℃, performing spray drying treatment, cooling the obtained aluminum hydroxide, sintering at 1200 ℃ for 1h after cooling to obtain 48g of high-purity aluminum oxide, and calculating to obtain the recovery rate of 90.4%.
Example 3
(1) Adding 20g of aluminum hydroxide waste liquid generated by the aluminum-air battery into a nitric acid solution, and detecting by using pH test paper until the pH of the solution is 5;
(2) after the pH is qualified, performing suction filtration and cleaning for 6 times to obtain 8.0g of aluminum hydroxide;
(3) putting the product obtained by suction filtration into a crucible, baking for 1h at 110 ℃, cooling to room temperature, continuing to sinter for 2h at 600 ℃ in the crucible, and then cooling; cooling to room temperature, heating to 1100 ℃, sintering for 2h, transferring a product obtained by sintering to a ball milling tank, and sintering the product according to the mass ratio: and (3) milling the zirconia balls in a ratio of 1:1 at a milling speed of 200r/min for 3h to obtain 7.5g of high-purity alumina, wherein the recovery rate reaches 93.8% by calculation.
Example 4
(1) Adding 100g of aluminum hydroxide waste liquid generated by the aluminum-air battery into a nitric acid solution, and detecting by using pH test paper until the pH of the solution is 6;
(2) after the pH is qualified, carrying out suction filtration and cleaning for 8 times to obtain 39.8g of aluminum hydroxide;
(3) putting the product obtained by suction filtration into a crucible, baking for 1h at 120 ℃, cooling to room temperature, continuing to sinter for 1.5h at 650 ℃ in the crucible, and then cooling; cooling to room temperature, heating to 1200 ℃, sintering for 1h, transferring a product obtained by sintering to a ball milling tank, and sintering the product according to the mass ratio: and (3) milling the zirconia balls at a speed of 1:3 and a milling speed of 400r/min for 1h to obtain 36g of high-purity alumina, wherein the recovery rate reaches 90.5 percent through calculation.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the nano alumina is characterized by at least comprising the following steps:
step S01, cleaning and impurity removing the aluminum hydroxide;
step S02, preparing the aluminum hydroxide obtained in the step S01 into suspension, then carrying out spray drying treatment, and then carrying out firing treatment at 1100-1200 ℃; or,
and (4) heating the aluminum hydroxide obtained in the step (S01), and then performing ball milling treatment.
2. The method for preparing nano alumina according to claim 1, wherein: the cleaning and impurity removing treatment comprises the steps of adding a strong-acid inorganic acid solution into aluminum hydroxide, adjusting the pH value to 5.0-6.0, and then carrying out repeated suction filtration treatment.
3. The method for preparing nano alumina according to any one of claims 1 to 2, wherein: in the spray drying treatment, the solid content of the suspension is 40-50%, the tower inlet temperature of the spray dryer is 550-650 ℃, the tower outlet temperature is 110-150 ℃, and the flow rate of spray drying is 120-160 mL/min.
4. The method for preparing nano alumina according to any one of claims 1 to 2, wherein: the heating treatment comprises the steps of firstly treating the aluminum hydroxide obtained in the step S01 at 110-200 ℃ for 1-2 h, cooling, transferring to 600-800 ℃ for firing for 1-2 h, cooling, and firing at 1100-1200 ℃ for 1-2 h.
5. The method for preparing nano alumina according to any one of claims 1 to 2, wherein: the ball milling rotation speed of the ball milling treatment is 200 r/min-400 r/min, and the ball milling time is 1-3 h.
6. The method for preparing nano alumina according to claim 1, wherein: the time of the firing treatment is 1-2 h.
7. The method for preparing nano alumina according to claim 2, wherein: and repeating the suction filtration treatment for 3-5 times.
8. The application of the nano aluminum hydroxide prepared by the preparation method of the nano aluminum oxide according to any one of claims 1 to 7 in ceramic diaphragms.
9. The use of nano-alumina as claimed in claim 8 in ceramic membranes, wherein: the application method comprises the steps of mixing the nano-alumina with a gelling agent and a solvent to obtain nano-alumina slurry, and then coating the nano-alumina slurry on the surface of the ceramic diaphragm.
10. Use of the nano alumina of claim 9 in a ceramic diaphragm, wherein: the gel is polyvinylidene fluoride; the solvent is N-methyl pyrrolidone; the nano-alumina, the gel and the solvent are mixed according to the mass ratio of (4-6) to (90-94) to (1-2).
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| CN201710441962.4A CN107285352A (en) | 2017-06-13 | 2017-06-13 | The preparation method and applications of nano aluminium oxide |
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| CN (1) | CN107285352A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408945A (en) * | 2019-07-29 | 2019-11-05 | 空天科技有限公司 | A kind of preparation method of alumina in Nano level |
| CN110844928A (en) * | 2019-12-06 | 2020-02-28 | 湖北工业大学 | Method for preparing micro-nano aluminum oxide from aluminum alloy hydrolysate |
| CN115764169A (en) * | 2022-12-29 | 2023-03-07 | 界首市天鸿新材料股份有限公司 | Beta-crystal-containing PP coating diaphragm |
| CN117800372A (en) * | 2024-01-03 | 2024-04-02 | 宁波国锋新材料科技有限公司 | A kind of high-purity nano-spherical aluminum oxide and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146973A (en) * | 1995-06-01 | 1997-04-09 | 王萍 | Process for production of nm. alumina |
| US20100326495A1 (en) * | 2005-07-19 | 2010-12-30 | Solyndra, Inc. | Self-cleaning protective coatings for use with photovoltaic cells |
| CN102583469A (en) * | 2012-03-09 | 2012-07-18 | 广州慧谷化学有限公司 | Industrial production method for superfine high-purity alpha-alumina |
| CN103708512A (en) * | 2013-12-11 | 2014-04-09 | 中国铝业股份有限公司 | Preparation method of submicron alumina |
| CN104229844A (en) * | 2014-09-12 | 2014-12-24 | 广西平果铝朗琨科技有限公司 | Preparation method of superfine low-sodium alpha-alumina powder with high activity |
| CN104993082A (en) * | 2015-06-01 | 2015-10-21 | 常州大学 | Preparation method for nano-alumina particle modified ceramic diaphragm |
-
2017
- 2017-06-13 CN CN201710441962.4A patent/CN107285352A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146973A (en) * | 1995-06-01 | 1997-04-09 | 王萍 | Process for production of nm. alumina |
| US20100326495A1 (en) * | 2005-07-19 | 2010-12-30 | Solyndra, Inc. | Self-cleaning protective coatings for use with photovoltaic cells |
| CN102583469A (en) * | 2012-03-09 | 2012-07-18 | 广州慧谷化学有限公司 | Industrial production method for superfine high-purity alpha-alumina |
| CN103708512A (en) * | 2013-12-11 | 2014-04-09 | 中国铝业股份有限公司 | Preparation method of submicron alumina |
| CN104229844A (en) * | 2014-09-12 | 2014-12-24 | 广西平果铝朗琨科技有限公司 | Preparation method of superfine low-sodium alpha-alumina powder with high activity |
| CN104993082A (en) * | 2015-06-01 | 2015-10-21 | 常州大学 | Preparation method for nano-alumina particle modified ceramic diaphragm |
Non-Patent Citations (5)
| Title |
|---|
| 丁亚茹: "《粉煤灰提取氧化铝生产》", 31 December 2013 * |
| 周书助: "《硬质材料与工具》", 31 August 2015 * |
| 周张健: "《无机非金属材料工艺学》", 31 January 2010 * |
| 曾贵玉: "《中国工程物理研究院科技丛书 微纳米含能材料》", 31 May 2015 * |
| 梁春来等: "中和法制备高纯超细氧化铝", 《轻金属》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408945A (en) * | 2019-07-29 | 2019-11-05 | 空天科技有限公司 | A kind of preparation method of alumina in Nano level |
| CN110844928A (en) * | 2019-12-06 | 2020-02-28 | 湖北工业大学 | Method for preparing micro-nano aluminum oxide from aluminum alloy hydrolysate |
| CN115764169A (en) * | 2022-12-29 | 2023-03-07 | 界首市天鸿新材料股份有限公司 | Beta-crystal-containing PP coating diaphragm |
| CN117800372A (en) * | 2024-01-03 | 2024-04-02 | 宁波国锋新材料科技有限公司 | A kind of high-purity nano-spherical aluminum oxide and preparation method thereof |
| CN117800372B (en) * | 2024-01-03 | 2025-01-21 | 宁波国锋新材料科技有限公司 | A kind of high-purity nano-spherical aluminum oxide and preparation method thereof |
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