CN111153421A - Large-specific-surface-area high-purity α -aluminum oxide and preparation method thereof - Google Patents
Large-specific-surface-area high-purity α -aluminum oxide and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 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 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000002105 nanoparticle Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 230000012010 growth Effects 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 230000036571 hydration Effects 0.000 claims abstract description 5
- 238000006703 hydration reaction Methods 0.000 claims abstract description 5
- 230000007246 mechanism Effects 0.000 claims abstract description 5
- 238000010899 nucleation Methods 0.000 claims abstract description 5
- 230000006911 nucleation Effects 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 12
- 238000010335 hydrothermal treatment Methods 0.000 claims description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 11
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 8
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 11
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000033228 biological regulation Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 2
- 239000013078 crystal Substances 0.000 description 18
- 239000002245 particle Substances 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 4
- 239000010431 corundum Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000033001 locomotion Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
- 229910006636 γ-AlOOH Inorganic materials 0.000 description 1
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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
- C01F7/021—After-treatment of oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
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- 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
- C01P2006/12—Surface area
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention relates to high-purity α -aluminum oxide with large specific surface area and a preparation method thereof, which adopts a solid hydrothermal method, in the hydrothermal synthesis route of aluminum oxide, the formation of a product follows the basic links of autogenous grinding, hydration, Hydrolysis, nucleation, crystallization, growth and the like, namely an autogenous grinding Hydrolysis crystallization mechanism (S-MHC), and the specific surface area of aluminum oxide nano-particles can reach 140 m2G-1. Adopts a solid oxide hydrothermal method, takes alumina as a reaction raw material, and synthesizes the surface area of about 140 m under the regulation and control action of a surfactant2High purity α -Al of g-12O3And (3) nanoparticles. The invention has simple process and mild preparation method, and the prepared nano-particle-Al2O3Can be directly used as a synthetic ammonia catalyst carrier without wash coating, and improves the catalytic activity.
Description
Technical Field
The invention relates to large-specific-surface-area high-purity α -aluminum oxide and a preparation method thereof, belonging to the field of material preparation.
Background
Nano Al2O3As an important nano material, the corundum (α -Al) has the advantages of large specific surface area, large pore volume, more surface active centers and the like, and is widely used as a catalyst carrier, a catalyst, an adsorbent and the like2O3) Highly mechanically stable, nanoparticulate α -Al2O3Can be used directly as a carrier without wash coating; the catalyst can be used as a carrier of a synthetic ammonia catalyst to improve the catalytic activity.
Corundum nanoparticles (α -Al) have been studied in the past in a few experiments2O3) Thermodynamics and synthesis methods. However, no one has been developed so far which can be used for preparing a surface area exceeding 100m2g-1A method for preparing high-purity corundum. The main reason is that the reaction needs to overcome the high activation energy barrier (485 kJ mol)-1) The reaction temperature is higher than 1473K so as to rearrange oxide ions from the cubic close-packed structure in the transition alumina into the hexagonal close-packed crystal form. Such transformations typically result in substantial mass transfer during the transformation process, which typically results in a loss of surface area.
At room temperature, gamma-Al2O3It may in fact be the thermodynamically most stable phase of the alumina nanoparticles, corresponding to 100 to 200 m2g-1Surface area of (a). At 800K, gamma-Al, even at lower surface areas2O3Thus, high temperature processes that tend to result in the formation of the most stable phase are never able to produce α -Al with high surface area2O3. Theoretical studies have shown that the surface energy of polymorphic alumina and its stability depend to a large extent on the size of the crystallites and the degree of hydroxylation. Thus, the resulting surface area is greater than 100m2g-1α -Al of2O3Is feasible, but α -Al is prepared by a high temperature process of 1500K2O3And was not successful.
In the oxide hydrothermal synthesis route, the formation of the product complies with the basic links of autogenous grinding, hydration, Hydrolysis, nucleation, crystallization, growth and the like, namely, the autogenous grinding Hydrolysis crystallization mechanism (S-MHC): (a) under the hydrothermal closed environment, under the promotion of high-speed thermal motion of water molecules, the alumina powder is mutually collided and rubbed among large oxide powder particles, so that the individual bodies are gradually reduced, and then the alumina powder is uniformly dispersed in a reaction system. In this process, each particle can be regarded as a pellet, and both substances are composed of an infinite number of pellets, and under the driving of water, countless ball milling rotors are formed, which are reactants per se. The dispersion process can be referred to visually as the Self-milling process (Self-milling). (b) As the particle size of the particles decreases, the surface energy of each particle rapidly increases and the activity of the surface particles increases, and in order to decrease the surface activity thereof, a large number of small particles and water molecules on the surface are hydrated to form a large number of hydrated ions (hydration process). (c) During the movement of the hydrated ions, further friction, collision, dehydration, rehydration, separation, crosslinking, etc. must occur, and when two hydrated ions collide or act with each other, dehydration (dehydration process) occurs to form γ -AlOOH molecules. (d) The number of gamma-AlOOH molecular molecules gradually increases to reach supersaturation and form crystal nuclei (nucleation process). (e) The formation of crystal nuclei is necessarily large, and these nuclei are gradually developed into microcrystals by a dissolution-sedimentation mechanism, accompanied by dissolution of small crystal grains and growth of large crystal grains, and finally grown into target crystals (crystal growth process).
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide α -alumina with large specific surface area and high purity.
The invention also aims to provide a preparation method of the high-purity α -alumina product with large specific surface area.
The invention aims to realize the purpose that the α -aluminum oxide with large specific surface area and high purity adopts a solid hydrothermal method and the formation of the product conforms to autogenous grinding, hydration, hydrolysis, nucleation, crystallization and growth in the hydrothermal synthesis route of the aluminum oxideThe basic links are as follows: the specific surface area of the alumina nano-particles can reach 140 m by an autogenous grinding Hydrolysis crystallization mechanism (S-MHC)2·g-1。
The invention also provides a preparation method of the high-purity α -alumina with large specific surface area, which adopts a solid hydrothermal method and comprises the following process steps:
(1) sequentially and respectively adding an alumina powder sample, a surfactant and deionized water into a clean polytetrafluoroethylene solution, wherein the surfactant is one or a combination of PEG400, PEG2000 or ethylenediamine; the mass ratio of the alumina powder to the surfactant is 1: 1-1: 2;
(2) placing the liner into an ultrasonic cleaner for dispersing for 10-20 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 373-473K for 12-36 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with a large specific surface area2O3And (3) nanoparticles.
In the step (1), the ratio of the added mass of the alumina to the total volume of the final reaction solution is 0.5 g/100 ml-5 g/100 ml.
The α -Al with large specific surface area and high purity is prepared by a low-temperature solid-state hydrothermal method2O3The alumina obtained by the above preparation method is α -Al2O3The crystal form is matched with a standard powder diffraction card (JCPDS: 10-173). The morphology is nano particles, the purity is more than 99 percent, and the specific surface area is about 140 m2G-1. The prepared rod-shaped bismuth oxide has higher specific surface area, higher purity and crystallinity, and wide application prospect in the fields of industrial catalysis, new materials and the like.
Adopts a solid oxide hydrothermal method, takes alumina as a reaction raw material, and synthesizes the surface area of about 140 m under the regulation and control action of a surfactant2High purity α -Al of g-12O3And (3) nanoparticles. The invention has simple process and mild preparation method, and the prepared nano-particle-Al2O3Can be directly used as a synthetic ammonia catalyst carrier without wash coating, and improves the catalytic activity.
Drawings
FIG. 1 Large specific surface area α -Al from example 12O3SEM image of (d).
Detailed Description
The invention is further illustrated by the following examples, which are intended only for a better understanding of the contents of the invention. The examples given therefore do not limit the scope of the invention.
Example 1
The α -alumina with large specific surface area and high purity is prepared by the following process steps:
(1) respectively adding 0.5 g of an alumina powder sample, 0.5 g of PEG400 and 100ml of deionized water into a clean polytetrafluoroethylene solution in sequence;
(2) placing the liner in an ultrasonic cleaner for dispersing for 20 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at 373 ℃ for 24 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3The SEM image of the nanoparticles is shown in figure 1.
Obtained α -Al2O3The crystal form of the crystal is matched with a standard powder diffraction card (JCPDS: 10-173), the appearance is nano particles, the particle size is about 50nm, the purity is more than 99 percent, and the specific surface area is 138 m2·g-1。
Example 2
The α -alumina with large specific surface area and high purity is prepared by the following process steps:
(1) sequentially and respectively adding 2.5 g of an alumina powder sample, 5 g of ethylenediamine and 100ml of deionized water into a clean polytetrafluoroethylene solution;
(2) placing the inner container in an ultrasonic cleaner for dispersing for 10 min;
(3) the inner container is put into a stainless steel reaction kettle to be sealed, and the high-pressure hydrothermal kettle is subjected to hydrothermal treatment 36 at the temperature of 473H, stopping the reaction, washing the precipitated product with deionized water, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
Obtained α -Al2O3The crystal form of the crystal is matched with a standard powder diffraction card (JCPDS: 10-173), the appearance is nano particles, the particle size is about 200nm, the purity is more than 99 percent, and the specific surface area is 102m2·g-1。
Example 3
The α -alumina with large specific surface area and high purity is prepared by the following process steps:
(1) sequentially and respectively adding 2 g of an alumina powder sample, 2 g of PEG2000 and 100ml of deionized water into a clean polytetrafluoroethylene solution;
(2) placing the inner container in an ultrasonic cleaner for dispersing for 15 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 403 for 12 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
Obtained α -Al2O3The crystal form of the crystal is matched with a standard powder diffraction card (JCPDS: 10-173), the appearance is nano particles, the particle size is about 80nm, the purity is more than 99 percent, and the specific surface area is 125 m2·g-1。
Example 4
The α -alumina with large specific surface area and high purity is prepared by the following process steps:
(1) sequentially and respectively adding 4 g of alumina powder sample, 3 g of PEG400, 1 g of PEG2000 and 100ml of deionized water into a clean polytetrafluoroethylene solution;
(2) placing the inner container in an ultrasonic cleaner for dispersing for 18 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at 373 ℃ for 36 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
Obtained α -Al2O3The crystal form of the crystal is matched with a standard powder diffraction card (JCPDS: 10-173), the appearance is nano particles, the particle size is about 80nm, the purity is more than 99 percent, and the specific surface area is 130 m2·g-1。
Example 5
The α -alumina with large specific surface area and high purity is prepared by the following process steps:
(1) respectively adding 3 g of an alumina powder sample, 2.5 g of PEG400, 1.5 g of ethylenediamine and 100ml of deionized water into a clean polytetrafluoroethylene solution in sequence;
(2) placing the liner in an ultrasonic cleaner for dispersing for 20 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 473 for 12 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
Obtained α -Al2O3The crystal form of the crystal is matched with a standard powder diffraction card (JCPDS: 10-173), the appearance is nano particles, the particle size is about 120nm, the purity is more than 99 percent, and the specific surface area is 117 m2·g-1。
Claims (8)
1. The α -aluminum oxide with large specific surface area and high purity is characterized in that a solid hydrothermal method is adopted, and the formation of the product follows the basic links of autogenous grinding, hydration, Hydrolysis, nucleation, crystallization and growth in an alumina hydrothermal synthesis route, namely, an autogenous grinding Hydrolysis crystallization mechanism (S-MHC), and the specific surface area of alumina nanoparticles can reach 140 m2·g-1。
2. The preparation method of high-specific surface area and high-purity α -alumina according to claim 1, wherein a solid-state hydrothermal method is adopted, comprising the following process steps:
(1) sequentially and respectively adding an alumina powder sample, a surfactant and deionized water into a clean polytetrafluoroethylene solution, wherein the surfactant is one or a combination of PEG400, PEG2000 or ethylenediamine; the mass ratio of the alumina powder to the surfactant is 1: 1-1: 2;
(2) placing the liner into an ultrasonic cleaner for dispersing for 10-20 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 373-473K for 12-36 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with a large specific surface area2O3And (3) nanoparticles.
3. The preparation method of high-specific surface area and high-purity α -alumina according to claim 2, wherein the ratio of the mass of alumina added in step (1) to the total volume of the final reaction solution is 0.5 g/100 ml to 5 g/100 ml.
4. The preparation method of α -alumina with large specific surface area and high purity according to claim 2 or 3, which is characterized by comprising the following steps:
(1) respectively adding 0.5 g of an alumina powder sample, 0.5 g of PEG400 and 100ml of deionized water into a clean polytetrafluoroethylene solution in sequence;
(2) placing the liner in an ultrasonic cleaner for dispersing for 20 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at 373 ℃ for 24 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
5. The preparation method of α -alumina with large specific surface area and high purity according to claim 2 or 3, which is characterized by comprising the following steps:
(1) sequentially and respectively adding 2.5 g of an alumina powder sample, 5 g of ethylenediamine and 100ml of deionized water into a clean polytetrafluoroethylene solution;
(2) placing the inner container in an ultrasonic cleaner for dispersing for 10 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 473 for 36 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
6. The preparation method of α -alumina with large specific surface area and high purity according to claim 2 or 3, which is characterized by comprising the following steps:
(1) sequentially and respectively adding 2 g of an alumina powder sample, 2 g of PEG2000 and 100ml of deionized water into a clean polytetrafluoroethylene solution;
(2) placing the inner container in an ultrasonic cleaner for dispersing for 15 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 403 for 12 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
7. The preparation method of α -alumina with large specific surface area and high purity according to claim 2 or 3, which is characterized by comprising the following steps:
(1) sequentially and respectively adding 4 g of alumina powder sample, 3 g of PEG400, 1 g of PEG2000 and 100ml of deionized water into a clean polytetrafluoroethylene solution;
(2) placing the inner container in an ultrasonic cleaner for dispersing for 18 min;
(3) placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at 373 ℃ for 36 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
8. The preparation method of α -alumina with large specific surface area and high purity according to claim 2 or 3, which is characterized by comprising the following steps:
(1) respectively adding 3 g of an alumina powder sample, 2.5 g of PEG400, 1.5 g of ethylenediamine and 100ml of deionized water into a clean polytetrafluoroethylene solution in sequence;
(2) placing the liner in an ultrasonic cleaner for dispersing for 20 min;
placing the inner container into a stainless steel reaction kettle, sealing, carrying out hydrothermal treatment on the high-pressure hydrothermal kettle at the temperature of 473 for 12 hours, washing a precipitation product with deionized water after stopping the reaction, and drying to obtain α -Al with large specific surface area2O3And (3) nanoparticles.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1712355A (en) * | 2004-06-15 | 2005-12-28 | 住友化学株式会社 | Method for producing an alpha - alumina powder |
| CN101182017A (en) * | 2007-12-17 | 2008-05-21 | 中国铝业股份有限公司 | Method for preparing sheet alumina powder |
| CN104386719A (en) * | 2014-10-31 | 2015-03-04 | 中国铝业股份有限公司 | Method for preparing alpha-aluminum oxide |
| CN108658107A (en) * | 2018-04-23 | 2018-10-16 | 上海大学 | A kind of nanometer-sized monodisperse spherical shape Alpha-alumina low cost preparation method and products thereof |
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2020
- 2020-03-05 CN CN202010146033.2A patent/CN111153421A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1712355A (en) * | 2004-06-15 | 2005-12-28 | 住友化学株式会社 | Method for producing an alpha - alumina powder |
| CN101182017A (en) * | 2007-12-17 | 2008-05-21 | 中国铝业股份有限公司 | Method for preparing sheet alumina powder |
| CN104386719A (en) * | 2014-10-31 | 2015-03-04 | 中国铝业股份有限公司 | Method for preparing alpha-aluminum oxide |
| CN108658107A (en) * | 2018-04-23 | 2018-10-16 | 上海大学 | A kind of nanometer-sized monodisperse spherical shape Alpha-alumina low cost preparation method and products thereof |
Non-Patent Citations (1)
| Title |
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| 李兆等: "一维纤维状α－Ａｌ２Ｏ３粉体的水热－热解法制备与表征", 《材料导报Ｂ：研究篇》 * |
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Application publication date: 20200515 |