CN114560485A - Preparation method of superfine alumina - Google Patents
Preparation method of superfine alumina Download PDFInfo
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- CN114560485A CN114560485A CN202210414639.9A CN202210414639A CN114560485A CN 114560485 A CN114560485 A CN 114560485A CN 202210414639 A CN202210414639 A CN 202210414639A CN 114560485 A CN114560485 A CN 114560485A
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- organic solvent
- aluminum
- alumina
- saturated fatty
- ultrafine alumina
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [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 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 238000009835 boiling Methods 0.000 claims abstract description 9
- 150000007824 aliphatic compounds Chemical class 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 5
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 5
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 2
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 2
- 229940009827 aluminum acetate Drugs 0.000 claims description 2
- 229940063655 aluminum stearate Drugs 0.000 claims description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical class C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- 235000021314 Palmitic acid Nutrition 0.000 claims 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 239000002135 nanosheet Substances 0.000 abstract description 9
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 230000001276 controlling effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 8
- -1 aluminum alkoxide Chemical class 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- WJYIASZWHGOTOU-UHFFFAOYSA-N Heptylamine Chemical compound CCCCCCCN WJYIASZWHGOTOU-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229940043279 diisopropylamine Drugs 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
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
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
- C01F7/36—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts from organic aluminium salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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
- C01F7/308—Thermal decomposition of nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- 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
Abstract
The invention discloses a preparation method of superfine alumina, which comprises the steps of mixing an aluminum source and an organic solvent, and reacting at 180-300 ℃ to obtain the superfine alumina; the organic solvent is a saturated aliphatic compound with the boiling point not lower than the reaction temperature. According to the invention, a pure saturated aliphatic compound with a boiling point not lower than the reaction temperature is used as an organic solvent for regulating and controlling the reaction, and the regulation and control effects of the organic solvent on the size and the dispersity of alumina can be fully exerted, so that the uniform-size ultrafine alumina nano-particles with the particle size range of 1-10 nm or the uniform-size ultrafine alumina nano-sheets with the thickness range of 1-10 nm are prepared.
Description
Technical Field
The invention relates to a preparation method of superfine alumina, belonging to the technical field of alumina preparation.
Background
Alumina (Al)2O3) The block alumina has excellent performances of high temperature resistance, wear resistance, corrosion resistance, high hardness, high stability and the like, wherein the crystal structure and the electronic structure on the surface of the superfine alumina are changed, and the block alumina has the characteristics of ultrahigh specific surface area, size effect and the like which are not possessed by the block alumina, is widely applied to the fields of metallurgy, aerospace, electronic devices, chemical industry, biology and the like, and has wide market prospect.
Decomposing the precursor salt of the aluminum element in an organic solvent to obtain the aluminum oxide, which is a brand new preparation method of the superfine aluminum oxide. In the process, one end of the organic solvent is adsorbed on the surface of the generated alumina crystal nucleus to form an organic protective layer, so that the alumina particles or the nanosheets are effectively prevented from further growing up.
For example, CN 106348324a discloses a production process of ultrafine alumina polishing powder, which mainly comprises the following steps: adding polyethylene glycol and a dispersant consisting of one of ethylenediamine, n-heptylamine, dodecylamine or hexadecylamine into the polyethylene glycol, uniformly mixing the polyethylene glycol and an aluminum salt aqueous solution, adjusting the pH value to obtain an aluminum hydroxide precipitate, and then calcining and crushing the aluminum hydroxide precipitate to obtain the aluminum oxide polishing powder with the central particle size of less than 0.5 mu m.
For example, CN 100443409A discloses a highly pure and ultrafine alpha-Al with good dispersibility2O3The preparation method mainly comprises the following production steps: adding one or more additives selected from stearic acid, lauric acid, glacial acetic acid, citric acid, oxalic acid, polyethylene glycol, diisopropylamine, and tween-80 during hydrolysis of aluminum alkoxide to obtain aluminum oxide precursor, adding alpha-Al2O3Ball milling, drying and calcining the seed crystal to obtain alpha-Al with the average particle size of 100-170 nm2O3And (3) powder.
For another example, CN 113830809 a invented a method for preparing ultrafine alumina powder and its product, the production steps mainly include: and forming a dispersing agent by polyvinylpyrrolidone with different average molecular weights and sodium dodecyl sulfate, adding ethylene glycol, adding aluminum nitrate, reacting to obtain a precipitate, and calcining to obtain the superfine alumina powder with the particle size of 50-150 nm.
In the prior art disclosed in the patent, organic matters are used for regulating and controlling the size of alumina in the process of preparing ultrafine alumina, but main reactions are still carried out in an aqueous solution, the application of organic solvents is still insufficient, the particle size of the alumina is difficult to be effectively refined, the size dispersion level is difficult to be controlled, and the high-quality ultrafine alumina is obtained.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of ultrafine alumina, which comprises the steps of placing an aluminum source in a specific pure organic solvent, and carrying out heating reaction to obtain ultrafine alumina nanoparticles with the particle size range of 1-10 nm or ultrafine alumina nanosheets with the thickness range of 1-10 nm.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a preparation method of superfine alumina comprises the steps of mixing an aluminum source and an organic solvent, and reacting at 180-300 ℃ to obtain the superfine alumina; the organic solvent is a saturated aliphatic compound with the boiling point not lower than the reaction temperature.
Preferably, the aluminum source is one or more selected from aluminum acetylacetonate, aluminum isopropoxide, aluminum stearate, aluminum chloride, aluminum nitrate and aluminum acetate.
Preferably, the organic solvent is selected from at least one of saturated fatty amine, saturated fatty alcohol and saturated fatty acid having a boiling point not lower than the reaction temperature; more preferably, the organic solvent is at least one selected from the group consisting of saturated aliphatic amines having 8 to 36 carbon atoms, saturated aliphatic alcohols having 7 to 30 carbon atoms, and saturated fatty acids having 5 to 40 carbon atoms; more preferably, the organic solvent is at least one selected from saturated aliphatic amines having 10 to 20 carbon atoms, saturated aliphatic alcohols and saturated aliphatic acids. Such as dodecylamine, hexadecylamine, octadecylamine, dodecylalcohol, hexadecylalcohol, octadecylalcohol, dodecylacid, hexadecylacid, octadecylic acid, and the like.
Preferably, the mass ratio of the aluminum source to the organic solvent is 0.1-10.
In the existing preparation process of the superfine alumina, although the size of the alumina is regulated and controlled by organic matters, the main reactions are still carried out in aqueous solution, and the regulation and control functions of the organic matters cannot be fully exerted. The method adopts a pure saturated aliphatic compound with the boiling point not lower than the reaction temperature as an organic solvent for regulating and controlling the reaction, an aluminum source is decomposed under the pure organic solvent and the reaction temperature to obtain alumina crystal nuclei, and one end of the organic solvent is adsorbed on the surface of the generated alumina crystal nuclei to prevent alumina particles or nano sheets from further growing up, so that the superfine alumina is obtained. The key points of the invention are as follows: firstly, the organic solvent adopted by the invention is not lower than the reaction temperature and cannot boil at the reaction temperature; secondly, the organic solvent adopted by the method is a saturated aliphatic compound, and the polymerization failure in the reaction process can not occur, so that the regulation and control effects of the organic solvent on the size and the dispersity of the alumina can be fully exerted, and the superfine alumina nano-particles with the particle size range of 1-10 nm or the superfine alumina nano-sheets with the thickness range of 1-10 nm can be obtained.
The invention has the advantages that:
according to the invention, a pure saturated aliphatic compound with a boiling point not lower than the reaction temperature is used as an organic solvent for regulating and controlling the reaction, and the regulation and control effects of the organic solvent on the size and the dispersity of alumina can be fully exerted, so that the uniform-size ultrafine alumina nano-particles with the particle size range of 1-10 nm or the uniform-size ultrafine alumina nano-sheets with the thickness range of 1-10 nm are prepared.
Drawings
FIG. 1 is a TEM image of ultrafine alumina nanoparticles obtained in example 1;
fig. 2 is a TEM image of the ultrafine alumina nanosheets obtained in example 2.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The following specific examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Taking octadecylamine as an organic solvent, weighing acetylacetone aluminum and the organic solvent according to the mass ratio of 0.25:1, melting at 90 ℃, and uniformly stirring;
(2) heating the solution to 200 ℃ at the speed of 5 ℃/min, and reacting for 10 min;
(3) washing and centrifuging for 3 times when the reaction solution prepared in the step (2) is naturally cooled to 80 ℃;
(4) and (4) drying the sample collected in the step (3) at 80 ℃ for 4 hours in vacuum to obtain the superfine alumina nano particles.
As shown in FIG. 1, the particle size of the ultrafine alumina nanoparticles prepared in this example is in the range of 1 to 10 nm.
Example 2
(1) Taking a mixed solution of octadecylamine and octadecanoic acid with the mass ratio of 7:1 as an organic solvent, weighing the aluminum acetylacetonate and the organic solvent according to the mass ratio of 1:1, melting at 90 ℃, and uniformly stirring;
(2) heating the solution to 200 ℃ at the speed of 5 ℃/min, and reacting for 10 min;
(3) washing and centrifuging for 3 times when the reaction solution prepared in the step (2) is naturally cooled to 80 ℃;
(4) and (4) drying the sample collected in the step (3) at 80 ℃ for 4h in vacuum to obtain the superfine alumina nano sheet.
As shown in FIG. 2, the thickness of the ultra-fine alumina nano-sheet prepared by the present embodiment is in the range of 1-10 nm.
Comparative example 1
(1) Taking oleylamine as an organic solvent, weighing the aluminum acetylacetonate and the organic solvent according to the mass ratio of 0.1:1, melting at 90 ℃, and uniformly stirring;
(2) heating the solution to 200 ℃ at the speed of 5 ℃/min, and reacting for 10 min;
(3) and (3) when the reaction solution prepared in the step (2) is naturally cooled to 80 ℃, washing and centrifuging for 3 times to obtain viscous dark brown organic matter lumps which cannot be separated to obtain the aluminum oxide.
As can be seen from comparative example 1, pure oleylamine having a high boiling point as an organic solvent is very likely to be polymerized while decomposing an aluminum precursor due to the presence of unsaturated bonds such as carbon-carbon double bonds, and thus cannot be used for producing ultrafine alumina.
Comparative example 2
(1) Taking octadecylamine as an organic solvent, weighing acetylacetone aluminum and the organic solvent according to the mass ratio of 0.25:1, melting at 90 ℃, and uniformly stirring;
(2) heating the solution to 100 ℃ at the speed of 5 ℃/min, and reacting for 10 min;
(3) and (3) when the reaction solution prepared in the step (2) is naturally cooled to 80 ℃, washing and centrifuging, and no precipitate is generated.
Claims (7)
1. A preparation method of superfine alumina is characterized by comprising the following steps: mixing an aluminum source and an organic solvent, and reacting at 180-300 ℃ to obtain superfine alumina; the organic solvent is a saturated aliphatic compound with the boiling point not lower than the reaction temperature.
2. The method for preparing ultrafine alumina according to claim 1, wherein: the aluminum source is one or more of aluminum acetylacetonate, aluminum isopropoxide, aluminum stearate, aluminum chloride, aluminum nitrate and aluminum acetate.
3. The method for preparing ultrafine alumina according to claim 1, wherein: the organic solvent is at least one selected from saturated fatty amine, saturated fatty alcohol and saturated fatty acid with the boiling point not lower than the reaction temperature.
4. The method for preparing ultrafine alumina according to claim 3, wherein: the organic solvent is at least one selected from saturated aliphatic amine with 8-36 carbon atoms, saturated aliphatic alcohol with 7-30 carbon atoms and saturated fatty acid with 5-40 carbon atoms.
5. The method for preparing ultrafine alumina according to claim 4, wherein: the organic solvent is at least one selected from saturated fatty amine with 10-20 carbon atoms, saturated fatty alcohol and saturated fatty acid.
6. The method for preparing ultrafine alumina according to claim 5, wherein: the organic solvent is at least one selected from dodecylamine, hexadecylamine, octadecylamine, dodecanol, hexadecanol, octadecanol, dodecanoic acid, hexadecanoic acid and octadecanoic acid.
7. The method for preparing ultrafine alumina according to claim 1, wherein: the mass ratio of the aluminum source to the organic solvent is 0.1-10.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2022102774177 | 2022-03-19 | ||
| CN202210277417 | 2022-03-19 |
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| CN114560485A true CN114560485A (en) | 2022-05-31 |
| CN114560485B CN114560485B (en) | 2024-03-22 |
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