CN115057459B - Preparation method of composite nano alumina - Google Patents
Preparation method of composite nano alumina Download PDFInfo
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- CN115057459B CN115057459B CN202210881044.4A CN202210881044A CN115057459B CN 115057459 B CN115057459 B CN 115057459B CN 202210881044 A CN202210881044 A CN 202210881044A CN 115057459 B CN115057459 B CN 115057459B
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- composite
- alumina
- aluminum
- hydrated
- water
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- 239000002131 composite material Substances 0.000 title claims abstract description 95
- 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 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002002 slurry Substances 0.000 claims abstract description 34
- 239000003513 alkali Substances 0.000 claims abstract description 29
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 17
- 239000003292 glue Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000005374 membrane filtration Methods 0.000 claims abstract description 8
- 238000001728 nano-filtration Methods 0.000 claims abstract description 8
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 8
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000011240 wet gel Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- -1 aluminum dipentaerythritol Chemical compound 0.000 claims description 11
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 9
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 claims description 8
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 8
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 8
- 150000001261 hydroxy acids Chemical class 0.000 claims description 8
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 claims description 7
- 229940082004 sodium laurate Drugs 0.000 claims description 7
- 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 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 5
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims description 5
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 4
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229940009827 aluminum acetate Drugs 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229920001470 polyketone Polymers 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 2
- UARGAUQGVANXCB-UHFFFAOYSA-N ethanol;zirconium Chemical compound [Zr].CCO.CCO.CCO.CCO UARGAUQGVANXCB-UHFFFAOYSA-N 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- UAEJRRZPRZCUBE-UHFFFAOYSA-N trimethoxyalumane Chemical compound [Al+3].[O-]C.[O-]C.[O-]C UAEJRRZPRZCUBE-UHFFFAOYSA-N 0.000 claims description 2
- OBROYCQXICMORW-UHFFFAOYSA-N tripropoxyalumane Chemical compound [Al+3].CCC[O-].CCC[O-].CCC[O-] OBROYCQXICMORW-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 2
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims 1
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000000352 supercritical drying Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- ATYZRBBOXUWECY-UHFFFAOYSA-N zirconium;hydrate Chemical compound O.[Zr] ATYZRBBOXUWECY-UHFFFAOYSA-N 0.000 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 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 1
- 229940070765 laurate Drugs 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of composite nano alumina, which comprises the steps of carrying out alcohol hydrolysis reaction on aluminum salt, adding a dispersing agent to disperse to obtain hydrated alumina slurry, and dissolving a composite substance in water to obtain a composite substance solution; carrying out hydrothermal reaction on the hydrated alumina slurry, a composite substance solution and alkali liquor to obtain a hydrated composite alumina slurry, and carrying out high-temperature high-pressure hydrothermal refinement to obtain a nano hydrated composite alumina slurry; aging the nano hydrated composite alumina slurry, performing solid-liquid separation, and performing ultrafiltration, nanofiltration, high-pressure reverse osmosis membrane filtration, water washing and solid-liquid separation to obtain purified composite nano alumina wet gel; drying the composite nano alumina wet glue, performing jet-grouting crushing and free-falling roasting on the dried powder to obtain a composite nano alumina finished product. The composite nano aluminum oxide prepared by the invention has uniform granularity, good granular feel, small granularity, good compositing property, higher compatibility and more stable application.
Description
Technical Field
The invention relates to a preparation method of composite nano aluminum oxide, and belongs to the technical field of nano material preparation.
Background
The nano aluminum oxide has the excellent characteristics of high strength, high hardness, corrosion resistance, high temperature resistance, oxidation resistance, good insulativity, large surface area and the like, and is widely applied to the fields of catalysis, ceramics, cutters, aerospace, functional materials and the like. The nano alumina is compounded with other materials, and the properties of the nano alumina doped with different elements are utilized, so that the performance and the application effect of the material can be greatly improved, and the nano alumina composite material can be widely applied in a plurality of fields.
The composite nano alumina material prepared by the prior art has poor compoundability and unstable performance, and limits the application effect, so a new preparation method of the composite nano alumina is needed.
Disclosure of Invention
Aiming at the defects, the invention provides a preparation method of composite nano aluminum oxide, which adopts the following technical scheme:
the preparation method of the composite nano alumina at least comprises the steps of:
the aluminum salt is subjected to alcohol hydrolysis reaction and added with a dispersing agent to be dispersed to obtain hydrated alumina slurry, wherein the amount of the dispersing agent is 1-10% of that of the aluminum salt, and the ratio of the aluminum salt to the water to the alcohol=1: (5-20): (0-50).
The composite material is dissolved in water to prepare composite material solution, the usage amount of the composite material is 2-30% of that of aluminum salt, and the ratio of the composite material to water is 1:6-30.
One or more of ammonia water, ethanolamine, cyclohexylamine and propanol amine are prepared into alkali liquor with the mass fraction of 10-30%.
The hydrated alumina slurry is subjected to hydrothermal reaction with a composite substance solution and alkali liquor to obtain the hydrated composite alumina slurry, and then the hydrated composite alumina slurry is subjected to high-temperature high-pressure hydrothermal refinement to obtain the nano hydrated composite alumina slurry.
And aging the nano-hydrated composite alumina slurry, performing solid-liquid separation, and performing ultrafiltration, nanofiltration, high-pressure reverse osmosis membrane filtration, water washing and solid-liquid separation to obtain the purified composite nano-alumina wet gel.
Drying the composite nano alumina wet glue, performing jet-grouting crushing and free-falling roasting on the dried powder to obtain a composite nano alumina finished product.
The aluminum salt is one or more of aluminum nitrate, aluminum acetate, aluminum ethoxide, aluminum chloride, aluminum methoxide, aluminum isopropoxide, aluminum propoxide, aluminum acetate, aluminum hexanoxide and aluminum dipentxide;
the dispersing agent is one or more of polyketone, laurate polyoxyethylene sodium hydroxy acid, polyethylene glycol and polyethylene oxide.
The composite substance is one or more of metasilicic acid, silicon tetrachloride, zirconium nitrate, zirconium acetate, zirconium ethoxide, zirconium isopropoxide, cerium nitrate, cerium acetate, butyl titanate, titanium ethoxide and titanium isopropoxide.
The alcohol is one or more of methanol, ethanol, propanol, isopropanol, butanol, dipentyl alcohol and hexanol.
Compared with the prior art, the invention has the beneficial effects that: the composite nano aluminum oxide prepared by the invention has uniform granularity, good granular feel, small granularity, good compositing property, higher compatibility and more stable application.
Drawings
FIG. 1 is an SEM image of composite nano-alumina of the present invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings and examples.
The preparation method of the composite nano alumina at least comprises the following steps of:
preparation of hydrated alumina slurry: slowly adding one or more of aluminum salts into a reaction kettle added with deionized water and alcohols, uniformly stirring, adding a dispersing agent, and fully and uniformly mixing to obtain hydrated alumina slurry; aluminum salt, water and alcohol=1: (5-20) and (0-50), and the amount of the dispersing agent is 1-10% of that of the aluminum salt.
Preparing a composite substance solution: dissolving one or more of the composite materials in water to obtain a composite material solution; the usage amount of the composite material is 2-30% of aluminum salt, and the composite material is 1:6-30.
Alkali liquor preparation: one or more of ammonia water, ethanolamine, cyclohexylamine and propanol amine are prepared into alkali liquor with the mass fraction of 10-30%.
Hydrothermal reaction: slowly adding alkali liquor into a hydrated alumina slurry reaction kettle, regulating the pH to 7-10, uniformly stirring, heating to 50-100 ℃, slowly adding a composite substance solution, simultaneously adding alkali liquor to keep the pH of a reaction solution to 7-10, and fully reacting for 1-50 hours in a stirring state at a temperature to obtain the hydrated composite alumina slurry.
High-temperature high-pressure hydrothermal refining: after the hydrothermal reaction is finished, slowly adding alkali liquor to adjust the PH to 8-11, heating to 150-200 ℃, keeping the pressure in the kettle to be 0.7-1 MPa, and fully reacting for 1-70 hours under the conditions of temperature, pressure and stirring to obtain the nano-hydrated composite alumina slurry.
Aging: after the high-temperature high-pressure hydrothermal refining reaction is finished, the temperature is reduced to 20-35 ℃, and the mixture is kept stand and aged for 10-70 hours.
Wet glue preparation: and (3) performing solid-liquid separation on the aged nano-hydrated composite alumina slurry, adding water for ultrafiltration, nanofiltration, high-pressure reverse osmosis membrane filtration, washing with water and performing solid-liquid separation, and repeating the above operations for a plurality of times to obtain the purified composite nano-alumina wet gel.
Preparing a composite nano aluminum oxide finished product: drying the composite nano alumina wet glue by one or more of supercritical, freezing or spray drying, and performing jet-grouting crushing and free-falling roasting on the dried powder at the roasting temperature of 500-1400 ℃ to obtain a composite nano alumina finished product.
Example 1:
adding water and ethanol into a reaction kettle, slowly adding aluminum ethoxide, stirring uniformly, adding polyketone and sodium laurate polyoxyethylene hydroxy acid, and fully and uniformly mixing to obtain hydrated alumina slurry; aluminum ethoxide: water: ethanol=1:8:1; sodium laurate polyoxyethylene hydroxy acid=2:1, the total added amount is 2% of aluminum ethoxide. Preparing metasilicic acid, zirconium acetate and water into a composite substance solution; the mass ratio of metasilicic acid to zirconium acetate to water is 0.5:0.5:6, and the ratio of the total amount of metasilicic acid to zirconium acetate to aluminum ethoxide is 1:15. Ammonia water is prepared into alkali liquor with the mass fraction of 10 percent.
Adding alkali liquor into a hydrated alumina slurry reaction kettle at a speed of 1.5kg/min, regulating the PH to be 8, uniformly stirring, heating to 80 ℃ at a speed of 2 ℃/min, adding a composite substance solution at a speed of 1.5kg/min, simultaneously adding alkali liquor to keep the PH at 8, keeping the temperature at 80 ℃, continuously stirring, and fully reacting for 20 hours. After the reaction, slowly adding alkali liquor to adjust the PH=9, heating to 170 ℃ at 2.5 ℃/min, maintaining the pressure in the kettle at 0.7MPa, and continuously stirring for 50 hours.
After the reaction is finished, the temperature is reduced to 20 ℃, and the mixture is kept stand and aged for 30 hours. And (3) performing solid-liquid separation after aging, adding water, adopting ultrafiltration, nanofiltration and high-pressure reverse osmosis membrane filtration, washing with water and performing solid-liquid separation, and repeating the operation for a plurality of times to obtain the composite nano alumina wet gel.
And (3) carrying out supercritical drying on the composite nano alumina wet glue, crushing the wet glue by adopting a jet-grouting jet mill after drying, and roasting the wet glue by adopting a free-falling roasting furnace after crushing at a roasting temperature of 800 ℃ to obtain a composite nano alumina finished product.
The free-falling roasting furnace is a vertical roasting furnace, and the free-falling roasting means that the powder is quickly roasted in the roasting furnace in a free-falling movement mode.
Example 2:
adding water and propanol into a reaction kettle, slowly adding aluminum nitrate, stirring uniformly, adding sodium laurate polyoxyethylene hydroxy acid and polyethylene glycol, and fully and uniformly mixing to obtain hydrated alumina slurry; aluminum nitrate: water: propanol=1:9:2; sodium laurate polyoxyethylene hydroxy acid: polyethylene glycol=1:3, the total added amount is 4% of aluminum nitrate. Preparing a composite substance solution from cerium nitrate, titanium ethoxide and water; the mass ratio of the cerium nitrate to the titanium ethoxide to the water is 1:0.5:4, and the ratio of the total amount of the cerium nitrate and the titanium ethoxide to the aluminum nitrate is 1:16. Preparing alkali liquor with the mass fraction of 15% from ethanolamine.
Adding alkali liquor into a hydrated alumina slurry reaction kettle at a speed of 1.5kg/min, regulating the PH value to be 8.5, uniformly stirring, heating to 90 ℃ at a speed of 2 ℃/min, adding a composite substance solution at a speed of 1.5kg/min, simultaneously adding the alkali liquor to keep the PH value to be 8.5, keeping the temperature at 90 ℃, continuously stirring, and fully reacting for 30 hours. After the reaction, slowly adding alkali liquor to adjust the PH=9, heating to 180 ℃ at 2.5 ℃/min, maintaining the pressure in the kettle at 0.8MPa, and continuously stirring for 40 hours.
After the reaction is finished, the temperature is reduced to 20 ℃, and the mixture is kept stand and aged for 20 hours. And (3) performing solid-liquid separation after aging, adding water, adopting ultrafiltration, nanofiltration and high-pressure reverse osmosis membrane filtration, washing with water and performing solid-liquid separation, and repeating the operation for a plurality of times to obtain the composite nano alumina wet gel.
And (3) carrying out supercritical drying on the composite nano alumina wet glue, crushing the wet glue by adopting a jet-grouting jet mill after drying, and roasting the wet glue by adopting a free-falling roasting furnace after crushing at a roasting temperature of 900 ℃ to obtain a composite nano alumina finished product.
Example 3:
adding water and hexanol into a reaction kettle, slowly adding aluminum chloride, stirring uniformly, adding sodium laurate polyoxyethylene hydroxy acid, polyethylene glycol and polyethylene silica, and fully and uniformly mixing to obtain hydrated alumina slurry; aluminum chloride: water: hexanol=1:7:3; sodium laurate polyoxyethylene hydroxy acid, polyethylene glycol, polyethylene silica=1:1:1, the total amount added being 5% of aluminum chloride. Silicon tetrachloride, zirconium acetate and water are prepared into a composite substance solution; the mass ratio of the silicon tetrachloride to the zirconium acetate to the water is 1:1:6.5, and the ratio of the total amount of the silicon tetrachloride to the zirconium acetate to the aluminum chloride is 1:17. Ammonia water is prepared into alkali liquor with the mass fraction of 15 percent.
Adding alkali liquor into a hydrated alumina slurry reaction kettle at a speed of 1.5kg/min, regulating the PH to be 8, uniformly stirring, heating to 70 ℃ at a speed of 2 ℃/min, adding a composite substance solution at a speed of 1.5kg/min, simultaneously adding the alkali liquor to keep the PH at 7, keeping the 70 ℃, continuously stirring, and fully reacting for 50 hours. After the reaction, slowly adding alkali liquor to adjust the PH=9, heating to 170 ℃ at 2.5 ℃/min, maintaining the pressure in the kettle at 0.8MPa, and continuously stirring for 60 hours.
After the reaction is finished, the temperature is reduced to 20 ℃, and the mixture is kept stand and aged for 40 hours. And (3) performing solid-liquid separation after aging, adding water, adopting ultrafiltration, nanofiltration and high-pressure reverse osmosis membrane filtration, washing with water and performing solid-liquid separation, and repeating the operation for a plurality of times to obtain the composite nano alumina wet gel.
And (3) carrying out supercritical drying on the composite nano alumina wet glue, crushing the wet glue by adopting a jet-grouting jet mill after drying, and roasting the wet glue by adopting a free-falling roasting furnace after crushing at a roasting temperature of 1100 ℃ to obtain a composite nano alumina finished product.
FIG. 1 is an SEM image of composite nano-alumina of the present invention, and it can be seen from the image that the composite nano-alumina prepared by the present invention has the characteristics of small particles, uniform particles, etc.; in the figure, the considerable powder is similar to round particles, the particle size is about 20nm, and the particle size distribution is relatively uniform.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles of the invention, such changes and modifications are also intended to be within the scope of the invention.
Claims (4)
1. The preparation method of the composite nano alumina is characterized in that the composite nano alumina is at least compounded with one or more elements of silicon, zirconium, cerium and titanium, and the preparation method is as follows:
slowly adding one or more of aluminum salts into a reaction kettle added with deionized water and alcohols, uniformly stirring, adding a dispersing agent, and fully and uniformly mixing to obtain hydrated alumina slurry; aluminum salt, water and alcohol=1: (5-20): (0-50), and the amount of the dispersing agent is 1-10% of that of the aluminum salt; dissolving a composite material in water to prepare a composite material solution, wherein the usage amount of the composite material is 2-30% of that of aluminum salt, and the ratio of the composite material to water is 1:6-30; preparing 10-30% alkali liquor by mass of one or more of ammonia water, ethanolamine, cyclohexylamine and propanolamine;
slowly adding alkali liquor into a hydrated alumina slurry reaction kettle, regulating the pH to 7-10, uniformly stirring, heating to 50-100 ℃, slowly adding a composite substance solution, simultaneously adding alkali liquor to keep the pH of a reaction solution to 7-10, and fully reacting for 1-50 hours in a stirring state at a maintained temperature to obtain a hydrated composite alumina slurry; after the hydrothermal reaction is finished, slowly adding alkali liquor to adjust the PH to 8-11, heating to 150-200 ℃, keeping the pressure in the kettle to be 0.7-1 MPa, and fully reacting for 1-70 hours in the state of temperature, pressure and stirring to obtain nano-hydrated composite alumina slurry;
aging the nano hydrated composite alumina slurry, performing solid-liquid separation, and performing ultrafiltration, nanofiltration, high-pressure reverse osmosis membrane filtration, water washing and solid-liquid separation to obtain purified composite nano alumina wet gel;
drying the composite nano alumina wet glue, performing jet-grouting crushing and free-falling roasting on the dried powder to obtain a composite nano alumina finished product;
the aluminum salt is one or more of aluminum nitrate, aluminum acetate, aluminum ethoxide, aluminum chloride, aluminum methoxide, aluminum propoxide, aluminum hexanoxide and aluminum dipentaerythritol;
the composite substance is one or more of metasilicic acid, silicon tetrachloride, zirconium nitrate, zirconium acetate, zirconium ethoxide, zirconium isopropoxide, cerium nitrate, cerium acetate, butyl titanate, titanium ethoxide and titanium isopropoxide.
2. The preparation method of the composite nano-alumina according to claim 1, which is characterized by comprising the following steps:
preparation of hydrated alumina slurry: slowly adding one or more of aluminum salts into a reaction kettle added with deionized water and alcohols, uniformly stirring, adding a dispersing agent, and fully and uniformly mixing to obtain hydrated alumina slurry; aluminum salt, water and alcohol=1: (5-20): (0-50), and the amount of the dispersing agent is 1-10% of that of the aluminum salt;
preparing a composite substance solution: dissolving one or more of the composite materials in water to obtain a composite material solution; the usage amount of the composite material is 2-30% of aluminum salt, and the composite material is water=1: (6-30);
alkali liquor preparation: preparing 10-30% alkali liquor by mass of one or more of ammonia water, ethanolamine, cyclohexylamine and propanolamine;
hydrothermal reaction: slowly adding alkali liquor into a hydrated alumina slurry reaction kettle, regulating the pH to 7-10, uniformly stirring, heating to 50-100 ℃, slowly adding a composite substance solution, simultaneously adding alkali liquor to keep the pH of a reaction solution to 7-10, and fully reacting for 1-50 hours in a stirring state at a maintained temperature to obtain a hydrated composite alumina slurry;
high-temperature high-pressure hydrothermal refining: after the hydrothermal reaction is finished, slowly adding alkali liquor to adjust the PH to 8-11, heating to 150-200 ℃, keeping the pressure in the kettle to be 0.7-1 MPa, and fully reacting for 1-70 hours in the state of temperature, pressure and stirring to obtain nano-hydrated composite alumina slurry;
aging: after the high-temperature high-pressure hydrothermal refining reaction is finished, the temperature is reduced to 20-35 ℃, and the mixture is kept stand and aged for 10-70 hours;
wet glue preparation: performing solid-liquid separation on the aged nano-hydrated composite alumina slurry, adding water for ultrafiltration, nanofiltration, high-pressure reverse osmosis membrane filtration, washing with water and performing solid-liquid separation, and repeating the above operations for multiple times to obtain purified composite nano-alumina wet gel;
preparing a composite nano aluminum oxide finished product: drying the composite nano alumina wet glue by one or more of supercritical, freezing or spray drying, and performing jet-grouting crushing and free-falling roasting on the dried powder at the roasting temperature of 500-1400 ℃ to obtain a composite nano alumina finished product.
3. The method for preparing composite nano alumina according to claim 1 or 2, wherein the dispersing agent is one or more of polyketone, sodium laurate polyoxyethylene hydroxy acid, polyethylene glycol and polyethylene oxide.
4. The method for preparing composite nano alumina according to claim 1 or 2, wherein the alcohol is one or more of methanol, ethanol, propanol, butanol, dipentaerythritol and hexanol.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4769351A (en) * | 1986-05-06 | 1988-09-06 | Chichibu Cement Co., Ltd. | Hydrothermal process for preparing zirconia-alumina base ultra-fine powders of high purity |
| RU2142412C1 (en) * | 1998-12-29 | 1999-12-10 | Копеин Олег Ремович | Zeolite x production method |
| KR20030083024A (en) * | 2002-04-18 | 2003-10-30 | 한국화학연구원 | Process for forming the alumina powders |
| JP2007055888A (en) * | 2005-07-25 | 2007-03-08 | Sumitomo Chemical Co Ltd | FINE alpha-ALUMINA PARTICLE |
| CN102583476A (en) * | 2012-01-10 | 2012-07-18 | 长春工业大学 | Method for preparing mesoporous gamma-Al2O3 by dynamic hydrothermal method |
| CN102659149A (en) * | 2012-02-28 | 2012-09-12 | 山东大学 | Preparation method for monodisperse high-purity alpha-Al2O3 powder |
| CN104085899A (en) * | 2014-07-24 | 2014-10-08 | 山东科技大学 | Template-free hydrothermal synthesis method of small crystal ZSM-5 molecular sieve |
| CN104445309A (en) * | 2013-09-17 | 2015-03-25 | 中国石油化工股份有限公司 | High-purity aluminium oxide and preparation method thereof |
| CN104492473A (en) * | 2014-12-30 | 2015-04-08 | 华东理工大学 | Molecular sieve-coating cerium oxide composite material and preparation method thereof |
| CN109704731A (en) * | 2019-03-15 | 2019-05-03 | 中南大学 | A kind of preparation method of the stable Zirconia-alumina composite powder of nanometer of yttrium |
| RU2740748C1 (en) * | 2020-04-03 | 2021-01-20 | Федеральное государственное бюджетное учреждение науки Физико-технологический институт им. А.Ф. Иоффе Российской академии наук | Method of producing hollow microspheres of aluminium oxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050029198A1 (en) * | 2003-08-08 | 2005-02-10 | Frederick Tepper | Heavy metals absorbent and method of use |
-
2022
- 2022-07-26 CN CN202210881044.4A patent/CN115057459B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4769351A (en) * | 1986-05-06 | 1988-09-06 | Chichibu Cement Co., Ltd. | Hydrothermal process for preparing zirconia-alumina base ultra-fine powders of high purity |
| RU2142412C1 (en) * | 1998-12-29 | 1999-12-10 | Копеин Олег Ремович | Zeolite x production method |
| KR20030083024A (en) * | 2002-04-18 | 2003-10-30 | 한국화학연구원 | Process for forming the alumina powders |
| JP2007055888A (en) * | 2005-07-25 | 2007-03-08 | Sumitomo Chemical Co Ltd | FINE alpha-ALUMINA PARTICLE |
| CN102583476A (en) * | 2012-01-10 | 2012-07-18 | 长春工业大学 | Method for preparing mesoporous gamma-Al2O3 by dynamic hydrothermal method |
| CN102659149A (en) * | 2012-02-28 | 2012-09-12 | 山东大学 | Preparation method for monodisperse high-purity alpha-Al2O3 powder |
| CN104445309A (en) * | 2013-09-17 | 2015-03-25 | 中国石油化工股份有限公司 | High-purity aluminium oxide and preparation method thereof |
| CN104085899A (en) * | 2014-07-24 | 2014-10-08 | 山东科技大学 | Template-free hydrothermal synthesis method of small crystal ZSM-5 molecular sieve |
| CN104492473A (en) * | 2014-12-30 | 2015-04-08 | 华东理工大学 | Molecular sieve-coating cerium oxide composite material and preparation method thereof |
| CN109704731A (en) * | 2019-03-15 | 2019-05-03 | 中南大学 | A kind of preparation method of the stable Zirconia-alumina composite powder of nanometer of yttrium |
| RU2740748C1 (en) * | 2020-04-03 | 2021-01-20 | Федеральное государственное бюджетное учреждение науки Физико-технологический институт им. А.Ф. Иоффе Российской академии наук | Method of producing hollow microspheres of aluminium oxide |
Non-Patent Citations (2)
| Title |
|---|
| 不同晶型纳米Al_2O_3的制备及其对环氧树脂耐磨性能的影响;芳;李巧玲;陈贝;张佳裕;;精细化工中间体(05);全文 * |
| 醇盐水解-水热法制备高结晶度纳米氢氧化铝;江琦等;材料导报;第第22卷卷;第23-25页 * |
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