CN1401575A - Method for mfg. nano alumina - Google Patents
Method for mfg. nano alumina Download PDFInfo
- Publication number
- CN1401575A CN1401575A CN 01124048 CN01124048A CN1401575A CN 1401575 A CN1401575 A CN 1401575A CN 01124048 CN01124048 CN 01124048 CN 01124048 A CN01124048 A CN 01124048A CN 1401575 A CN1401575 A CN 1401575A
- Authority
- CN
- China
- Prior art keywords
- alumina according
- preparing nano
- aluminum
- triton
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 9
- 239000012530 fluid Substances 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000000654 additive Substances 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 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
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical group [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- FCZYGJBVLGLYQU-UHFFFAOYSA-M sodium;2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethanesulfonate Chemical compound [Na+].CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCS([O-])(=O)=O)C=C1 FCZYGJBVLGLYQU-UHFFFAOYSA-M 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 2
- 229920004890 Triton X-100 Polymers 0.000 claims 1
- 239000013504 Triton X-100 Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229960003511 macrogol Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
A gamma-Al2O3 nanoparticle (less than 20 nm) is prepared through reverse sol-gel method, supercritical fluid drying method, and calcining at 900 deg.C for 2 hr. Its specific surface area is 140 sq.m/g.
Description
Technical field
The present invention relates to a kind of preparation method of nano-aluminium oxide.
Background technology
Aluminium sesquioxide (the Al that the present invention proposes
2O
3) be one of important source material of commercial catalysts, vehicle emission pollution cleaning catalyst, electronic industry and high-performance ceramics.
Nanometer Al
2O
3Particulate is active and most important in the catalytic field application, because nanometer Al
2O
3The particulate small-size effect, surface effects, aspects such as quantum size effect and macro quanta tunnel effect present the characteristic that conventional material does not possess, and at the catalysis ambit broad prospect of application are arranged.Nano particle is because size is little, and the shared percent by volume in surface is big, and the key attitude on surface is different with granule interior with electronic state, the not congruent active sites increase that causes the surface of surface atom coordination, and this just makes it possess supremacy clause as catalyzer.Nanometer Al
2O
3Particle is the collaborative speed of response that improves as the main effect of support of the catalyst, increases reaction efficiency; The decision response path has good selectivity; Reduce temperature of reaction.These characteristics and superiority are that other catalyzer is incomparable.
At present especially patent is rare that report arranged for the background technology of relevant this respect, can see having: CN1085187, CN1146973 and CN1079718.In these reports, relevant nanometer Al
2O
3The preparation method, generally adopting the soluble aluminum salts solution is raw material, is added drop-wise in the aluminum salt solution as precipitation agent with ammoniacal liquor.So the PH in the precipitin reaction process changes in time, uncontrollablely reacts the gel size distribution broad that finally makes in a fixed PH scope.And the present invention uses the reverse precipitation method, being distributed in certain scope of may command gel particle diameter.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano-aluminium oxide, the nano-aluminium oxide particle size that the present invention makes is little, and surperficial shared percent by volume is big.
It is raw material that nano-aluminium oxide preparation method provided by the invention adopts aluminum soluble salt, is made into certain concentration solution, is added drop-wise to then in the precipitation agent that contains emulsifying agent and additive and obtains gel, and through washing, supercritical fluid drying, roasting obtains Al
2O
3
The present invention adopts exsiccated ammonium alum, aluminum nitrate, aluminum chloride, pure metal aluminium flake or kaolin as preparation nanometer Al
2O
3Raw material, the soluble aluminum salt concn of above-mentioned raw materials preparation is 0.1-0.3mol/L; With ammoniacal liquor is precipitation agent, and its concentration is ammoniacal liquor: water=1: 3, emulsifying agent are triton x-100, Triton-155 or Triton 200, and add-on is 0.05-0.13vol% in above-mentioned precipitation agent; Additive is Macrogol 200 or Macrogol 1540, and add-on is 0.5-2.5vol% in above-mentioned precipitation agent; The temperature of reaction of preparation gel is 25-60 ℃, pH9-12; The ultra-fine grain that obtains can obtain being of a size of γ-Al of several-20nm through 900 ℃ of roastings
2O
3
Description of drawings
For further understanding the present invention, elaborate with embodiment below, and provide accompanying drawing and describe nanometer γ-Al that the present invention obtains
2O
3The characteristic present, wherein:
Fig. 1 is Al
2O
3X-diffraction (XRD) spectrogram of sample;
Fig. 2 is Al
2O
3The transmission electron microscope of sample (TEM) photo;
Fig. 3 is Al
2O
3The selected area electron diffraction photo of sample.
Embodiment
Embodiment 1: raw material is an exsiccated ammonium alum, the soluble aluminum salt concn that is mixed with is 0.1mol/L, and precipitation agent concentration is ammoniacal liquor: water=1: 3, get the 400ml precipitation agent, add emulsifying agent Triton 100 respectively, its add-on is 0.05vol%, and additives polyethylene glycol 200 is incorporated as 2.5vol%, 40 ℃ of powerful stirrings 15 minutes, drip soluble aluminum salts solution 1000ml, can get alumina hydrate gel solution, its pH is between 9-12; Gel ageing in mother liquor with the preparation gained, digestion time can be at 12-24 hour, present embodiment ageing 18 hours is suction filtration then, with deionized water wash 8-10 time, exchange water in the gel for several times with dehydrated alcohol, use the supercritical fluid drying drying, the ultra-fine grain that dry back obtains promptly obtains nanometer γ-Al 900 ℃ of roastings 2 hours
2O
3
Embodiment 2, raw material are aluminum nitrate, the soluble aluminum concentration of salt solution that is mixed with is 0.3mol/L, add Triton X-155 in the precipitation respectively, its add-on is 0.1vol%, and additives polyethylene glycol 1540 is incorporated as 0.5vol%, 40 ℃ of powerful stirrings 10 minutes, drip soluble aluminum salts solution 1000ml, can get alumina hydrate gel solution, its pH is between 9-12; 900 ℃ of roastings 4 hours.All the other are with embodiment 1.
Embodiment 3, raw material are aluminum chloride, and the soluble aluminum salt concn that is mixed with is 0.2mol/L, add Triton X-200 in the precipitation respectively, and its add-on is 0.13vol%, and additives polyethylene glycol 1540 is incorporated as 1.5vol%.All the other are with embodiment 1.
Embodiment 4, raw material are the metal aluminium flake.All the other are with embodiment 1.
Embodiment 5, raw material are kaolin.All the other conditions are with embodiment 1.
Please referring to Fig. 1.From Fig. 1 XRD, the sample characteristic diffraction peak that the present invention obtains is γ-Al
2O
3Its characteristic peak presents the broadening phenomenon, illustrates that particle is very little, is about 17nm with Scherre Equation for Calculating particle size.
Please referring to Fig. 2.From Fig. 2 sample transmission electron microscope pattern photo, particle size is at several-10nm.Because particle size is very little, specific surface energy is big, has the part particle aggregation to become whiskers.
Please referring to Fig. 3.From the selected area electron diffraction figure of Fig. 3 sample, there is diffraction spot to occur, the interpret sample particle is very little, has the crystallization phenomenon to occur again.
After 2 hours, BET (mensuration of specific surface area) measurement result is 140m to sample through 900 ℃ of roastings
2/ g.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011240482A CN1151070C (en) | 2001-08-09 | 2001-08-09 | Method for mfg. nano alumina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011240482A CN1151070C (en) | 2001-08-09 | 2001-08-09 | Method for mfg. nano alumina |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1401575A true CN1401575A (en) | 2003-03-12 |
| CN1151070C CN1151070C (en) | 2004-05-26 |
Family
ID=4665465
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011240482A Expired - Fee Related CN1151070C (en) | 2001-08-09 | 2001-08-09 | Method for mfg. nano alumina |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1151070C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004001278A3 (en) * | 2002-06-25 | 2004-08-19 | Univ Aalborg | Method for production of a product having sub-micron primary particle size, product produced by the method and apparatus for use of the method |
| CN102701154A (en) * | 2012-04-17 | 2012-10-03 | 华南理工大学 | Method for preparing ultrafine alumina by supercritical drying |
| CN103204526A (en) * | 2012-01-15 | 2013-07-17 | 湖南晟通科技集团有限公司 | A method for preparing an alumina sol |
| CN103928564A (en) * | 2013-01-11 | 2014-07-16 | 长春工业大学 | A method for preparing aluminum oxide passivation film on the surface of crystalline silicon solar cell |
| CN105060323A (en) * | 2015-07-23 | 2015-11-18 | 厦门大学 | High pore volume gamma-aluminium oxide and preparation method therefor |
| CN108531044A (en) * | 2018-05-23 | 2018-09-14 | 芜湖市创源新材料有限公司 | A kind of preparation method of antibacterial hydrophobic epoxy coating |
| CN112281020A (en) * | 2020-10-19 | 2021-01-29 | 西安工程大学 | A kind of wear-resistant copper-alumina composite material and preparation method thereof |
| CN116380822A (en) * | 2023-06-05 | 2023-07-04 | 未名环境分子诊断（常熟）有限公司 | Sewage continuous monitoring method and system |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BRPI0806597A2 (en) | 2007-01-15 | 2014-05-06 | Saint Gobain Ceramics | CERAMIC PARTICULAR MATERIAL AND FORMATION PROCESSES |
-
2001
- 2001-08-09 CN CNB011240482A patent/CN1151070C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004001278A3 (en) * | 2002-06-25 | 2004-08-19 | Univ Aalborg | Method for production of a product having sub-micron primary particle size, product produced by the method and apparatus for use of the method |
| CN103204526A (en) * | 2012-01-15 | 2013-07-17 | 湖南晟通科技集团有限公司 | A method for preparing an alumina sol |
| CN103204526B (en) * | 2012-01-15 | 2016-02-17 | 晟通科技集团有限公司 | A kind of method preparing alumina sol |
| CN102701154A (en) * | 2012-04-17 | 2012-10-03 | 华南理工大学 | Method for preparing ultrafine alumina by supercritical drying |
| CN102701154B (en) * | 2012-04-17 | 2014-04-02 | 华南理工大学 | Method for preparing ultrafine alumina by supercritical drying |
| CN103928564A (en) * | 2013-01-11 | 2014-07-16 | 长春工业大学 | A method for preparing aluminum oxide passivation film on the surface of crystalline silicon solar cell |
| CN105060323A (en) * | 2015-07-23 | 2015-11-18 | 厦门大学 | High pore volume gamma-aluminium oxide and preparation method therefor |
| CN108531044A (en) * | 2018-05-23 | 2018-09-14 | 芜湖市创源新材料有限公司 | A kind of preparation method of antibacterial hydrophobic epoxy coating |
| CN112281020A (en) * | 2020-10-19 | 2021-01-29 | 西安工程大学 | A kind of wear-resistant copper-alumina composite material and preparation method thereof |
| CN112281020B (en) * | 2020-10-19 | 2022-02-22 | 西安工程大学 | Wear-resistant copper-aluminum oxide composite material and preparation method thereof |
| CN116380822A (en) * | 2023-06-05 | 2023-07-04 | 未名环境分子诊断（常熟）有限公司 | Sewage continuous monitoring method and system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1151070C (en) | 2004-05-26 |
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