CN103172096A - Method for preparing nanometer aluminium oxide sheet - Google Patents
Method for preparing nanometer aluminium oxide sheet Download PDFInfo
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- CN103172096A CN103172096A CN2013100949676A CN201310094967A CN103172096A CN 103172096 A CN103172096 A CN 103172096A CN 2013100949676 A CN2013100949676 A CN 2013100949676A CN 201310094967 A CN201310094967 A CN 201310094967A CN 103172096 A CN103172096 A CN 103172096A
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Abstract
The invention provides a method for preparing a nanometer aluminium oxide sheet. The method comprises the steps of: (1) adding organic aluminium salt into an opening container containing an organic solvent, and stirring to completely dissolve the organic aluminium salt; (2) putting the opening container into a closed container containing distilled water, putting the closed container into a water bath, controlling the temperature of the water bath to be less than the boiling point of the organic solvent, heating and reacting for 5-24hours; and (3) separating, carrying out alcohol washing, drying and calcinating a product at 400-900 DEG C for 2-8hours, naturally cooling to a room temperature, thus obtaining the nanometer aluminium oxide sheet. The preparation process is completed at low temperature, the method is moderate in reaction, simple in technological process, convenient to operate, easy to control and has low requirements on equipment, the agglomeration influence on product performances can be greatly reduced, and the product has good dispersibility and high purity; and moreover, the obtained aluminium oxide sheet has high specific surface area and narrow pore size distribution and is suitable for being applied to the fields of catalysis, adsorption and the like.
Description
Technical field
That the present invention relates to is a kind of preparation method of inorganic nano material, specifically a kind of nano aluminium oxide preparation of sections method.
Background technology
Nano material refer in the three-dimensional space size of material have at least one dimension be in nanoscale scope (1-100nm) within or the material that formed as basic structural unit by them.Nano material has a wide range of applications it because the ad hoc structure of its micro-scale has unique various physics-chem characteristics that are different under macrostate such as surface effects, small-size effect, quantum size effect and quantum tunneling effect in a lot of fields.The assembling meeting of initial nano material has a huge impact the size of material, pattern, crystalline structure etc., and then affects the performance of material, and zero dimension and nanometer particle are by being assembled into two dimension or ordered 3 D structure in hydrogen bond, electrostatic force and Van der Waals etc.These novel graded structures are perhaps started the New Times of advanced nano-component, and might fundamentally thoroughly solve the problems such as the energy, health, environment of facing mankind.
Nano aluminium oxide is except having the feature that nano material generally has, also have high strength, high rigidity, the characteristic such as heat-resisting, corrosion-resistant, show a series of excellent properties in fields such as power, light, heat, electricity and chemical reactions, can be widely used in the high-tech areas such as traditional industries (chemical industry, metallurgy, building materials etc.) and novel material, microelectronics, aerospace.Activated alumina has that surface-area is high, pore volume is large, pore size distribution is concentrated and the advantage such as Active sites is many; very strong adsorptive power and catalytic activity are arranged; can effectively solve the problems such as the highly selective of catalyzer and sorbent material and high reaction activity, have a wide range of applications in fields such as petrochemical complex and environment protection.Aluminum oxide and hydrated aluminum oxide be applied in the features such as pattern, size and degree of crystallinity that depend on to a great extent sample, therefore the aluminium oxide nano material of design and preparation controllable appearance and size has attracted numerous investigators' interest.Raw-material existence when synthetic can be simply be summarised as vapor phase process, liquid phase method and solid phase method three classes with the synthetic method of aluminum oxide.The people such as Roy [J.Mater.Sci., 2011,46 (14): 4812-4819] adopt vapour deposition process under 77 ℃ of successive pulse effects at trimethyl aluminium and water vapor at continuous carbon fiber surface deposition of aluminium oxide thin slice, carbon fiber can optionally be removed by thermooxidizing under higher than the condition of 550 ℃ in temperature.The people such as Yan Guojin [diamond and grinding materials and grinding tool engineering, 2006,156 (6): 68-70] are with analytically pure NH
4Al (SO
4)
2And NH
4HCO
3Be raw material, under suitable processing condition, make NH
4Al (OH)
2CO
3Presoma is calcined 1h under 1100 ℃, obtaining particle diameter is superfine spherical α-Al of 80～100nm
2O
3Niesz etc. [Chem.Commun., 2005,1986-1987] use the sol-gel method based on self-assembling technique to synthesize to have the ordered mesoporous aluminium oxide material of high-specific surface area and narrow pore size distribution.
Although and can obtain desirable pattern by the material that these method sides get, all more or less exist some defectives.Vapor phase process requires starting material to be gasified totally before reaction, and is larger to the consumption of energy, simultaneously reaction unit had relatively high expectations, and technique controlling difficulty is larger, is not suitable for scale operation.The prepared product particle of solid phase method without reunite, fillibility is good and technique is simple, but still there are some outstanding shortcomings in this method, as large in energy consumption, efficient is low, sneak into easily that impurity, powder are easily reunited and granularity wayward etc.Prepare in nano alumina powder jointed process in wet method, the reunion of powder often can occur, grow into the process such as washing, drying, roasting of product from nucleation, crystal, the reunion of product might occur in each stage, thereby causes the reduction of material property.
Summary of the invention
The object of the present invention is to provide a kind of reaction temperature and, technical process is simple and reunite nano aluminium oxide preparation of sections method few.
The object of the present invention is achieved like this:
(1) organic aluminium salt is joined in the open container that contains organic solvent, stirring is dissolved organic aluminium salt fully;
(2) open container is placed in the encloses container that contains distilled water, encloses container in water-bath, is controlled bath temperature lower than the boiling point of organic solvent, carry out reacting by heating 5-24h;
(3) products therefrom separation, alcohol wash, drying at 400-900 ℃ of roasting 2-8h, naturally cool to room temperature, obtain nano oxidized aluminum slice.
The present invention can also comprise:
1, controlling bath temperature is 50-99 ℃.
2, described aluminium salt is a kind of in aluminum isopropylate, aluminium secondary butylate or isoamyl aluminium alcoholates.
3, described organic solvent is a kind of in ethanol, Virahol, toluene, methylene dichloride or monochloroethane.
Technical characterictic of the present invention is: the water in outside encloses container is heated to vaporize and is full of in whole container, and the aluminium alcoholates in inner beaker solution contacts with water vapour and can be hydrolyzed, reaction only occurs over just the interface of water vapour and solution, so method can be referred to as the liquid-gas interface method.In system, low water concentration can reduce the speed of aluminium alcoholates hydrolysis and condensation, makes aluminium alcoholates being hydrolyzed progressively, deposit to slowly beaker bottom, thereby the generation of minimizing product agglomeration is conducive to obtain dispersiveness nano oxidized aluminum slice preferably.
The invention has the advantages that preparation process carries out at low temperatures, reaction temperature and, technical process is simple, easy to operate being easy to controlled, requirement to equipment is lower, can reduce to a great extent the impact of reuniting on product performance, and good product dispersibility, purity are high, and the alumina wafer that obtains has higher specific surface area and narrower pore size distribution, is adapted at the application in the fields such as catalysis and absorption.
Description of drawings
Fig. 1 is the TEM figure of the prepared nano oxidized aluminum slice of the embodiment of the present invention 2.
Fig. 2 is the nitrogen adsorption desorption curve of the prepared nano oxidized aluminum slice of the embodiment of the present invention 1
Fig. 3 is the graph of pore diameter distribution that reaches of the prepared nano oxidized aluminum slice of the embodiment of the present invention 1.
Embodiment
Below in conjunction with specific examples, technical scheme of the present invention and effect are further described, still, these are that concrete grammar and the explanation used in embodiment do not limit protection scope of the present invention.
Embodiment 1:
Take a certain amount of aluminum isopropylate and join in the beaker that contains appropriate toluene, stirring is dissolved it fully, forms the solution of 1mol/L.Beaker is placed in the encloses container that contains 100ml distilled water, with the 80 ℃ of heating in water-bath of this container, reaction 8h; Products therefrom separation, alcohol wash, 80 ℃ of dryings at 700 ℃ of roasting 4h, naturally cool to room temperature, obtain nano oxidized aluminum slice.
This nano oxidized aluminum slice has higher specific surface area and pore volume, and the BET specific surface area is 308.8m
2/ g, pore volume are 0.55cm
3/ g, pore size distribution mainly concentrate in mesoporous scope, and mean pore size is 7.8nm.
Embodiment 2:
Take a certain amount of aluminum isopropylate and join in the beaker that contains appropriate Virahol, stirring is dissolved it fully, forms the solution of 1mol/L.Beaker is placed in the encloses container that contains 100ml distilled water, with the 60 ℃ of heating in water-bath of this container, reaction 12h; Products therefrom separation, alcohol wash, 80 ℃ of dryings at 500 ℃ of roasting 4h, naturally cool to room temperature, obtain nano oxidized aluminum slice.
Embodiment 3:
Take a certain amount of aluminium secondary butylate and join in the beaker that contains appropriate dehydrated alcohol, stirring is dissolved it fully, forms the solution of 1mol/L.Beaker is placed in the encloses container that contains 100ml distilled water, with the 50 ℃ of heating in water-bath of this container, reaction 16h; Products therefrom separation, alcohol wash, 80 ℃ of dryings at 500 ℃ of roasting 4h, naturally cool to room temperature, obtain nano oxidized aluminum slice.
Claims (5)
1. nano aluminium oxide preparation of sections method is characterized in that:
(1) organic aluminium salt is joined in the open container that contains organic solvent, stirring is dissolved organic aluminium salt fully;
(2) open container is placed in the encloses container that contains distilled water, encloses container in water-bath, is controlled bath temperature lower than the boiling point of organic solvent, carry out reacting by heating 5-24h;
(3) products therefrom separation, alcohol wash, drying at 400-900 ℃ of roasting 2-8h, naturally cool to room temperature, obtain nano oxidized aluminum slice.
2. nano aluminium oxide preparation of sections method according to claim 1 is characterized in that: controlling bath temperature is 50-99 ℃.
3. nano aluminium oxide preparation of sections method according to claim 1 and 2 is characterized in that: described aluminium salt is a kind of in aluminum isopropylate, aluminium secondary butylate or isoamyl aluminium alcoholates.
4. nano aluminium oxide preparation of sections method according to claim 1 and 2 is characterized in that: described organic solvent is a kind of in ethanol, Virahol, toluene, methylene dichloride or monochloroethane.
5. nano aluminium oxide preparation of sections method according to claim 3 is characterized in that: described organic solvent is a kind of in ethanol, Virahol, toluene, methylene dichloride or monochloroethane.
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| CN201310094967.6A CN103172096B (en) | 2013-03-22 | 2013-03-22 | Method for preparing nanometer aluminium oxide sheet |
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| CN201310094967.6A CN103172096B (en) | 2013-03-22 | 2013-03-22 | Method for preparing nanometer aluminium oxide sheet |
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| CN103172096B CN103172096B (en) | 2015-02-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560485A (en) * | 2022-03-19 | 2022-05-31 | 长沙宁曦新材料有限公司 | Preparation method of superfine alumina |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143047A (en) * | 1995-07-14 | 1997-02-19 | 余忠清 | Preparing method for high purity super fine dispersing ball shape AL2O3 powder |
| CN1374251A (en) * | 2002-04-08 | 2002-10-16 | 常耀辉 | Prepn of superpurity nano level alumina powder |
-
2013
- 2013-03-22 CN CN201310094967.6A patent/CN103172096B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143047A (en) * | 1995-07-14 | 1997-02-19 | 余忠清 | Preparing method for high purity super fine dispersing ball shape AL2O3 powder |
| CN1374251A (en) * | 2002-04-08 | 2002-10-16 | 常耀辉 | Prepn of superpurity nano level alumina powder |
Non-Patent Citations (3)
| Title |
|---|
| M.M. AMINI ET AL.: "Effect of Solution Chemistry on Preparation of Boehmite by Hydrothermal Assisted Sol-Gel Processing of Aluminum Alkoxides", 《JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY》, vol. 36, no. 1923, 31 December 2005 (2005-12-31), pages 19 - 23 * |
| 石涛等: "水热辅助溶胶-凝胶法制备纳米晶γ-Al2O3及表征", 《无机化学学报》, vol. 25, no. 5, 31 May 2009 (2009-05-31), pages 915 - 919 * |
| 赵晓媛等: "异丙醇铝加压水解合成亚微米级球形氧化铝粉", 《无机盐工业》, vol. 39, no. 11, 30 November 2007 (2007-11-30), pages 12 - 14 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560485A (en) * | 2022-03-19 | 2022-05-31 | 长沙宁曦新材料有限公司 | Preparation method of superfine alumina |
| CN114560485B (en) * | 2022-03-19 | 2024-03-22 | 长沙宁曦新材料有限公司 | Preparation method of superfine alumina |
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| CN103172096B (en) | 2015-02-25 |
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