CN102372298B - Alumina nanobelt and production method thereof - Google Patents
Alumina nanobelt and production method thereof Download PDFInfo
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- CN102372298B CN102372298B CN 201010264233 CN201010264233A CN102372298B CN 102372298 B CN102372298 B CN 102372298B CN 201010264233 CN201010264233 CN 201010264233 CN 201010264233 A CN201010264233 A CN 201010264233A CN 102372298 B CN102372298 B CN 102372298B
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Abstract
The invention disclosed an alumina nanobelt and a production method thereof. The production method comprises the following steps of: uniformly mixing an aluminum source, polyethylene glycol, urea and water; then feeding the mixture in a hydrothermal kettle and carrying out a hydro-thermal reaction; and separating, washing, drying and roasting the reacted product to obtain the alumina nanobelt. The alumina has a polycrystalline structure and a specific surface area of 180-350m<2>/g; holes with the diameter of 2-10nm are distributed on the surface of a ribbon; the alumina nanobelt is in a fusiform shape in two-dimensional directions of width and length; and the alumina belt has a maximum width of 100-300nm, a length of 500-2000nm and a thickness of 10-50nm. The production method disclosed by the invention adopts a hydrothermal method and has the advantages of mild conditions, easiness for operation and production in large batches. The raw materials used by the invention are conventionalraw materials and have low cost. The polyethylene glycol adopted in the invention is an alumina directional growth regulator with no poison or odor and environment friendliness.
Description
Technical field
The present invention relates to a kind of aluminium oxide nano band and preparation method thereof, belong to field of inorganic material preparing technology.
Background technology
Aluminum oxide has application widely as a kind of important inorganic functional material in fields such as petrochemical complex, catalysis, fractionation by adsorption and ceramic toughening materials.The aluminium oxide nano material of one-dimentional structure has excellent physics, chemical property because of the anisotropy of its shape, the field such as separates in solar cell, sensor, catalyzer, sorbent material and selection and has a wide range of applications.Therefore, the preparation of one dimension aluminium oxide nano material and performance study have consequence in the modern material science.One dimension aluminium oxide nano material comprises forms such as nano wire, nanometer rod, nanotube, nano belt in constitutional features.
The present employing the whole bag of tricks aluminium oxide nano material of synthetic one dimension form has nano wire, nanometer rod, nanotube.The banded aluminum oxide of one dimension is as a kind of important form, and its preparation method also has related in some documents.
" Advanced Materials " (2005,17:1661-1665) a kind of employing chemical Vapor deposition process is disclosed, successfully having synthesized ring shape, both sides is the zigzag aluminium oxide nano band of being cut apart by twin boundary, and observes the high dielectric characteristics that this nano belt is better than conventional alumina powder jointed material.
" Journal Material Chemestry " (2003; 13:3040-3043) mixture that discloses with aluminium powder and aluminum oxide is raw material; under the condition of argon shield and 1350 ℃, adopt chemical Vapor deposition process to prepare the aluminium oxide nano band of single crystal structure.
" Journal of the European Ceramic Society " (2007,27:2629-2634) disclosing with purity is that 99.7% 325 purpose aluminium powders are raw material, under 1150 ℃ condition, adopt chemical Vapor deposition process to prepare the aluminium oxide nano band of single crystal structure.
This shows that above-mentioned several one dimension aluminium oxide nano bands are to adopt the chemical Vapor deposition process preparation.Temperature required higher, the condition of chemical gas-phase method sedimentation is comparatively harsh, and output is lower, does not have universality.Simultaneously, in catalyzer, sorbent material and chemical catalysis field such as selection separates, the alumina material that adopts mostly is the activated alumina of polycrystalline structure, and this polycrystalline activated alumina is porous material, has that loading capacity is big, specific surface area is big, intensity is high, Heat stability is good is than advantages such as height.And signle crystal alumina is less at aspects such as loading capacity, specific surface areas because crystalline structure is comparatively complete, therefore uses the restriction that is subjected to a certain degree in catalyzer, sorbent material and chemical catalysis field such as selection separates.
Summary of the invention
In order to overcome deficiency of the prior art, the invention provides a kind of porous surface, have aluminium oxide nano band of polycrystalline structure and preparation method thereof.
The character of aluminium oxide nano band of the present invention is as follows: have polycrystalline structure, specific surface area is 180～350m
2/ g is distributed with the hole that bore dia is 2～10nm on the belt surfaces, be fusiform at width and length two-dimensional directional, and the aluminium oxide nano band is in maximum width, and width is 10～300nm, and its length is 500～2000nm, and thickness is 10～50nm.
The preparation method of aluminium oxide nano band of the present invention comprises the steps:
(1) aluminium source, polyoxyethylene glycol, urea and water are mixed;
(2) mixture with step (1) places water heating kettle under 100～220 ℃, and hydro-thermal reaction is 12～72 hours under autogenous pressure;
(3) after the product separation that step (2) is obtained, washing, drying, the roasting, obtain the aluminium oxide nano band.
The addition sequence of the described various materials of step (1) is not limited.Water-soluble aluminum salt can be adopted in aluminium source described in the step (1), is preferably in aluminum chloride, aluminum nitrate and the Tai-Ace S 150 one or more.The viscosity-average molecular weight of described polyoxyethylene glycol is 10000～2500000, is preferably 100000～1000000.
Weight with the resulting final mixture of step (1) is benchmark, and the content of polyoxyethylene glycol is 0.05%～10.0%, is preferably 0.15%～3.0%; Urea and aluminium source total content are 10～40%, and urea and aluminium source are (with Al
3+Meter) mol ratio is 2.0～6.5, is preferably 3.0～5.0, and surplus is water.
Hydro-thermal reaction optimum condition described in the step (2) is, 140～190 ℃ of temperature of reaction, and the reaction times is 24～48 hours.
Separation method described in the step (3) is for filtering or centrifugation, and the used cleaning solvent of described washing is water, low-carbon alcohol or its mixture, is preferably water.Described low-carbon alcohol is the following alcohol of C4, as in methyl alcohol, ethanol, propyl alcohol and the butanols one or more.Described drying conditions is as follows: drying temperature is 0～120 ℃, and be 1～72 hour time of drying.Roasting condition in the step (3) is as follows: maturing temperature is 450～800 ℃, and roasting time is 1～15 hour, and preferred roasting condition is as follows: maturing temperature is 550～700 ℃, and roasting time is 3～8 hours.
By the resulting aluminium oxide nano band of the inventive method, be polycrystalline structure, be fusiform at width and length two-dimensional directional, in maximum width, its scope is at 100～300nm on the oxidation aluminium strip, and length is 500～2000nm, thickness is 10～50nm, the preparation method of aluminium oxide nano band provided by the invention, employed raw material is conventional raw material, and is with low cost.It is alumina oriented growth regulator that the present invention adopts polyoxyethylene glycol, and advantages of nontoxic raw materials is tasteless, is the environment-friendly material of generally acknowledging.The material preparation process is hydro-thermal reaction, and mild condition, easy handling can prepare in enormous quantities.
Polycrystal alumina nano belt provided by the invention, owing to belong to nanoscale in a dimension, and contain the hole of 2～10nm on the surface of material, being used for catalyzer, sorbent material and chemical industry catalytic processs such as selection separates, diffusional resistance is little, is very beneficial for the material mass transfer.
Description of drawings
Fig. 1 is low power transmission electron microscope (TEM) image of the prepared one dimension polycrystal alumina nano belt of the embodiment of the invention 1;
Fig. 2 is high power transmission electron microscope (TEM) image of the prepared one dimension polycrystal alumina nano belt of the embodiment of the invention 1;
Fig. 3 is the selected area electron diffraction figure of the prepared one dimension polycrystal alumina nano belt of the embodiment of the invention 1.
Embodiment
Below by the detailed explanation in addition of the inventive method of embodiment.Among the present invention, wt% represents massfraction.
Embodiment 1
(1) at room temperature prepares the mixed solution of aluminum chloride, polyoxyethylene glycol (viscosity-average molecular weight 100000), urea and water, in the mixed solution, polyethyleneglycol content is 0.15wt%, and urea and aluminum chloride total content are 15wt% (mol ratio of urea and aluminum chloride is 3), and water-content is 84.85wt%.
(2) mixture with step (1) places water heating kettle under 140 ℃, and hydro-thermal reaction is 48 hours under autogenous pressure.
(3) after the mixture filtration with step (2), wash with water again, reach or approaching neutrality until the pH of washings value.Product oven dry after 100 ℃ following washing 10 hours in 550 ℃ of roastings 3 hours, obtains the aluminium oxide nano band at last.
The pattern of this aluminium oxide nano band is comparatively regular, is fusiform, and is wide in the middle of showing as, the ribbon that two is narrow.The material specific surface area is 210m
2/ g is distributed with the hole that bore dia is 2～10nm on the belt surfaces, strap width is 100～200nm, and length is about 800～1000nm, and thickness is 40～50nm.Through the electron diffraction test, electron diffraction pattern is ring-type, illustrates that prepared nano belt is polycrystalline structure.
Embodiment 2
(1) at room temperature prepares the mixed solution of aluminum chloride, polyoxyethylene glycol (viscosity-average molecular weight 500000), urea and water, in the mixed solution, polyethyleneglycol content is 1wt%, and urea and aluminum chloride total content are 30wt% (mol ratio of urea and aluminum chloride is 4), and water-content is 69wt%.
(2) mixture with step (1) places water heating kettle under 170 ℃, and hydro-thermal reaction is 32 hours under autogenous pressure.
(3) after the mixture filtration with step (2), wash with water again, reach or approaching neutrality until the pH of washings value.Product oven dry after 100 ℃ following washing 10 hours in 650 ℃ of roastings 3 hours, obtains the aluminium oxide nano band at last.
This aluminium oxide nano belt surface is porous, and pattern is comparatively regular, is fusiform, and is wide in the middle of showing as, the ribbon that two is narrow, and specific surface area is 265m
2/ g, ribbon are distributed with the hole that bore dia is 2～10nm, and strap width is 200～420nm, and length is about 1000～1200nm, and thickness is 25～40nm.Through the electron diffraction test, be indicated as polycrystalline structure.
Embodiment 3
(1) at room temperature prepares the mixed solution of aluminum chloride, polyoxyethylene glycol (viscosity-average molecular weight 1000000), urea and water, in the mixed solution, polyethyleneglycol content is 3wt%, and urea and aluminum chloride total content are 40wt% (mol ratio of urea and aluminum chloride is 5), and water-content is 57wt%.
(2) mixture with step (1) places water heating kettle under 190 ℃, and hydro-thermal reaction is 24 hours under autogenous pressure.
(3) after the mixture filtration with step (2), wash with water again, reach or approaching neutrality until the pH of washings value.Product oven dry after 100 ℃ following washing 10 hours in 800 ℃ of roastings 2 hours, obtains the aluminium oxide nano band at last.
This aluminium oxide nano belt surface is porous, and pattern is comparatively regular, is fusiform, and is wide in the middle of showing as, the ribbon that two is narrow, and specific surface area is 338m
2/ g is distributed with the hole that bore dia is 2～10nm on the belt surfaces, strap width is 300～480nm, and length is about 1600～1800nm, and thickness is 15～25nm.Through the electron diffraction test, be indicated as polycrystalline structure.
Claims (7)
1. aluminium oxide nano band, its character is as follows: have polycrystalline structure, specific surface area is 180～350m
2/ g is distributed with the hole that bore dia is 2～10nm on the belt surfaces, be fusiform at width and length two-dimensional directional, and the aluminium oxide nano band is in maximum width, and width is 10～300nm, and its length is 500～2000nm, and thickness is 10～50nm.
2. the preparation method of the described aluminium oxide nano band of claim 1 comprises the steps:
(1) aluminium source, polyoxyethylene glycol, urea and water are mixed; The viscosity-average molecular weight of the described polyoxyethylene glycol of step (1) is 10000～2500000; Weight with the resulting final mixture of step (1) is benchmark, and the content of polyoxyethylene glycol is 0.05%～10.0%, and urea and aluminium source total content are 10%～40%, and urea and aluminium source are with Al
3+The mol ratio of meter is 2.0～6.5, and surplus is water;
(2) mixture with step (1) places water heating kettle under 100～220 ℃, and hydro-thermal reaction is 12～72 hours under autogenous pressure; Described hydrothermal reaction condition: 140～190 ℃ of temperature of reaction, the reaction times is 24～48 hours;
(3) after the product separation that step (2) is obtained, washing, drying, the roasting, obtain described aluminium oxide nano band.
3. according to the described preparation method of claim 2, it is characterized in that the aluminium source described in the step (1) adopts one or more in aluminum chloride, aluminum nitrate and the Tai-Ace S 150.
4. according to the described preparation method of claim 2, it is characterized in that the viscosity-average molecular weight of the described polyoxyethylene glycol of step (1) is 100000～1000000.
5. according to the described preparation method of claim 2, it is characterized in that the weight with the resulting final mixture of step (1) is benchmark, the content of polyoxyethylene glycol is 0.15%～3.0%, and urea and aluminium source total content are 10%～40%, and urea and aluminium source are with Al
3+The mol ratio of meter is 3.0～5.0, and surplus is water.
6. according to the described preparation method of claim 2, it is characterized in that the separation method described in the step (3) is for filtering or centrifugation; The cleaning solvent that described washing is adopted is one or more in water and the low-carbon alcohol, and wherein low-carbon alcohol is the following alcohol of C4.
7. according to the described preparation method of claim 2, it is characterized in that the drying conditions described in the step (3) is as follows: drying temperature is 0～120 ℃, and be 1～72 hour time of drying; Described roasting condition is as follows: maturing temperature is 450～800 ℃, and roasting time is 1～15 hour.
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| CN104108748B (en) * | 2013-04-17 | 2016-03-30 | 中国石油化工股份有限公司 | The preparation method of Sn-Al composite oxides and the application of these composite oxides |
| CN104556160B (en) * | 2013-10-22 | 2016-10-26 | 中国石油化工股份有限公司 | A kind of γ-Al2o3nanocrystal and preparation method thereof |
| CN105621462B (en) * | 2014-10-30 | 2017-05-17 | 中国石油化工股份有限公司 | Method for preparing aluminium oxide material |
| CN105879831B (en) * | 2016-04-11 | 2019-05-24 | 武汉理工大学 | A kind of γ-Al2O3The preparation method of adsorbent |
| CN108130595B (en) * | 2017-12-22 | 2020-08-07 | 西南交通大学 | Method for preparing alumina whisker by controlling atmosphere |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3853789A (en) * | 1971-03-26 | 1974-12-10 | J Warthen | Preparation of macroporous alumina extrudates |
| CN101041905A (en) * | 2007-03-13 | 2007-09-26 | 南京大学 | Aluminum oxide porous one-dimensional nano material and method for making same and usage |
| CN101318677A (en) * | 2008-07-10 | 2008-12-10 | 上海交通大学 | Method for preparing aluminum oxide nano-stick |
| CN101774533A (en) * | 2009-09-28 | 2010-07-14 | 南京大学 | Preparation method for gamma-alumina nanotube with prior exposure of (111) face |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3853789A (en) * | 1971-03-26 | 1974-12-10 | J Warthen | Preparation of macroporous alumina extrudates |
| CN101041905A (en) * | 2007-03-13 | 2007-09-26 | 南京大学 | Aluminum oxide porous one-dimensional nano material and method for making same and usage |
| CN101318677A (en) * | 2008-07-10 | 2008-12-10 | 上海交通大学 | Method for preparing aluminum oxide nano-stick |
| CN101774533A (en) * | 2009-09-28 | 2010-07-14 | 南京大学 | Preparation method for gamma-alumina nanotube with prior exposure of (111) face |
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