CN1285509C - Method for preparing unidimensional Al00H and gamma-Al2O3 nano materials - Google Patents
Method for preparing unidimensional Al00H and gamma-Al2O3 nano materials Download PDFInfo
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- CN1285509C CN1285509C CN 200310114419 CN200310114419A CN1285509C CN 1285509 C CN1285509 C CN 1285509C CN 200310114419 CN200310114419 CN 200310114419 CN 200310114419 A CN200310114419 A CN 200310114419A CN 1285509 C CN1285509 C CN 1285509C
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Abstract
The present invention provides a method for preparing unidimensional Al00H and gamma-Al2O3 nano materials. The method comprises the following steps: a, solutable aluminium salt is dissolved in the deionized water and added with ammonia water under the condition of icewater bath, and is strongly stirred with a stirrer until white precipitate Al(OH)3 is generated; then, b, the white precipitate Al(OH)3 is washed with deionized water in a centrifugal way until the PH value is neutrality; then, c, the solution is dispersed in the distilled water again and diverted to a stainless steel reaction vessel after uniformly stirred, the solution is completely reacted under the condition of heating and then naturally cooled, white dry products are obtained by radiating the reaction liquid with microwave, and the products are calcined in a muffle furnace to obtain gamma-Al2O3 nano needles; or only the condition for adding ammonia water is changed to obtain gamma-Al2O3 nano sticks; or the PH values of the white precipitate and the hydrothermal system are changed to obtain gamma-Al2O3 nano pipes.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to the preparations of nanomaterials method, relate in particular to a kind of one dimension AlOOH and γ-Al
2O
3The preparations of nanomaterials method.
Background technology
Develop a kind of controlled synthetic method is the target that the Materials science scholar is pursued always, since carbon nanotube is found, one-dimensional nano structure material receives much attention because of its peculiar electricity, optics, magnetic and mechanical property and the potential application in nano-device structure thereof, thereby to explore preparation low-dimension nano material structurally ordered, excellent property be the focus of research always.People are doing a lot of trials aspect the preparation of one-dimensional nano structure, but because the size of these monodimension nanometer materials is minimum and their anisotropy, make their synthetic and preparation still be faced with many challenges, therefore seek nucleus formation and the growing technology that to control monodimension nanometer material and become more and more important.Ultra-fine alumina is because of it has high temperature resistant, corrosion resistant, specific surface area is big, reactive behavior is high, electrical insulating property is good, be easy to excellent specific properties such as moulding at low temperatures, obtained using widely at aspects such as artificial lens, fine ceramics, transmitter, catalyzer, thereby the preparation of aluminium oxide nano material is significant.In in the past several years, continuous development along with nanotechnology, people are to the low-dimension nano material preparation and use growing interest, and the one dimension aluminium oxide nano material of different-shape such as nano wire, nanotube, nano belt, nanofiber, nanowhisker, nanometer ball prepare with diverse ways.But except R.Brusasco seminar in 1984 with AlCl
3And Al
2O
3Solution is raw material, obtains [R.Brusasco, J.Gaassi outside the fibrous AlOOH in 40 hours with 160 ℃ of reactions in autoclave, J.Baglio, Mater.Res.Bull., 19,1489], major part is to have introduced surfactant or template prepares one dimension γ-Al in reaction system
2O
3Nano material.Zhu et al has reported with polyethylene and has prepared the aluminium hydroxide intermediate as surfactant, thereby obtains one dimension γ-Al
2O
3Nanofiber [H.Zhu, J.D.Riches and J.C.Barry, Chem.Mater., 2002,14,2086.] Zhang et al has synthesized the bar-shaped γ-Al of porous with non-ionic surface active agent
2O
3Nano particle [Z.ZhangThomas J.Pinnavaia, J.Am.Chem.Soc., 2001,124,12294.]; Kuang et al has reported with CTAB and has prepared γ-Al as surfactant
2O
3Nanotube [D.Kuang, Y.Fang, H.Liu, C.Frommen and D.Fonske, J.Mater Chem.2003,13,660.]; Lee et al. prepares one dimension γ-Al with surfactant as template
2O
3Nanostructured [Hyun.Chul.Lee.et al., J.Am.Chem.Soc., 2003,125,2882].In view of this, up to now, preparation one dimension γ-Al
2O
3Nano material all be unable to do without surfactant or template, complex process, and the cost height is unfavorable for large-scale industrial production.
Summary of the invention
The purpose of this invention is to provide a kind ofly without surfactant or template, simple for process, cost is low, is suitable for one dimension AlOOH and the γ-Al of large-scale industrial production
2O
3The preparations of nanomaterials method is badly in need of to satisfy society.
Purpose of the present invention can be achieved by the following technical measures:
This one dimension AlOOH and γ-Al
2O
3The preparations of nanomaterials method is carried out as follows:
A, aluminum soluble salt is dissolved in the deionized water, under the ice-water bath condition, adds ammoniacal liquor, with the agitator vigorous stirring to producing white Al (OH)
3Precipitation; Then
B, with white Al (OH)
3Precipitate with deionized water centrifuge washing to pH value is neutral; Then
C, be re-dispersed in the distilled water again, transfer in the stainless steel cauldron after stirring, under heating condition, react completely, naturally cooling, gained reactant liquor microwave gets the white dried product and is AlOOH, and the product warp is calcined in Muffle furnace, gets γ-Al
2O
3Nanoneedle; Perhaps
Other steps are constant, only in a operation, add at ambient temperature ammoniacal liquor, get γ-Al
2O
3Nanometer rods; Perhaps
Other steps are constant, in a operation, will generate white Al (OH)
3The pH value of precipitation is adjusted into 9～11; In the c operation, dripping n-butylamine to pH value to hydrothermal system is 13～15, gets γ-Al
2O
3Nanotube.
Purpose of the present invention also can be achieved by the following technical measures:
Described aluminum soluble salt is selected from aluminum nitrate, Tai-Ace S 150 or aluminum chloride, and the reacting by heating temperature is 240～260 ℃ in the described reactor, and calcining temperature is 650～750 ℃ in the described retort furnace, and the calcination time is 1.5～2.5 hours.
The present invention is a raw material with aluminum soluble salt and ammoniacal liquor, with colloidal sol-Hydrothermal Preparation one dimension aluminium oxide nano material, systematic research the influence of preparation condition (dripping the condition of precipitation agent, the pH value of hydrothermal system etc.) to product size and pattern, employing X ray powder diffracting technology, TEM, HRTEM, Fourier infrared spectrum, solid fluorescence technology characterize products obtained therefrom.Experimental result shows, by changing experiment condition, can obtain the boehmite AlOOH monodimension nanometer material of different structure, at 700 ℃ of calcining 2h, can obtain the uniform aluminum oxide monodimension nanometer material of corresponding size with the dry products obtained therefrom of microwave irradiation.Because monodimension nanometer material has specific physiques such as anisotropy, therefore, be expected to obtain to use widely simultaneously in fields such as magnetic, electricity, optics.
Boehmite of the present invention (AlOOH) and aluminium oxide (γ-Al
2O
3) do not use any surfactant and template in the production process of nanometer rods, nanoneedle and nanotube, production technology is simple, production cost is low, just can control boehmite (AlOOH) and aluminium oxide (γ-Al by controlling certain pH value and reaction temperature
2O
3) pattern of nano material, and be suitable for adopting large-scale industrial production.
Description of drawings:
Fig. 1 is the XRD figure of the boehmite (AlOOH) for preparing of the present invention;
Fig. 2 is aluminium oxide (γ-Al that the present invention prepares
2O
3) XRD figure;
Fig. 4 is aluminium oxide (γ-Al that the present invention prepares
2O
3) the TEM photo of nanoneedle;
Fig. 6 is aluminium oxide (γ-Al that the present invention prepares
2O
3) the TEM photo of nanometer rods;
Fig. 7 is the TEM photo of boehmite (AlOOH) nanotube for preparing of the present invention;
Fig. 8 is aluminium oxide (γ-Al that the present invention prepares
2O
3) the TEM photo of nanotube;
Fig. 9 is aluminium oxide (γ-Al that the present invention prepares
2O
3) the high-resolution photo of nanometer rods;
Figure 10 is aluminium oxide (γ-Al that the present invention prepares
2O
3) the high-resolution photo of nanotube;
Figure 11 is aluminium oxide (γ-Al that the present invention prepares
2O
3) electron diffraction pattern of nanometer rods;
Figure 12 is aluminium oxide (γ-Al that the present invention prepares
2O
3) electron diffraction pattern of nanotube.
Figure 13 is aluminium oxide (γ-Al that the present invention prepares
2O
3) infrared spectrogram;
Figure 14 is aluminium oxide (γ-Al that the present invention prepares
2O
3) photoluminescence spectra figure.
Embodiment:
Embodiment 1:
Take by weighing the Al (NO) of 0.001mol
39H
2O is dissolved in the 20ml water, adds the NH of the 0.3M of new preparation under the ice-water bath condition
3H
2O uses the magnetic stirrer vigorous stirring, until produce white Al (OH)
3Precipitation, measuring the pH value is 8, repeatedly washs with deionized water, removes NO
3 -And NH
4 +To the pH value be about 7, be re-dispersed into then in the distilled water, transfer to after stirring in the 20ml stainless steel cauldron, tighten kettle cover, behind reaction 8h under 250 ℃ of conditions, naturally cooling, the gained reactant liquor is used microwave 3 minutes, and getting the white dried product is boehmite (AlOOH) nanoneedle, product with 700 ℃ of calcination 2h, gets γ-Al in Muffle furnace
2O
3Nanoneedle.
Embodiment 2:
Take by weighing the Al (NO) of 0.001mol
39H
2O is dissolved in the 20ml water, adds the NH of the 0.3M of new preparation at ambient temperature
3H
2O uses the magnetic stirrer vigorous stirring, up to producing white Al (OH)
3Precipitation, measuring the pH value is 8, repeatedly washs with deionized water, removes NO
3 -And NH
4 +To the pH value be about 7, again be distributed in the distilled water then, transfer to after stirring in the 20ml stainless steel cauldron, tighten kettle cover, behind reaction 8h under 250 ℃ of conditions, naturally cooling, the gained reaction solution is used microwave radiation 3 minutes, and getting the white dried product is boehmite (AlOOH) nanoneedle, product with 700 ℃ of calcination 2h, gets γ-Al in retort furnace
2O
3Nanometer rod.
Embodiment 3:
Take by weighing the Al (NO) of 0.001mol
39H
2O is dissolved in the 20ml water, adds at ambient temperature the NH of the 0.3M of new preparation
3H
2O uses the magnetic stirrer vigorous stirring, until produce white Al (OH)
3Precipitation, measuring the pH value is 10, repeatedly washs with deionized water, to remove NO
3 -And NH
4 +To the pH value be about 7, and then be re-dispersed in the distilled water, be about 14 by dripping n-butylamine adjusting pH value afterwards, be moved in the 20ml stainless steel cauldron, tighten kettle cover, behind reaction 8h under 250 ℃ of conditions, what obtain is boehmite (AlOOH) nanotube, and product with 700 ℃ of calcination 2h, gets γ-Al in Muffle furnace
2O
3Nanotube.
Claims (3)
1, a kind of one dimension AlOOH preparation of nanomaterials is characterized in that this method carries out as follows:
A, aluminum soluble salt is dissolved in the deionized water, under the ice-water bath condition, adds ammoniacal liquor, with the agitator vigorous stirring to producing white Al (OH)
3Precipitation; Then
B, with white Al (OH)
3Precipitate with deionized water centrifuge washing to pH value is neutral; Then
C, be distributed to again in the distilled water again, transfer in the stainless steel cauldron after stirring, under heating condition, react completely, naturally cooling, gained reaction solution microwave radiation, product.
2, a kind of γ-Al
2O
3The preparations of nanomaterials method is characterized in that this method carries out as follows:
A, aluminum soluble salt is dissolved in the deionized water, under the ice-water bath condition, adds ammoniacal liquor, with the agitator vigorous stirring to producing white Al (OH)
3Precipitation; Then
B, with white Al (OH)
3Precipitate with deionized water centrifuge washing to pH value is neutral; Then
C, be re-dispersed in the distilled water again, transfer in the stainless steel cauldron after stirring, under heating condition, react completely, naturally cooling, gained reactant liquor microwave gets the white dried product, and the product warp is calcined in Muffle furnace, gets γ-Al
2O
3Nanoneedle; Perhaps
Other steps are constant, in a operation, add at ambient temperature ammoniacal liquor, get γ-Al
2O
3Nanometer rods; Perhaps
Other steps are constant, in a operation, will generate white Al (OH)
3The pH value of precipitation is adjusted into 9～11; In the c operation, dripping n-butylamine to pH value to hydrothermal system is 13～15, gets γ-Al
2O
3Nanotube.
3, preparation method according to claim 1 and 2, it is characterized in that described aluminum soluble salt is selected from aluminum nitrate, Tai-Ace S 150 or aluminum chloride, the reacting by heating temperature is 240～260 ℃ in the described reactor, calcining temperature is 650～750 ℃ in the described retort furnace, and the calcination time is 1.5～2.5 hours.
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|---|---|---|---|
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| CN1285509C true CN1285509C (en) | 2006-11-22 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177291B (en) * | 2007-10-26 | 2010-05-19 | 上海大学 | Method for preparing special-shaped AlOOH nano material |
| CN101885501B (en) * | 2009-05-13 | 2012-06-27 | 中国石油化工股份有限公司 | Preparation method of one-dimensional alumina nanowire/nano rod |
| CN104549534B (en) * | 2013-10-23 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of alumina support and preparation method thereof |
| CN106458623A (en) * | 2014-05-25 | 2017-02-22 | 王胜国 | Method and apparatus for producing alumina monohydrate and sol gel abrasive grain |
| CN105174293B (en) * | 2015-09-10 | 2017-11-28 | 中海油天津化工研究设计院有限公司 | A kind of preparation method for the boehmite that pore-size distribution is concentrated |
| CN106448964B (en) * | 2016-08-24 | 2017-11-17 | 长乐智睿恒创节能科技有限责任公司 | A kind of high-temperature insulation cable insulating materials and preparation method thereof |
| CN107298453A (en) * | 2017-07-03 | 2017-10-27 | 中国科学院青海盐湖研究所 | The nanocrystalline preparation method of boehmite |
| CN107500323B (en) * | 2017-07-14 | 2019-04-12 | 山东旭晟东阳新材料科技有限公司 | A kind of γ phase alumina nanotube and preparation method thereof |
| CN107879368A (en) * | 2017-12-06 | 2018-04-06 | 宁波爱克创威新材料科技有限公司 | Nano aluminium oxide and preparation method thereof |
| CN111317123A (en) * | 2018-12-14 | 2020-06-23 | 解冰 | Papaya enzyme composition for improving and promoting functions of digestive absorption system, preparation method and composite nano preparation |
| CN111317132A (en) * | 2018-12-14 | 2020-06-23 | 解冰 | Papaya enzyme composition for assisting in enhancing digestion and absorption functions of critically ill patients, preparation method and composite nano-preparation |
| CN110357135B (en) * | 2019-06-19 | 2020-11-24 | 苏州盛曼特新材料有限公司 | Preparation method of special alumina for high-purity lithium battery diaphragm |
| CN111470523A (en) * | 2020-05-07 | 2020-07-31 | 郑州中科新兴产业技术研究院 | Template-free graded growth preparation method of water-dispersible boehmite nanosheet |
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