CN105948087A - Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure - Google Patents

Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure Download PDF

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CN105948087A
CN105948087A CN201610186410.9A CN201610186410A CN105948087A CN 105948087 A CN105948087 A CN 105948087A CN 201610186410 A CN201610186410 A CN 201610186410A CN 105948087 A CN105948087 A CN 105948087A
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alooh
nanostructured
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郑文君
秦清
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Nankai University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13Nanotubes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area

Abstract

Disclosed is a method for preparing gamma-AlOOH and gamma-Al2O3 through ionic-liquid-assisted hydrothermal synthesis. The method is characterized in that divalent metal ions are utilized to drive a decomposition reaction of a precursor so as to generate gamma-AlOOH in a mild condition. The method comprises main steps: 1) dissolving aluminium salt, an ionic liquid and divalent metal ions in deionized water according to different ratios, and performing uniform stirring; 2) transferring the obtained solution to a reactor and performing a reaction at different reaction temperatures for a while; 3) after the reaction is over, performing cooling to the room temperature, performing centrifugalization, performing alternate washing with deionized water and absolute ethanol, and performing drying to obtain a precursor of gamma-AlOOH; and 4) putting the precursor of gamma-AlOOH in a muffle furnace, and carrying out calcination to obtain a gamma-Al2O3 nanometer material with the identical shape. According to the method, gamma-AlOOH in the shape of a needle-shaped crystal whisker, a nanotube, and a bamboo-leaf-shaped nanometer flower and gamma-Al2O3 converted from gamma-AlOOH are synthesized. The obtained gamma-Al2O3 is relatively high in degree of crystallinity and specific surface area and has comparatively high potential of large-scale production.

Description

A kind of γ-AlOOH and γ-Al2O3Nanotube and the preparation method of nanostructured
Technical field
The invention belongs to field of inorganic nano material.It is specifically related under temperate condition, ionic liquid auxiliary synthesis Gao Bibiao Area γ-aluminum oxyhydroxide, and as presoma, the method for the thermally treated gama-alumina obtaining identical pattern.The present invention can Hope for pottery, catalysis, optics, adsorb, separate, photoelectricity turns device, the field such as nano material and composite.
Background technology
In numerous nonmetal and transition metal oxide materials, aluminium oxide because of have aboundresources, cheap, compare table The features such as area is big and chemical stability is good and nontoxic, exchange at catalysis, ion, the field such as adsorbent and pottery has suitable It is widely applied.The particularly low-temperature stabilization phase gama-alumina surface of aluminium oxide has abundant hydroxyl, is absorption and catalysis neck The alumina material being most widely used in territory.In view of the processes such as absorption and catalysis occur mainly in the surface of material, gamma oxidation The surface texture of aluminum plays pivotal role in the application.Though amorphous gama-alumina has the highest specific surface area (> 800m2/ G), but its poor heat stability and microstructural stability seriously restrict its application in catalytic process, and improve material Degree of crystallinity is to improve material heat stability and the effective means of microstructural stability.Therefore, explore that degree of crystallinity is higher, specific surface area The synthetic technology of big gama-alumina nano material is still current problem demanding prompt solution.
Gama-alumina nano material can pass through the side of the presomas such as heat treatment aluminium carbonate, aluminium hydroxide and hydrated alumina Method obtains.So far, people by the approach such as liquid phase method and vapor phase method, successfully prepare the gama-alumina nanometer of different appearance Material, such as: nanometer rods, nano wire, nanotube, nano hollow structure and pore structure etc. (Adv.Funct.Mater., 2007,17, 2411-2418;J.Mater.Chem., 2008,18,442-449;J.Phys.Chem.C, 2007,111,700-707; J.Phys.Chem.C, 2008,112.16764-16768;J.Phys.Chem.C, 2009,113.17527-17535; J.Mater.Chem., 2010,20,4587-4595;J.Mater.Chem, 2003,13,660-662;Nano Lett., 2008, 8,2155-2160;Gryst.Grouth Des, 2010,10,2928-2933;Chem.Commum, 2010,46,2650- 2652).But, these methods also exist following several respects problem: it is generally required to add template, surfactant or other is auxiliary Helping reagent, the purge process making product is complex, and the removal process of auxiliary reagent also may cause the broken of product micro structure Bad, what is more important surface rearrangement often results in the reduction of gama-alumina nano material surface active;Part Methods exists Need to add volatility or toxic organic solvents, reaction temperature is higher or needs two steps to prepare, and could obtain γ-hydroxyl oxidize The problems such as aluminum presoma.Though the existing Patents of the preparation of gama-alumina nanotube, such as: CN201110327588, CN200910035950 and CN200510086373 etc., but method therefor is that electrostatic spinning, surfactant are as template etc. Method, there are still the common problem of other solution chemical method documents.Therefore, under conditions of more gentleness, exploitation low energy consumption, Environmental friendliness, method are easy, equipment requirements is low and are suitable for the preparation method of gama-alumina nano material of large-scale production, It is still one of key technology of meeting gama-alumina Application of micron demand.
Summary of the invention
Key issue to be solved by this invention is: provide the Hydrothermal Synthesis that the ionic liquid under a kind of temperate condition assists Method, to realize γ-aluminum oxyhydroxide presoma that degree of crystallinity is higher, specific surface area is bigger, before being thermally treated resulting in succession The method driving the gama-alumina nano material of bodily form looks.Product has higher degree of crystallinity and higher specific surface area, it is expected to should For fields such as catalysis and absorption, and there is the feasibility of higher large-scale production.
The scheme that the present invention uses is: under the hydrothermal condition of ionic liquid auxiliary, by adding Zn2+The metals such as ion from Son, utilizes the complexing power of metal ion as driving force, promotes the decomposition reaction containing aluminum intermediate product, to realize temperate condition The synthesis of lower γ-aluminum oxyhydroxide.In the present invention, the addition of metal ion reduce reaction precursor decomposition temperature, and from The addition of sub-liquid then achieves effective control of product morphology.γ-the aluminum oxyhydroxide of synthesis is thermally treated, is crystallized Degree is preferable, surface area is higher, and pattern keeps good gama-alumina nano material.
The preparation process of the present invention is as follows:
First, by the AlCl of 2mmol3·6H2Zn (the NO of O, 1mmol3)2·6H2The CH of O, 5mmol3COOK and a certain amount of Ionic liquid be sequentially added into, be dissolved in the deionized water of 15mL, be stirred until homogeneous.
Second, above-mentioned prepared clear solution is moved to in teflon-lined stainless steel cauldron, juxtaposition In baking oven, at a temperature of differential responses, react a period of time.Being cooled to room temperature, product is performing centrifugal separation on, and uses deionized water With dehydrated alcohol alternately washing, it is dried.Obtain γ-aluminum oxyhydroxide presoma.
3rd, collect the γ-aluminum oxyhydroxide presoma obtained, be placed in muffle furnace, at 600 DEG C, calcine 2h, obtain Gama-alumina nano material.
Chemical reaction involved in the present invention is as shown in Figure 1.Preparation aluminum source can be aluminum chloride, aluminum nitrate, aluminum sulfate, The aluminum soluble salt such as aluminum acetate and Alumen, aqueous salt and anhydrous salt;Ionic liquid is glyoxaline ion liquid, and its purity is 95~99.9%, water content≤2%;Anion not with aluminium ion generation precipitation on the premise of, soluble-salt For the preparation of the present invention, and the most alternative zinc salt of soluble salt of alkaline-earth metal soluble salt and First Transition system divalent metal, use Preparation in the present invention.The mol ratio of described aluminium salt and ionic liquid is 1: 0.2~1: 10;The mol ratio of aluminium salt and zinc salt is 1: 0.1~1: 2;Aluminium salt concentration is 0.05~2mol/L;Reaction temperature is 70~200 DEG C;γ-aluminum oxyhydroxide presoma calcining bar Part is 600 DEG C, 2 hours.
As shown in Figure 2, under above-mentioned preparation condition, reaction temperature is 130 DEG C, during reaction 24h, and the γ-hydroxyl oxygen obtained The X-ray powder diagram changing aluminum presoma can be attributed to orthogonal γ-aluminum oxyhydroxide (JCPDS Card 21-1307).Forge After burning, the X-ray powder diagram (Fig. 3) of product, then can be attributed to a cube gama-alumina (JCPDS Card 50-0741). The elementary analysis structure of the gama-alumina that γ-aluminum oxyhydroxide and calcining obtain shows, both alumina ratios are all sufficiently close to two The stoichiometric proportion (Fig. 2 and Fig. 3) of person.
Present invention have an advantage that the decomposition driving eston presoma is anti-1. by introducing divalent ion Should, hence it is evident that reduce the generation temperature of γ-aluminum oxyhydroxide, make to prepare reaction condition the gentleest, and be not added with divalent zinc ion Time product eston (Fig. 4, thing corresponds to CH3COO)2Al(OH)(JCPDS No.54-0321));2. imidazoles Class ionic liquid does not has obvious vapour pressure, and the pressure of reaction system is significantly less than conventional hydrothermal or solvent-thermal process, therefore this The compressive resistance of reaction vessel is required substantially to reduce by bright method;3. conventional mould agent or surfactant etc. are not used, it is to avoid The problems such as the removal of additive;4. having good water solublity because of glyoxaline ion liquid used, ionic liquid can be by simple Washing process remove, and ionic liquid can be recycled through simple still-process, it is expected to realize gama-alumina nanometer The eco-friendly large-scale production of material;5. the present invention passes through reaction temperature and the consumption of ionic liquid, can realize product shape Looks, degree of crystallinity, the Effective Regulation of specific surface area, it is expected to there is the broader scope of application and higher practical value.
Accompanying drawing illustrates:
The chemical reaction process that accompanying drawing 1 technical solution of the present invention relates to.
Accompanying drawing 2, at 130 DEG C, reacts XRD spectra and the power spectrum elementary analysis of γ-aluminum oxyhydroxide nanotube prepared by 10h.
Accompanying drawing 3 at 130 DEG C, the reaction γ-aluminum oxyhydroxide nanotube prepared of 10h XRD spectra after calcining and power spectrum Elementary analysis.
Accompanying drawing 4 does not adds zinc ion, and at 130 DEG C, reaction 10h prepares the XRD spectra of product.
Under the conditions of accompanying drawing 5 embodiment 1, scanning and the projection electron microscope of the γ of preparation-aluminum oxyhydroxide nanotube divide Analysis result.
Under the conditions of accompanying drawing 6 embodiment 1, scanning and projection electron after the γ of preparation-aluminum oxyhydroxide nanotube calcining show Micro mirror analysis result.
Under the conditions of accompanying drawing 7 embodiment 2, the γ of preparation-aluminum oxyhydroxide presoma XRD spectra after calcining and energy spectral element Element is analyzed.
Under the conditions of accompanying drawing 8 embodiment 2, scanning and the projection electron microscope of the γ of preparation-aluminum oxyhydroxide presoma divide Analysis result.
Under the conditions of accompanying drawing 9 embodiment 3, the XRD spectra of the γ of preparation-aluminum oxyhydroxide presoma.
Under the conditions of accompanying drawing 10 embodiment 3, the transmission electron microscope morphology analysis result of the γ of preparation-aluminum oxyhydroxide presoma.
Under the conditions of accompanying drawing 11 embodiment 3, the XRD of the γ of preparation-aluminum oxyhydroxide presoma calcined product and morphology analysis Result.
Under the conditions of accompanying drawing 12 embodiment 4, the XRD spectra of the γ of preparation-aluminum oxyhydroxide presoma and EDAX results.
Under the conditions of accompanying drawing 13 embodiment 4, the morphology analysis result of the γ of preparation-aluminum oxyhydroxide presoma.
Under the conditions of accompanying drawing 14 embodiment 4, the XRD of the γ of preparation-aluminum oxyhydroxide presoma calcined product and energy spectrum analysis Result.
Under the conditions of accompanying drawing 15 embodiment 4, the morphology analysis result of the γ of preparation-aluminum oxyhydroxide presoma calcined product.
Subordinate list 1 embodiment 5 synthesis condition and product thing phase.
Under the conditions of accompanying drawing 16 embodiment 6, the morphology analysis result of the γ-aluminum oxyhydroxide of preparation.
Under the conditions of accompanying drawing 17 embodiment 6, different chlorination 1-octyl groups-, the transmission electron microscope of 3-Methylimidazole. ionic liquid consumption product Photo.
Under the conditions of subordinate list 2 embodiment 7, the thing phase of each product and appearance.
Under the conditions of subordinate list 3 embodiment 7, the specific surface area of γ-aluminum oxyhydroxide presoma calcined product.
Detailed description of the invention:
Embodiment 1
Preparation process as described in summary of the invention, 5mol chlorination 1-butyl-2,3-methylimidazole ([Bdmim] Cl) ion Liquid, reaction temperature is 130 DEG C, response time 10h.After reaction, naturally cool to room temperature.Product is through filtering, using deionized water And absolute ethanol washing, the vacuum drying oven of 80 DEG C is dried 3h, obtains γ-aluminum oxyhydroxide nano material.By γ-hydroxyl Alumina precursor is placed in ceramic crucible, in muffle furnace, calcines 2h, obtain gama-alumina nano material at 600 DEG C.
Gained γ-aluminum oxyhydroxide and gama-alumina are respectively orthogonal γ-aluminum oxyhydroxide (JCPDS Card 21- 1307) and cube gama-alumina (JCPDS Card 50-0741), XRD spectra and elementary analysis as shown in accompanying drawing 2 and accompanying drawing 3, And energy spectrum analysis fails to detect element.Scanning nuclear microprobe result is as shown in accompanying drawing 5 and accompanying drawing 6, it is seen that γ-hydroxyl oxygen Change aluminum and gama-alumina is diameter 4-6 nanometer.It is about the nanotube of tens nanometer.
Embodiment 2
Reaction condition is same as embodiment 1, only replaces zinc nitrate with equimolar magnesium nitrate.The XRD of synthetic product and electronics Power spectrum test result, as shown in Figure 7.The XRD figure spectrum preparing product is similar to embodiment 1 product, can be attributed to orthohormbic structure γ-AlOOH (JCPDS Card21-1307), and and electron spectrum elementary analysis result show, product fails detect magnesium Element product.The scanning electron microscope analysis result of product shows, product appearance is also in embodiment 1 product similar (accompanying drawing 8).
Embodiment 3
Reaction condition is same as embodiment 1, only reaction temperature is promoted to 150 DEG C.After reaction, naturally cool to room temperature.Produce Thing, through filtering, with deionized water and absolute ethanol washing, is dried 3h in the vacuum drying oven of 80 DEG C, obtains γ-hydroxyl oxidize Aluminum nano material.γ-aluminum oxyhydroxide is placed in ceramic crucible, in muffle furnace, calcines 2h at 600 DEG C, obtain gamma oxidation Aluminum nano material.
The thing of gained γ-aluminum oxyhydroxide and gama-alumina is mutually same as in Example 1 (accompanying drawing 9 and accompanying drawing 11), but pattern For Folium Bambusae shape nanometer flower structure (accompanying drawing 10 and accompanying drawing 11).
Embodiment 4
Reaction condition is same as embodiment 1, only reaction temperature is promoted to 100 DEG C.After reaction, naturally cool to room temperature.Produce Thing, through filtering, with deionized water and absolute ethanol washing, is dried 3h in the vacuum drying oven of 80 DEG C, obtains γ-hydroxyl oxidize Aluminum nano material.γ-aluminum oxyhydroxide is placed in ceramic crucible, in muffle furnace, calcines 2h at 600 DEG C, obtain gamma oxidation Aluminum nano material.
Thing (accompanying drawing 12 and the accompanying drawing mutually same as in Example 1 of gained γ-aluminum oxyhydroxide presoma and gama-alumina 14), but pattern be acicular nanometer flower (accompanying drawing 13 and accompanying drawing 15).
Embodiment 5
Reaction condition is same as embodiment 1, only by chlorination 1-butyl-2, and 3-methylimidazole ([Bdmim] Cl) ionic liquid Consumption be respectively set as: 0,2,4,8,10mmol.After reaction, naturally cool to room temperature.Product through filtering, with deionized water and Absolute ethanol washing, is dried 3h in the vacuum drying oven of 80 DEG C, obtains end-product.
The thing of end-product is summarized in subordinate list 1 mutually.Products therefrom thing is mutually same as in Example 1, but when being not added with ionic liquid, produces Thing is block (accompanying drawing 16d), and when ionic liquid addition is 2-8mmol, product is nanostructured (accompanying drawing 16a-c), but works as When the ionic liquid scale of construction increases to 10mmol, product volume production thing amount significantly reduces.
Subordinate list 1 embodiment 5 synthesis condition and product thing phase.
Embodiment 6
Reaction condition is same as embodiment 1, only by chlorination 1-butyl-2, and 3-methylimidazole ([Bdmim] Cl) ionic liquid Respectively with same amount of 1-ethyl-, 3-Methylimidazole. ([Emim] Cl), 1-butyl-2,3-methylimidazole ([Bdmim] NO3)、 1-octyl group-, 3-Methylimidazole. ([C8Mim] Cl), 1-16 alkyl-, 3-Methylimidazole. ([C16Mim] Cl) ionic liquid replacement.From So it is cooled to room temperature.Product, through filtering, with deionized water and absolute ethanol washing, is dried 3h in the vacuum drying oven of 80 DEG C, Obtain end-product.
End-product thing is same as embodiment 1, be γ-AlOOH, the 1-octyl group of orthohormbic structure-, 3-Methylimidazole. ([C8Mim] Cl) prepare the pattern (accompanying drawing 17) of product, it is still nano tube structure similar to Example 1, but ([C16mim]Cl) During for ionic liquid, product is then changed into submicron particles.
Embodiment 7
Reaction condition is same as embodiment 1, only will be adjusted to 2 the response time, 3.5,6,8h.Naturally cool to room temperature.Product Through filtering, with deionized water and absolute ethanol washing, the vacuum drying oven of 80 DEG C is dried 3h, obtains end-product.
End-product thing is as shown in subordinate list 2.When response time reaches 6h, product is pure mutually orthogonal γ-AlOOH, with enforcement Example 1 is identical.Extend the response time, then degree of crystallinity and the draw ratio of product all can increase, and pattern is more uniformly distributed.
Under the conditions of subordinate list 2 embodiment 7, the thing phase of each product and appearance.
Response time/h Product morphology (SEM) Thing phase
2.5 Nanoparticle (CH3COO)2Al(OH)
3.5 The nanoparticle that size is less (CH3COO)2Al(OH)+γ-AlOOH
6 A small amount of nanometer rods occurs γ-AlOOH (on a small quantity)+(CH3COO)2Al(OH)
8 The nano bar-shape thing of draw ratio γ-AlOOH
10 The nano bar-shape thing of relatively high length-diameter ratio γ-AlOOH
Embodiment 8
Reaction condition is same as embodiment 1, but reaction temperature is respectively as follows: 100 DEG C, 130 DEG C, 150 DEG C, 180 DEG C and 200 DEG C. Naturally cool to room temperature.Product, through filtering, with deionized water and absolute ethanol washing, is dried in the vacuum drying oven of 80 DEG C 3h, obtains end-product.γ-aluminum oxyhydroxide presoma is placed in ceramic crucible, in muffle furnace, calcines 2h at 600 DEG C, obtain Gama-alumina nano material.
The thing of γ-aluminum oxyhydroxide presoma and gama-alumina is same as embodiment 1.Use the ratio of BET method test product Surface area, result is as shown in subordinate list 3, and product is respectively provided with higher specific surface area.
Under the conditions of subordinate list 3 embodiment 7, the specific surface area of γ-aluminum oxyhydroxide presoma calcined product.
Reaction temperature/DEG C Calcined product thing phase Product morphology Specific surface area/m2/g
100 Cube γ-Al2O3 Needle-like 296.1
130 Cube γ-Al2O3 Tubulose 285.4
150 Cube γ-Al2O3 Folium Bambusae shape 158.5
180 Cube γ-Al2O3 Banding 104.2
200 Cube γ-Al2O3 Banding 63.5

Claims (9)

1., under an ionic liquid auxiliary water heat condition, drive the presoma eston in aluminum by introducing bivalent metal ion Decompose, prepare realizing the γ-AlOOH under temperate condition, and the γ-Al of identical pattern can be converted into2O3Nanostructured, it is special Levy and be that preparation process is as follows:
1) aluminium salt, zinc salt and potassium acetate are dissolved in deionized water successively, stir;2) add in above-mentioned solution a certain amount of Ionic liquid, after stirring, be transferred in reactor, and with different temperatures under react a period of time.After reaction terminates, cold But to room temperature, centrifugation, with deionized water and absolute ethanol washing alternately washing, it is dried.Obtain γ-AlOOH nano material; 3) it is placed in tube furnace calcining by preparing product, obtains the γ-Al that crystallization is preferable, specific surface area is higher2O3Nanostructured.
A kind of ionic liquid auxiliary hydrothermal condition under, preparation γ-AlOOH nanostructured and It is converted into γ-Al2O3The method of nanostructured, it is characterised in that: use the decomposition containing aluminum presoma that bivalent metal ion drives Reaction, bivalent metal ion can use the first transition metal ion and alkaline-earth metal ions.
A kind of ionic liquid auxiliary hydrothermal condition under, preparation γ-AlOOH nanostructured and It is converted into γ-Al2O3The method of nanostructured, it is characterised in that: described aluminium salt be aluminum halide, aluminum sulfate, aluminum nitrate, Alumen and The soluble salt of the aluminum such as aluminum acetate.
A kind of ionic liquid auxiliary hydrothermal condition under, preparation γ-AlOOH nanostructured and It is converted into γ-Al2O3The method of nanostructured, it is characterised in that: described ionic liquid is glyoxaline ion liquid, comprises difference The ionic liquid that substituent group and different anions combination are formed.
A kind of ionic liquid auxiliary hydrothermal condition under, preparation γ-AlOOH nanostructured and It is converted into γ-Al2O3The method of nanostructured, it is characterised in that: the mol ratio of described aluminium salt and ionic liquid is 1: 0.2~1: 10;The mol ratio of aluminium salt and divalent metal salt is 1: 0.1~1: 2;Aluminium salt concentration is 0.05~5mol/L.
6. prepare γ-AlOOH nanostructured and be converted into γ-Al2O3The method of nanostructured, it is characterised in that: described water Thermal response temperature is 70~200 DEG C;Response time is 4-16 hour;Under low temperature (70-130 DEG C), can prepare needle-like γ- AlOOH one-dimensional nano structure and nanotube, under high temperature (130-200 DEG C), product is also lamellar or banding γ-AlOOH structure, and Reaction temperature and the degree of crystallinity of response time scalable product and specific surface area.
A kind of ionic liquid auxiliary hydrothermal condition under, preparation γ-AlOOH nanostructured and It is converted into γ-Al2O3The method of nanostructured, it is characterised in that: described γ-AlOOH presoma mode of washing for spend respectively from Sub-water and dehydrated alcohol alternately washing 2-3 time, baking temperature 60-80 DEG C.
A kind of ionic liquid auxiliary hydrothermal condition under, preparation γ-AlOOH nanostructured and It is converted into γ-Al2O3The method of nanostructured, it is characterised in that: the calcining heat of described γ-AlOOH presoma is 400-700 DEG C, calcination time is 2-6 hour.
γ-AlOOH that the most according to claim 1, prepared by method and γ-Al2O3The application of nanostructured, it is characterised in that: It is mainly used in catalysis, absorption, pottery and field of photoelectric devices.
CN201610186410.9A 2016-03-25 2016-03-25 Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure Pending CN105948087A (en)

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* Cited by examiner, † Cited by third party
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CN107500323A (en) * 2017-07-14 2017-12-22 山东旭晟东阳新材料科技有限公司 A kind of γ phase aluminas nanotube and preparation method thereof
CN110560158A (en) * 2019-08-30 2019-12-13 浙江工业大学 High-dispersion supported ionic liquid-palladium aluminum oxide catalyst and preparation method and application thereof
CN114223670A (en) * 2021-11-23 2022-03-25 江苏科技大学 Antibacterial agent and preparation method thereof
CN116273018A (en) * 2021-12-06 2023-06-23 苏州市清泽环境技术有限公司 Al@Al based on aluminum mud hazardous waste 2 O 3 Preparation method of micro-nano catalytic material

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