CN101367535B - Hydrothermal method for preparing gamma-AL2O3 hollow microsphere polishing material without mould plate - Google Patents

Hydrothermal method for preparing gamma-AL2O3 hollow microsphere polishing material without mould plate Download PDF

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CN101367535B
CN101367535B CN2008101972081A CN200810197208A CN101367535B CN 101367535 B CN101367535 B CN 101367535B CN 2008101972081 A CN2008101972081 A CN 2008101972081A CN 200810197208 A CN200810197208 A CN 200810197208A CN 101367535 B CN101367535 B CN 101367535B
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polishing material
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tiny balloon
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CN101367535A (en
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余家国
蔡卫权
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Wuhan University of Technology WUT
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Abstract

The invention relates to a hydrothermal method for preparing Gamma-Al2O3 hollow micro balloon polishing material without a template, which comprises the following steps: firstly, urea is added in aluminum-salt distilled water solution; after being uniformly mixed, the mixed solution is moved into a hydrothermal reactor to perform the hydrothermal reaction, so as to get the hydrothermal product; secondly, after the hydrothermal product is cooled down and pumped and filtered in vacuum, the filtered mass is washed by water to be neutral, and then the filtered mass is washed by absolute ethyl alcohol and filtered; the obtained filtered mass is dried for six hours in vacuum at the temperature of 80 DEG C, so as to get the pseudoboehm hollow micro balloon. Thirdly, the obtained pseudoboehm hollow micro balloon is calcined more than 3 hours at the temperature of 400 to 700 DEG C, so that the Gamma-Al2O3 hollow micro balloon polishing material can be obtained. The method is free from organic template agent, and has lower requirement on the reaction condition, and is simple to be operated, and has low cost.

Description

A kind of no template prepares γ-Al 2O 3The hydrothermal method of hollow microsphere polishing material
Technical field
The present invention relates to the preparation of chemical aluminum oxide, relate in particular to a kind of no template and prepare γ-Al 2O 3The hydrothermal method of hollow microsphere polishing material.
Background technology
Aluminum oxide comprises α-Al 2O 3And transition state of alumina, the latter is that various white lakes finally are converted into stable state α-Al 2O 3Intermediate product.Research shows that transition state of alumina has γ-Al at least 2O 3, η-Al 2O 3, ρ-Al 2O 3, χ-Al 2O 3, κ-Al 2O 3, δ-Al 2O 3And θ-Al 2O 3Seven kinds of forms; New transition state of alumina is [Levin I in finding and confirming still; Brandon D.Metastable alumina polymorphs:crystal structures and transition sequences.J.Am.Ceram.Soc., 1998,81 (8): 1995-2012].In various transition state of alumina, by pseudo-boehmite (γ-AlOOHnH 2O, n=0.08～0.62) γ-Al that specific surface area is higher and pore volume is bigger that roasting forms between 400～700 ℃ 2O 3Be widely used as polishing material, support of the catalyst, catalyzer and sorbent material in many industries such as machinery, petrochemical compleies.
Good characteristics such as the aluminum oxide tiny balloon has that density is low, surface-area is big, stability and Surface Permeability height have a extensive future in fields such as polishing material, support of the catalyst and sorbent materials.[Kimberly A D such as Kimberly; Andrew R B.Aflexible route to high strength α-alumina and aluminate spheres.J.Mater.Science; 2003,38:2673-2678] be that the polystyrene microsphere of 3 μ m and 50～80 μ m is a template once with diameter, at its surface-coated aluminium salt colloid; Be translated into amorphous alumina 220 ℃ of heating then; Remove the template of microballoon nexine through toluene wash, obtain the amorphous alumina tiny balloon, after 1000 ℃ of roastings have formed particle diameter at 1～80 μ m, the hardness α-Al near corundum 2O 3Tiny balloon.[Zolt á n K such as Zoltan; J á no S.Hollow alumina microspheres prepared by RF thermalplasma.Powder Technol.; 2003,132:211-215] be raw material then with bayer's process product gipsite, adopt radio frequency thermal plasma revulsion; Improve the heat passage situation of Ar plasma body through adding some diatomic gas, prepared the aluminum oxide tiny balloon of particle diameter about 30～80 μ m.People such as Wu [Wu X Y, Wang D B, Hu Z S, Gu G H.Synthesis of γ-AlOOH (γ-Al 2O 3) self-encapsulated and hollow architectures.Mater.Chem.Phys.; 2008; 109; 560-564.] to adopt compound amphiphilic block copolymer PS-b-PHEA be inductor, at 150 ℃ of following hydro-thermal Tai-Ace S 150 and urea soln 24h, made boehmite and the γ-Al of particle diameter about 4 μ m 2O 3Tiny balloon.
CN 1884083A discloses a kind of preparation method of nano alumina hollow ball structure, with AlCl 3With the alcoholic acid mixing solutions by N 2Be written in the vaporizer and vaporize, mix with 200～350 ℃ air and hydrogen then, hydrolysis in 1200～2500 ℃ combustion chamber makes the nano alumina hollow ball structure.
The defective of aforesaid method is: need to add organic formwork agent or inductor, or reaction conditions has relatively high expectations, or complicated operation etc.And be that raw material prepares the aluminum oxide tiny balloon through liquid phase method with the inorganic aluminate of cheapness, especially prepare γ-Al through direct hydro-thermal-sinter process 2O 3The method of tiny balloon is not also seen document and patent public reported so far.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of no template to prepare γ-Al 2O 3The hydrothermal method of hollow microsphere polishing material, this method need not to add organic formwork agent, and reaction conditions is less demanding, and is simple to operate, and cost is low.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
A kind of no template prepares γ-Al 2O 3The hydrothermal method of hollow microsphere polishing material, concrete steps comprise:
The first step, in the distilled water solution of aluminium salt, add urea, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, hydrothermal product;
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake more than 6 hours, can obtain the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings again.
The 3rd the step, gained pseudo-boehmite tiny balloon more than 3 hours, is made γ-Al 400～700 ℃ of following roastings 2O 3Hollow microsphere polishing material.
Said aluminium salt is one or both the combination in exsiccated ammonium alum and the potassium aluminium sulfate.
In the distilled water solution of said aluminium salt, Al 3+Concentration be 0.005～0.30mol/L.
Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 1～3 hour.
In the such scheme, said urea and Al 3+Mol ratio be 2～2.5: 1.
The inventive method is a raw material with aluminium salt, with the precipitation agent of urea as aluminium salt distilled water solution, adopts no template hydrothermal preparation to go out pseudo-boehmite and γ-Al 2O 3Tiny balloon, cost is low, has broken through the defective that the conventional template method prepares hollow oxide microsphere.Compound method of the present invention has that technology is simple, gentleness, product epigranular, pore volume are big relatively, specific surface area is higher and the hollow structure high repeatability and other advantages for hydrothermal condition, has shown that it is used as the potential application foreground of polishing material, support of the catalyst, catalyzer and sorbent material etc. in industries such as machinery, petrochemical compleies.
Being also advantageous in that of the inventive method:
1, aluminium salt is one or more the combination in Tai-Ace S 150, exsiccated ammonium alum and the potassium aluminium sulfate, Al in the distilled water solution 3+Concentration be 0.005～0.30mol/L, can make aluminium source concentration higher, can guarantee further that product epigranular, pore volume are bigger.
2, hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 1～3 hour, can guarantee that hydro-thermal reaction is abundant.
γ-the Al of the present invention's preparation 2O 3Hollow microsphere polishing material also can be at petrochemical industry as support of the catalyst, catalyzer and sorbent material etc.
Description of drawings
Fig. 1 is ESEM (Scanning electron microscopy, the SEM) photo of no template hydrothermal preparation pseudo-boehmite tiny balloon.
Fig. 2 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Fig. 3 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Fig. 4 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Fig. 5 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Fig. 6 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Fig. 7 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Fig. 8 is no template hydrothermal preparation γ-Al 2O 3The SEM photo of tiny balloon.
Embodiment
The inventive method embodiment 1:
The first step, at Tai-Ace S 150 (Al 2(SO 4) 318H 2O) add urea in the distilled water solution, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, get hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.30mol/L, said urea and Al 3+Mol ratio be 2: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 3 hours.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, again with filter cake with absolute ethanol washing once and suction filtration; The gained filter cake obtains the surface and is that the hydrated alumina tiny balloon of flower-like structure, particle diameter are 1～5 μ m 80 ℃ of following vacuum-dryings 8 hours; See Fig. 1; (X-ray diffraction XRD) analyzes to pseudo-boehmite thing phase, promptly obtains the pseudo-boehmite tiny balloon through X-ray powder diffraction.
The 3rd the step, with gained pseudo-boehmite tiny balloon 400 ℃ of following roastings 4 hours, make γ-Al 2O 3Hollow microsphere polishing material.Seeing Fig. 2, is γ-Al through XRD analysis 2O 3, its specific surface area and pore volume are respectively 124.0m 2/ g and 0.20cm 3/ g.
The inventive method embodiment 2:
The first step, at potassium aluminium sulfate (KAl (SO 4) 212H 2O) add urea in the distilled water solution, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, get hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.005mol/L, said urea and Al 3+Mol ratio be 2: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 3 hours.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake obtains the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings 6 hours again.The particle diameter of pseudo-boehmite tiny balloon is 1～5 μ m.
The 3rd the step, with gained pseudo-boehmite tiny balloon 500 ℃ of following roastings 4 hours, make γ-Al 2O 3Hollow microsphere polishing material.Seeing Fig. 3, is γ-Al through the X-ray powder diffraction XRD analysis 2O 3The thing phase, its specific surface area and pore volume are respectively 215.3m 2/ g and 0.47cm 3/ g.
The inventive method embodiment 3:
The first step, at Tai-Ace S 150 (Al 2(SO 4) 318H 2O) add urea in the distilled water solution, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, get hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.05mol/L, said urea and Al 3+Mol ratio be 2.5: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 3 hours.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake obtains the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings 8 hours again.The particle diameter of pseudo-boehmite tiny balloon is 1～5 μ m.
The 3rd the step, with gained pseudo-boehmite tiny balloon 700 ℃ of following roastings 4 hours, make γ-Al 2O 3Hollow microsphere polishing material.Seeing Fig. 4, is γ-Al through XRD analysis 2O 3The thing phase, its specific surface area and pore volume are respectively 166.3m 2/ g and 0.54cm 3/ g.
The inventive method embodiment 4:
The first step, at Tai-Ace S 150 (Al 2(SO 4) 318H 2O) add urea in the distilled water solution, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, get hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.20mol/L, said urea and Al 3+Mol ratio be 2: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 1 hour.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake obtains the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings 8 hours again.The particle diameter of pseudo-boehmite tiny balloon is 1～5 μ m.
The 3rd the step, with gained pseudo-boehmite tiny balloon 500 ℃ of following roastings 4 hours, make γ-Al 2O 3Hollow microsphere polishing material.Seeing Fig. 5, is γ-Al through XRD analysis 2O 3The thing phase, its specific surface area and pore volume are respectively 154.2m 2/ g and 0.42cm 3/ g.
The inventive method embodiment 5:
The first step, at Tai-Ace S 150 (Al 2(SO 4) 318H 2O) add urea in the distilled water solution, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, get hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.20mol/L, said urea and Al 3+Mol ratio be 2.3: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 2 hours.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake obtains the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings 6 hours again.
The 3rd the step, with gained pseudo-boehmite tiny balloon 550 ℃ of following roastings 3 hours, make γ-Al 2O 3Hollow microsphere polishing material.See Fig. 6, the particle diameter of microballoon is 1～5 μ m, is γ-Al through XRD analysis 2O 3The thing phase, its specific surface area and pore volume are respectively 146.3m 2/ g and 0.34cm 3/ g.
The inventive method embodiment 6:
The first step, in the distilled water solution of Tai-Ace S 150, exsiccated ammonium alum, potassium aluminium sulfate compsn, add urea, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.20mol/L, said urea and Al 3+Mol ratio be 2: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 3 hours.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake obtains the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings 6 hours again.
The 3rd the step, with gained pseudo-boehmite tiny balloon 500 ℃ of following roastings 4 hours, make γ-Al 2O 3Hollow microsphere polishing material.See Fig. 7, the particle diameter of microballoon is 1～5 μ m, is γ-Al through XRD analysis 2O 3The thing phase, its specific surface area and pore volume are respectively 139.1m 2/ g and 0.37cm 3/ g.
The inventive method embodiment 7:
The first step, at exsiccated ammonium alum (AlNH 4(SO 4) 212H 2O) add urea in the distilled water solution, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, get hydrothermal product.The distilled water solution of said aluminium salt is 70ml, Al 3+Concentration be 0.005mol/L, said urea and Al 3+Mol ratio be 2: 1.Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 3 hours.
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake obtains the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings 6 hours again.
The 3rd the step, with gained pseudo-boehmite tiny balloon 550 ℃ of following roastings 3 hours, make γ-Al 2O 3Hollow microsphere polishing material.See Fig. 8, the particle diameter of microballoon is 1～5 μ m, is γ-Al through XRD analysis 2O 3The thing phase, its specific surface area and pore volume are respectively 161.2m 2/ g and 0.60cm 3/ g.
The above is merely preferred embodiment of the present invention; In fact aluminium salt all can be used as the raw material of the inventive method; Above embodiment is not in order to restriction the present invention, and common variation that those skilled in the art carries out in technical scheme scope of the present invention and replacement all should be included in protection scope of the present invention.

Claims (2)

1. a no template prepares γ-Al 2O 3The hydrothermal method of hollow microsphere polishing material, concrete steps comprise:
The first step, in the distilled water solution of aluminium salt, add urea, be transferred to after stirring and carry out hydro-thermal reaction in the water heating kettle, hydrothermal product;
Second step, hydrothermal product be through cooling, behind the vacuum filtration, and first water washing leaching cake is to neutral, and with filter cake with absolute ethanol washing once and suction filtration, the gained filter cake more than 6 hours, can obtain the pseudo-boehmite tiny balloon 80 ℃ of following vacuum-dryings again;
The 3rd the step, gained pseudo-boehmite tiny balloon more than 3 hours, is made γ-Al 400～700 ℃ of following roastings 2O 3Hollow microsphere polishing material;
Said aluminium salt is one or both the combination in exsiccated ammonium alum and the potassium aluminium sulfate;
In the distilled water solution of said aluminium salt, Al 3+Concentration be 0.005～0.30mol/L;
Said hydro-thermal reaction is airtight hydro-thermal reaction, and hydrothermal temperature is 160～180 ℃, and the reaction times is 1～3 hour.
2. hydrothermal method according to claim 1 is characterized in that: said urea and Al 3+Mol ratio be 2～2.5: 1.
CN2008101972081A 2008-10-09 2008-10-09 Hydrothermal method for preparing gamma-AL2O3 hollow microsphere polishing material without mould plate Expired - Fee Related CN101367535B (en)

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