CN112707423A - Preparation method of self-assembled octahedral particles of polycrystalline alumina - Google Patents
Preparation method of self-assembled octahedral particles of polycrystalline alumina Download PDFInfo
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- CN112707423A CN112707423A CN201911020901.6A CN201911020901A CN112707423A CN 112707423 A CN112707423 A CN 112707423A CN 201911020901 A CN201911020901 A CN 201911020901A CN 112707423 A CN112707423 A CN 112707423A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000002245 particle Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 17
- 150000001412 amines Chemical class 0.000 claims abstract description 14
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- 239000011343 solid material Substances 0.000 claims abstract description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 24
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- 238000001338 self-assembly Methods 0.000 claims description 5
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- -1 lanthanum modified pseudo-boehmite Chemical class 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 23
- 239000012071 phase Substances 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000002524 electron diffraction data Methods 0.000 description 3
- 239000012634 fragment Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
- C01F7/025—Granulation or agglomeration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
- C01F7/023—Grinding, deagglomeration or disintegration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of self-assembled octahedral particles of polycrystalline alumina, which comprises the following steps: (1) fully adsorbing the organic amine solution by the calcined alumina precursor powder by an isometric impregnation method, and then treating the powder by using a high-energy ball mill; (2) drying the material obtained in the step (1), and screening the material with proper granularity; (3) carrying out closed hydrothermal treatment on the material screened in the step (2); in the closed system, the device is divided into an upper part and a lower part: the upper part is an alumina precursor solid material, the lower part is a liquid phase, the solid phase and the liquid phase are not directly contacted, gas-solid reaction is carried out at high temperature, and after the reaction is finished, the product is obtained by drying and roasting. The method is simple and environment-friendly, and the aluminum oxide material synthesized by the method has wide application prospects in the fields of catalysis and adsorption.
Description
Technical Field
The invention belongs to the field of inorganic material preparation, and particularly relates to a preparation method of self-assembled octahedral particles of polycrystalline alumina.
Background
Alumina is a widely used catalyst support material, and crystal faces exposed by surface properties of the alumina are directly related and have important influence on the performance of the catalyst. For gamma-alumina, the (110) lattice plane is thermodynamically most stable and is usually preferentially exposed. The (111) crystal face and the (100) crystal face of the aluminum oxide have different atomic arrangement and chemical properties from the (110) crystal face, so that special interface properties can be obtained by regulating the crystal face of the aluminum oxide. However, the situation in which the aluminum oxide (110) crystal face predominates is hardly easily changed as a whole.
The existing research shows that the single crystal alumina crystal grains mainly expose { 110 } crystal face family and { 111 } crystal face family, the { 110 } crystal face family accounts for 70.4%, and the { 111 } crystal face family accounts for 29.6%. The crystal plane distribution ratio of alumina crystal grains is difficult to regulate due to the intrinsic constraint mechanism of crystal habit, and the { 110 } crystal plane family is always in a dominant position.
[ petroleum refining and chemical engineering, 2013, 44 (9): 47-50 ] regulating and controlling the crystal face distribution of the aluminum oxide single crystal by introducing sodium nitrate, wherein the obtained crystal grains are still mainly the (110) crystal face.
CN200910011627.6, cn200910206229.x and CN200910011626.1 synthesized rod-shaped alumina assembly particles by a supersolubilization micelle method. The self-assembly method has no obvious effect on the distribution ratio of the oxidation crystal face.
[ chemical bulletin of fuel, 2013, 41 (10): 1262-1267 aluminum chloride is used as precursor, hexagonal prism shaped polycrystal gamma-alumina polycrystal particles are prepared by a hydrothermal method in an ammonia water medium, and the obtained product contains a large amount of chlorine element, and needs to be removed by a special means, which is not beneficial to green utilization in industry.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of self-assembled octahedral particles of polycrystalline alumina, the invention uses organic amine of a specific type as a self-assembly regulating agent to enable an alumina precursor to generate self-assembly action under a certain chemical environment to form an octahedral morphology structure, and the method is simple, green and environment-friendly.
The preparation method of the polycrystalline alumina self-assembled octahedral particles comprises the following steps:
(1) fully adsorbing the organic amine solution by the calcined alumina precursor powder by an isometric impregnation method, and then treating the powder by using a high-energy ball mill;
(2) drying the material obtained in the step (1), and screening the material with proper granularity;
(3) carrying out closed hydrothermal treatment on the material screened in the step (2); in the closed system, the device is divided into an upper part and a lower part: the upper part is solid material, the lower part is organic amine water solution, the solid phase and the liquid phase are not directly contacted, gas-solid reaction is carried out at high temperature, and after the reaction is finished, the product is obtained by drying and roasting.
In the method of the present invention, the alumina precursor in step (1) refers to pseudo-boehmite and pseudo-boehmite powder modified by various elements such as silicon, boron, titanium, magnesium, lanthanum, etc.
In the method, the roasting conditions of the alumina precursor in the step (1) are as follows: roasting at 250-450 ℃ for 1-12 hours; the preferred firing conditions are: baking at 300-450 deg.C for 2-8 hr.
In the method, the high-energy ball milling treatment in the step (1) is carried out to obtain powder granularity of 5000-. The operating conditions of the high-energy ball mill are flexibly adjusted by taking the powder granularity meeting the requirements as a standard.
In the method, the organic amine in the step (1) is one or more of ethanolamine, diethanolamine, triethanolamine, aniline, diphenylamine, benzidine or o-phenylenediamine. The adsorption capacity of the organic amine is 1-20% of the calcined mass of the alumina precursor, and preferably 5-15%. The concentration of the organic amine solution can be reasonably adjusted according to specific adsorption conditions, and the solvent of the organic amine solution can be water and/or low-carbon alcohol.
In the method, the drying condition in the step (2) is 60-120 ℃, and the drying time is 2-24 hours.
In the method, the closed hydrothermal conditions in the step (3) are as follows: hydrothermal treatment is carried out for 12 to 96 hours at the temperature of between 100 and 250 ℃, and the hydrothermal time is preferably 24 to 72 hours.
In the method of the present invention, the concentration of the aqueous organic amine solution in the lower part of step (3) is 1 to 300 g/L, preferably 50 to 200 g/L.
In the method, the drying temperature in the step (3) is not more than 200 ℃, preferably not more than 120 ℃, and the drying degree is the constant weight of the material at the drying temperature. The roasting conditions are as follows: baking at 500-700 ℃ for 1-24 hours.
The alumina self-assembly particles prepared by the method have a hexagonal prism-shaped octahedron stereo morphology, 8 surfaces outside the particles are divided into 4 groups, every two surfaces of each group are opposite and parallel or approximately parallel, the 4 groups of surfaces are intersected and sealed to form an octahedron, and the ratio of the height of a prism to the longest diagonal line of the cross section of the prism is 2-15. The material has wide application prospect in the fields of adsorption and catalysis.
Drawings
FIG. 1 is a scanning electron micrograph of octahedral alumina particles prepared in example 1.
FIG. 2 is an electron diffraction spectrum of the octahedral alumina particles prepared in example 1.
Fig. 3 is an XRD spectrum of the octahedral alumina particles prepared in example 1.
Detailed Description
The process of the present invention is illustrated in detail by the following examples. The octahedral alumina particle size is measured according to scanning electron microscope images. Randomly measuring the heights of 20 particles, and taking the average value as the height value of the particles; the small crystal grains constituting the polyhedral particles are observed by a transmission electron microscope to observe the size range of the particles. The crystal form is characterized by X-ray diffraction. Electron diffraction spectra were collected by transmission electron microscopy.
Example 1
15 g of SB powder is roasted and ground into micro powder by a ball mill, powder with about 5000 meshes is selected to prepare aniline solution, and then the aniline solution is adsorbed on the alumina precursor powder by an isovolumetric impregnation method, wherein the dosage of the aniline is 4 percent of the dosage of the roasted alumina precursor. After drying at 120 ℃, the material is placed in a closed system, the lower part of the closed system is 25g/L aniline solution, the upper part of the closed system is the treated alumina precursor, and the solid phase is not directly contacted with the liquid phase.
Heating the closed system to 250 ℃, and carrying out hydrothermal treatment for 24 hours. And naturally cooling to take out the product, drying at 120 ℃, and roasting at 550 ℃ for 4 hours to obtain the product. The observation of a scanning electron microscope shows that the product is hexagonal prism-shaped octahedron particles and has an approximate regular octahedron stereo morphology, 8 surfaces outside the particles are divided into 4 groups, every two surfaces of each group are opposite and parallel or approximately parallel, and the 4 groups of surfaces are intersected and sealed to form the octahedron particles. The XRD result of the product shows that the phase state is gamma phase. The electron diffraction pattern of the sample fragment is annular, indicating a polycrystalline structure. The ratio of the height of the particle column to the diameter of the column (maximum) is about 9.
Example 2
15 g of SB powder is roasted and ground into micro powder by a ball mill, powder with about 10000 meshes is selected to prepare aniline solution, and then the aniline solution is adsorbed on the alumina precursor powder by an isovolumetric impregnation method, wherein the dosage of the aniline is 2.5 percent of the dosage of the roasted alumina precursor. After drying at 120 ℃, the material is placed in a closed system, the lower part of the closed system is 20g/L aniline solution, the upper part of the closed system is the treated alumina precursor, and the solid phase is not directly contacted with the liquid phase.
Heating the closed system to 200 ℃, and carrying out hydrothermal treatment for 36 hours. And naturally cooling to take out the product, drying at 120 ℃, and roasting at 550 ℃ for 4 hours to obtain the product. The observation of a scanning electron microscope shows that the product is hexagonal prism-shaped octahedron particles and has an approximate regular octahedron stereo morphology, 8 surfaces outside the particles are divided into 4 groups, every two surfaces of each group are opposite and parallel or approximately parallel, and the 4 groups of surfaces are intersected and sealed to form the octahedron particles. The XRD result of the product shows that the phase state is gamma phase. The electron diffraction pattern of the sample fragment is annular, indicating a polycrystalline structure. The ratio of the height of the particle column to the diameter of the column (maximum) is about 7.
Example 3
15 g of silicon modified SB powder is roasted and ground into micro powder by a ball mill, powder with about 20000 meshes is selected to prepare ethanolamine solution, and then the ethanolamine solution is adsorbed on alumina precursor powder by an isovolumetric impregnation method, wherein the dosage of aniline is 6 percent of the dosage of the calcined alumina precursor. After drying at 120 ℃, the material is placed in a closed system, the lower part of the closed system is 20g/L aniline solution, the upper part of the closed system is the treated alumina precursor, and the solid phase is not directly contacted with the liquid phase.
Heating the closed system to 200 ℃, and carrying out hydrothermal treatment for 12 hours. And naturally cooling to take out the product, drying at 120 ℃, and roasting at 550 ℃ for 4 hours to obtain the product. The observation of a scanning electron microscope shows that the product is hexagonal prism-shaped octahedron particles and has an approximate regular octahedron stereo morphology, 8 surfaces outside the particles are divided into 4 groups, every two surfaces of each group are opposite and parallel or approximately parallel, and the 4 groups of surfaces are intersected and sealed to form the octahedron particles. The XRD result of the product shows that the phase state is gamma phase. The electron diffraction pattern of the sample fragment is annular, indicating a polycrystalline structure. The ratio of the height of the particle column to the diameter of the column (maximum) is about 12.
Comparative example 1
According to the chemical journal of fuel, 2013, 41 (10): 1262-1267 ] prismatic alumina octahedron is prepared with aluminum chloride as material. The obtained product is tested to contain a large amount of chlorine element, and if the chlorine element is removed, a large amount of acidic water is consumed, so that the environmental pollution is caused. The process of the present invention for producing prismatic alumina uses a starting chlorine content which is present only as an impurity and the resulting product does not require additional dechlorination.
Claims (10)
1. A preparation method of self-assembled octahedral particles of polycrystalline alumina is characterized by comprising the following steps: (1) fully adsorbing the organic amine solution by the calcined alumina precursor powder by an isometric impregnation method, and then treating the powder by using a high-energy ball mill; (2) drying the material obtained in the step (1), and screening the material with proper granularity; (3) carrying out closed hydrothermal treatment on the material screened in the step (2); in the closed system, the device is divided into an upper part and a lower part: the upper part is solid material, the lower part is organic amine water solution, the solid phase and the liquid phase are not directly contacted, gas-solid reaction is carried out at high temperature, and after the reaction is finished, the solid phase is dried and roasted to obtain the product.
2. The method of claim 1, wherein: the alumina precursor in the step (1) is pseudo-boehmite or a silicon, boron, titanium, magnesium and lanthanum modified pseudo-boehmite powder.
3. The method of claim 1, wherein: the roasting conditions of the alumina precursor in the step (1) are as follows: the roasting temperature is 250 ℃ and 450 ℃, and the roasting time is 1-12 hours.
4. The method of claim 1, wherein: the high-energy ball mill in the step (1) is used for processing to obtain powder granularity of 5000-20000 meshes.
5. The method of claim 1, wherein: the organic amine in the step (1) is one or more of ethanolamine, diethanolamine, triethanolamine, aniline, diphenylamine, benzidine or o-phenylenediamine.
6. The method of claim 1, wherein: the adsorption amount of the organic amine in the step (1) is 1-20% of the mass of the calcined alumina precursor, and is preferably 5-15%.
7. The method of claim 1, wherein: the drying conditions in the step (2) are as follows: the drying temperature is 60-120 ℃, and the drying time is 2-24 hours.
8. The method according to claim 1, characterized in that: the closed hydrothermal condition of the step (3) is as follows: hydrothermal treatment at 100-250 deg.c for 12-96 hr.
9. The method of claim 1, wherein: the concentration of the organic amine aqueous solution at the middle lower part of the step (3) is 1-300 g/L, preferably 50-200 g/L.
10. An alumina self-assembly particle prepared by the method of any one of claims 1 to 9, characterized in that: the octahedron has a hexagonal prism-shaped octahedron stereo morphology, 8 surfaces outside the particles are divided into 4 groups, every two surfaces of each group are opposite and parallel or approximately parallel, the 4 groups of surfaces are intersected and sealed to form the octahedron, and the ratio of the height of a prism to the longest diagonal of the cross section of the prism is 2-15.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4610866A (en) * | 1985-10-11 | 1986-09-09 | Battelle Memorial Institute | Method for producing beta-aluminas |
| CN104556178A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Preparation method for polycrystal gamma-aluminum oxide |
| CN104556163A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Prism-shaped poly-crystal gamma-alumina and preparation method thereof |
-
2019
- 2019-10-25 CN CN201911020901.6A patent/CN112707423B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4610866A (en) * | 1985-10-11 | 1986-09-09 | Battelle Memorial Institute | Method for producing beta-aluminas |
| CN104556178A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Preparation method for polycrystal gamma-aluminum oxide |
| CN104556163A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Prism-shaped poly-crystal gamma-alumina and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘冬梅等: "六棱柱状多晶γ-Al2O3的制备、表征及其形成机制研究", 《燃料化学学报》 * |
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