CN114105177A - Preparation method of sphere-like nano gamma-alumina - Google Patents
Preparation method of sphere-like nano gamma-alumina Download PDFInfo
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- CN114105177A CN114105177A CN202111616877.XA CN202111616877A CN114105177A CN 114105177 A CN114105177 A CN 114105177A CN 202111616877 A CN202111616877 A CN 202111616877A CN 114105177 A CN114105177 A CN 114105177A
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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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
- C01F7/444—Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
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- 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
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- 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
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- 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
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a preparation method of sphere-like nano gamma-alumina, which comprises the following steps: 1) taking ultrapure water for later use; 2) adding an organic or inorganic compound with low-temperature thermal decomposition property into ultrapure water for dissolving, adding an additive, and stirring to obtain a solution; 3) slowly and gradually adding boehmite powder into the solution, and stirring to obtain a mixture; 4) putting the mixture into a ball mill for ball milling; 5) drying the ball-milled mixture to obtain dry solid particles; 6) crushing the dry solid particles to obtain dry powder; and calcining the dried powder to obtain the nano gamma-alumina. The preparation method is simple and stable, has few working procedures, low requirements on equipment, few types of used raw materials, low production cost and easy absorption and treatment of tail gas; the nano gamma-alumina produced by the method is spherical-like, the particle size is 5-20nm, the particle size distribution is uniform, the particle size distribution is concentrated, and the dispersion is easy; the obtained powder has wide application range.
Description
Technical Field
The invention relates to the technical field of metal oxides, in particular to a preparation method of sphere-like nano gamma-alumina.
Background
When the particle size of the substance reaches the nanometer level, the substance has many excellent properties and characteristics, such as quantum size effect, quantum tunneling effect, surface effect and the like, and particularly, the nanometer material has the advantages of high specific surface area, easiness in processing and treatment and the like, and the properties enable the nanometer material to have many special application prospects. Alumina is an inorganic substance, of the formula Al2O3It is a high-hardness compound with a melting point of 2054 ℃ and a boiling point of 2980 ℃. Alumina exists in eleven crystal forms, and has a plurality of homogeneous and heterogeneous crystals, and mainly has three crystal forms, namely alpha-alumina, beta-alumina and gamma-alumina. The gamma-alumina is a porous solid material, has large specific surface area and pore volume, adjustable pore distribution, good thermal stability, good formability, stronger surface acidity and certain surface alkalinity, and is low in production cost and easy to obtain, so that the gamma-alumina is widely used as a new green material such as a catalyst, a catalyst carrier, an additive, an adsorbent and the like, and is a new material with wide development and application prospects. The industrial gamma-alumina is usually colorless or slightly pink cylindrical particles, has good pressure resistance, and is a common adsorbent, catalyst and catalyst carrier in petrochemical industry and petroleum refining; the deacidification agent is used for transformer oil and turbine oil in industry and is also used for chromatography; neutral strong desiccant in the laboratory; the gamma-alumina can be converted into alpha-alumina through high-temperature calcination, and secondary development and utilization are carried out. With the development of science and technology, the demand of ultrafine high-purity alumina powder is increasing at home and abroad, and higher requirements on the granularity, purity and uniformity of the high-purity alumina powder are provided.
At present, most of patent technologies adopt aluminum salts such as aluminum nitrate, aluminum ammonium sulfate, aluminum chloride and the like to carry out long-time treatment such as precipitation, electric treatment, hydrothermal treatment, grinding and the like, or further carry out ultrahigh-temperature calcination treatment at 1200-. During the preparation process, a large amount of organic substances such as various organic alcohols, ketones or lipids which are easy to volatilize and generate toxic and harmful substances are often added. And the preparation process flow is complex. In the preparation process, a lot of waste gas or high-risk waste liquid with high corrosivity, toxicity, harm and pollution is often generated, the harm to equipment and the environment is great, and the cost of the equipment and the environment is increased.
Therefore, it is important to design a simple, efficient, low-cost, pollution-free, and low-energy-consumption method for synthesizing nano gamma-alumina with uniform particle size distribution and excellent performance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of spheroidal nano gamma-alumina, which overcomes the defects in the prior art.
The technical problem to be solved by the invention is realized by the following technical scheme:
a preparation method of spheroidal nano gamma-alumina comprises the following steps:
1) taking ultrapure water, and controlling the temperature of the ultrapure water to be 5-90 ℃ for later use;
2) adding an organic or inorganic compound with low-temperature thermal decomposition property into the ultrapure water obtained in the step 1), stirring at room temperature for dissolving, adding a trace amount of additive after fully dissolving, and fully stirring to obtain a solution;
3) slowly and gradually adding boehmite powder into the solution obtained in the step 2), and continuously stirring and uniformly dispersing at room temperature until boehmite is completely added or a mixture with good uniformity is formed;
4) putting the mixture obtained in the step 3) into a ball mill for ball milling;
5) drying the mixture subjected to ball milling in the step 4) to obtain dry solid particles;
6) crushing the dry solid particles obtained in the step 5) to obtain dry powder;
7) calcining the dried powder obtained in the step 6) to obtain the nano gamma-alumina.
Preferably, in the above technical solution, the treatment manner of the ultrapure water temperature in step 1) is as follows: non-contact heat conduction in a clean environment; the temperature of the ultrapure water is 30 to 70 ℃, preferably 60 ℃.
Preferably, in the above technical solution, the organic or inorganic compound having low-temperature thermal decomposition property in step 2) is one or more of ammonium carbonate, ammonium bicarbonate, ammonium chloride, citric acid, ammonium citrate, glycine, urea or acetic acid; wherein the mass ratio of the compound to the ultrapure water is 1: (0.1-10); the additive is one or more of polyethylene glycol, ammonium polymethacrylate, oleylamine, emulsifying wax, isopropanol, stearic acid, quaternary ammonium compound and hexadecyl trimethyl ammonium bromide; wherein the mass ratio of the additive to the ultrapure water is 1 (50-1000). The continuous stirring mode is mechanical stirring at room temperature, and the effect of the continuous stirring mode is to dissolve and disperse the compound and the additive in ultrapure water uniformly.
Preferably, in the above technical solution, the boehmite in step 3) is high-purity boehmite or high-purity pseudo boehmite, preferably high-purity boehmite; the mass ratio of the boehmite to the ultrapure water is as follows: 1: (0.1-10); the stirring mode is double-cone screw planetary mechanical stirring at room temperature, and the function is as follows: 1. and 2, uniformly mixing and dispersing the boehmite, the compound in the solution and the additive to ensure that the boehmite, the compound in the solution and the additive can be effectively adhered to each other.
Preferably, in the above technical scheme, a planetary ball mill is adopted in the step 4) for ball milling, the ball milling rotation speed is 150-. The ball milling has the following functions: (1) the boehmite, the compound and the additive are mixed more finely and uniformly; (2) the attachment of large particles of the crushed boehmite, the compound and the additive can effectively prevent the occurrence of the particle agglomeration phenomenon, and is beneficial to the subsequent calcination.
Preferably, in the above technical solution, the drying manner adopted in step 5) is: oven heat drying, microwave drying, roller heat drying or spray drying at 80-110 deg.C until the water content is less than or equal to 5 wt%.
Preferably, in the above technical solution, the crushing manner adopted in step 6) is: grinding, alligator crushing, roller crushing or airflow crushing, wherein the size of the crushed solid particles is less than 1 mm.
Preferably, in the above technical scheme, the equipment used in the calcination in step 7) is a muffle furnace, a tube furnace, a rotary furnace, a crucible resistance furnace, a box furnace, a lift furnace, a shaft furnace, a trolley furnace, a mesh belt furnace, a roller kiln, a pusher kiln, a tunnel furnace, a rotary kiln or a suspension calciner, and the calcination method includes the following steps:
71) heating the temperature from room temperature to 300 ℃, wherein the heating rate is 0.1-50 ℃/min, activating the precursor, particularly the organic or inorganic compound with low-temperature thermal decomposition property in the preheating process, and dissolving or decomposing part of the compound;
72) the temperature is increased from 300 ℃ to 600 ℃, the heating rate is 0.1-50 ℃/min, organic or inorganic compounds with low-temperature thermal decomposition property are decomposed rapidly at high temperature, and the generated hot ascending air flow can break partial agglomeration or boehmite or alumina with agglomeration tendency to a certain extent; effectively preventing the growth and agglomeration of alumina, and simultaneously, the boehmite begins to carry out crystal form transformation and gradually turns to uniform and stable gamma-alumina from an amorphous form;
73) heating the temperature from 600 to 800 ℃ at a heating rate of 0.1-50 ℃/min;
74) the heat preservation temperature is 700-; the crystallization of the gamma-alumina and the further complete conversion of the crystal form are promoted by the constant temperature and the time, and the size of the gamma-alumina crystal grain is controlled.
75) Cooling with the furnace body or then quickly cooling to obtain the nano alumina.
The sphere-like nano gamma-alumina prepared by the preparation method.
An application of the sphere-like nano gamma-alumina prepared by the preparation method.
The technical scheme of the invention has the following beneficial effects:
(1) the preparation method is simple and stable, has few working procedures, low requirements on equipment, few types of used raw materials, low production cost and easy absorption and treatment of tail gas;
(2) the nano gamma-alumina produced by the method is spherical-like, the particle size is 5-20nm, the particle size distribution is uniform, the particle size distribution is concentrated, and the dispersion is easy;
(3) the sphere-like nano gamma-alumina powder obtained by the method can be applied to the aspects of catalysts, catalyst carriers, adsorbents, additives and the like, and has a wide application range;
(4) the nano gamma-alumina powder produced and prepared by the method is easy to carry out secondary processing and utilization, and on one hand, the nano gamma-alumina powder can be directly molded by a product, and on the other hand, the nano gamma-alumina powder can be further prepared into alpha-type or other types of alumina for utilization.
Drawings
Fig. 1 is an XRD pattern of nano gamma-alumina prepared by the present invention.
FIG. 2 is SEM image of nano-gamma-alumina of about 8-10nm prepared by the present invention.
FIG. 3 is SEM image of nanometer 12-16nm gamma-alumina prepared by the present invention.
FIG. 4 is SEM image of nano-gamma-alumina of about 16-20nm prepared by the present invention.
FIG. 5 is SEM image of nano 20nm or so gamma-alumina prepared by the present invention.
Detailed Description
Specific examples of the invention are described in detail below to facilitate a further understanding of the invention.
All experimental procedures used in the following examples are conventional unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
Uniformly dissolving 10g of citric acid in 90g of ultrapure water at 60 ℃, and continuously stirring until the citric acid is completely dissolved to form a colorless transparent solution; then adding 0.4g of polyethylene glycol and 0.2g of isopropanol, and stirring to fully dissolve the mixture; taking 20g of high-purity boehmite powder, slowly adding the boehmite powder while stirring the solution, and continuously stirring the solution until the boehmite is completely added, and continuously stirring and uniformly dispersing; putting the obtained slurry into a ball mill, ball-milling for 30min at the rotating speed of 200r/min, and sieving the ball-milled slurry by a filter sieve of 80 meshes; then, the slurry is stirred and spray-dried, the spray-drying temperature is controlled to be 110 ℃, and the feeding amount is controlled to be 500ml/h, so that dry mixture powder is obtained; then, the dried mixture powder is placed in a corundum crucible, the corundum crucible is placed in a muffle furnace, and the temperature rise rate is set as follows: the temperature is between room temperature and 700 ℃, the time is 240min, the heat preservation time at 700 ℃ is 120min, when the crucible is cooled to 500 ℃ along with the furnace, the crucible is taken out and rapidly cooled for 40min, and the nano gamma-alumina powder with the particle size of about 10nm and uniform distribution can be obtained.
Example 2
Uniformly dissolving 10g of citric acid in 15g of ultrapure water at 90 ℃, and continuously stirring until the citric acid is completely dissolved to form a colorless transparent solution; then adding 0.1g of polyethylene glycol and 0.1g of hexadecyl trimethyl ammonium bromide, and stirring to fully dissolve the mixture; taking 20g of high-purity boehmite powder, slowly adding the boehmite powder while stirring the solution, and continuously stirring the solution until the boehmite is completely added, and continuously stirring and uniformly dispersing; putting the obtained slurry into a ball mill, ball-milling for 30min at the rotating speed of 200r/min, and sieving the ball-milled slurry by a filter sieve of 80 meshes; then placing the slurry in an oven at 80 ℃, stirring and drying at the same time, and refining the dried solid to powder with uniform fineness by using an airflow pulverizer to obtain mixture powder; then, the dried mixture powder is placed in a corundum crucible, the corundum crucible is placed in a muffle furnace, and the temperature rise rate is set as follows: the temperature is between room temperature and 800 ℃, the time is 240min, the heat preservation time at 800 ℃ is 120min, when the crucible is cooled to 500 ℃ along with the furnace, the crucible is taken out and rapidly cooled for 40min, and the nano gamma-alumina powder with the particle size of about 8nm and uniform distribution can be obtained.
Example 3
Uniformly dissolving 10g of citric acid in 30g of ultrapure water at 40 ℃, and continuously stirring until the citric acid is completely dissolved to form a colorless transparent solution; then adding 0.2g of ammonium polymethacrylate and 0.1g of oleylamine, and stirring to fully dissolve the mixture; taking 20g of boehmite powder, slowly adding the boehmite powder while stirring the solution, and continuously stirring the solution until the boehmite is completely added, and continuously stirring and uniformly dispersing; putting the obtained slurry into a ball mill, ball-milling for 30min at the rotating speed of 200r/min, and sieving the ball-milled slurry by a filter sieve of 80 meshes; then, placing the slurry in a drying oven at 100 ℃, stirring and drying the slurry, grinding and crushing the dried solid by agate until the powder with uniform fineness and no granular feeling is obtained, and obtaining mixture powder; then, the dried mixture powder is placed in a corundum crucible, the corundum crucible is placed in a muffle furnace, and the temperature rise rate is set as follows: the temperature is between room temperature and 700 ℃, the time is 240min, the heat preservation time at 700 ℃ is 120min, when the crucible is cooled to 500 ℃ along with the furnace, the crucible is taken out and rapidly cooled for 40min, and the nano gamma-alumina powder with the particle size of about 12nm and uniform distribution can be obtained.
Example 4
Uniformly dissolving 10g of glycine in 100g of 5 ℃ ultrapure water, and continuously stirring until the citric acid is completely dissolved to form a colorless transparent solution; then adding 0.2g of ammonium polymethacrylate and 0.1g of stearic acid, and stirring to fully dissolve the ammonium polymethacrylate and the stearic acid; taking 20g of boehmite powder, slowly adding the boehmite powder while stirring the solution, and continuously stirring the solution until the boehmite is completely added, and continuously stirring and uniformly dispersing; putting the obtained slurry into a ball mill, ball-milling for 30min at the rotating speed of 200r/min, and sieving the ball-milled slurry by a filter sieve of 80 meshes; then, the slurry is stirred and spray-dried, the spray-drying temperature is controlled to be 100 ℃, and the feeding amount is controlled to be 500ml/h, so that dry mixture powder is obtained; then, the dried mixture powder is placed in a corundum crucible, the corundum crucible is placed in a muffle furnace, and the temperature rise rate is set as follows: the temperature is between room temperature and 800 ℃, the time is 240min, the heat preservation time at 800 ℃ is 120min, when the crucible is cooled to 500 ℃ along with the furnace, the crucible is taken out and rapidly cooled for 40min, and the nano gamma-alumina powder with the particle size of about 16nm and uniform distribution can be obtained.
Example 5
Uniformly dissolving 10g of ammonium chloride in 60g of ultrapure water at 25 ℃, and continuously stirring until the citric acid is completely dissolved to form a colorless transparent solution; then adding 0.2g of polyethylene glycol and 0.1g of emulsifying wax, and stirring to fully dissolve the mixture; taking 20g of boehmite powder, slowly adding the boehmite powder while stirring the solution, and continuously stirring the solution until the boehmite is completely added, and continuously stirring and uniformly dispersing; putting the obtained slurry into a ball mill, ball-milling for 30min at the rotating speed of 200r/min, and sieving the ball-milled slurry by a filter sieve of 80 meshes; drying at 100 ℃ by using an oven, stirring and drying at the same time, grinding and crushing the dried solid by using agate until the powder is uniform in fineness and free of particle feeling, and obtaining mixture powder; then, the dried mixture powder is placed in a corundum crucible, the corundum crucible is placed in a muffle furnace, and the temperature rise rate is set as follows: the temperature is between room temperature and 800 ℃, the time is 240min, the heat preservation time at 800 ℃ is 120min, and the nano gamma-alumina powder with the particle size of about 20nm and uniform distribution can be obtained after furnace cooling.
The nano gamma-alumina powder obtained in the embodiment can be further calcined for 1-2 hours after the temperature is raised to 1200 ℃ or above, and alpha-nano alumina with excellent quality can be obtained.
The method for preparing the high-purity nano gamma-alumina powder is characterized in that high-purity boehmite/pseudo-boehmite is used as a raw material, an organic or inorganic compound with low-temperature thermal decomposition property is added, a simple high-temperature calcination process is adopted, and the nano gamma-alumina powder prepared by the method has the characteristics of spheroidal morphology, nano particle size of 5-20nm, uniform particle size distribution, high purity and the like, is simple in preparation process and high in production efficiency, is mainly used for catalysts, catalyst carriers, adsorbents, additives and the like, and has good performance.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited thereto, and various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the present invention.
Claims (10)
1. A preparation method of quasi-spherical nano gamma-alumina is characterized by comprising the following steps:
1) taking ultrapure water, and controlling the temperature of the ultrapure water to be 5-90 ℃ for later use;
2) adding an organic or inorganic compound with low-temperature thermal decomposition property into the ultrapure water obtained in the step 1), stirring at room temperature for dissolving, adding a trace amount of additive after fully dissolving, and fully stirring to obtain a solution;
3) slowly and gradually adding boehmite powder into the solution obtained in the step 2), and continuously stirring and uniformly dispersing at room temperature until boehmite is completely added or a mixture with good uniformity is formed;
4) putting the mixture obtained in the step 3) into a ball mill for ball milling;
5) drying the mixture subjected to ball milling in the step 4) to obtain dry solid particles;
6) crushing the dry solid particles obtained in the step 5) to obtain dry powder;
7) calcining the dried powder obtained in the step 6) to obtain the nano gamma-alumina.
2. The method for preparing spheroidal nano gamma-alumina according to claim 1, wherein the ultrapure water in the step 1) is processed in a manner of: non-contact heat conduction in a clean environment; the temperature of the ultrapure water is 30 to 70 ℃, preferably 60 ℃.
3. The method for preparing spheroidal nano gamma-alumina according to claim 1, wherein the organic or inorganic compound having low temperature thermal decomposition property in step 2) is one or more of ammonium carbonate, ammonium bicarbonate, ammonium chloride, citric acid, ammonium citrate, glycine, urea or acetic acid; wherein the mass ratio of the compound to the ultrapure water is 1: (0.1-10); the additive is one or more of polyethylene glycol, ammonium polymethacrylate, oleylamine, emulsifying wax, isopropanol, stearic acid, quaternary ammonium compound and hexadecyl trimethyl ammonium bromide; wherein the mass ratio of the additive to the ultrapure water is 1 (50-1000).
4. The method for preparing spheroidal nano gamma-alumina according to claim 1, wherein the boehmite is a high purity boehmite or a high purity pseudo-boehmite in step 3), preferably a high purity boehmite; the mass ratio of the boehmite to the ultrapure water is as follows: 1: (0.1-10); the stirring mode is double-cone screw planetary mechanical stirring at room temperature.
5. The method for preparing spheroidal nano gamma-alumina as claimed in claim 1, wherein the ball milling in step 4) is performed by a planetary ball mill at a rotation speed of 150-.
6. The method for preparing spheroidal nano gamma-alumina according to claim 1, wherein the drying method adopted in the step 5) is as follows: oven heat drying, microwave drying, roller heat drying or spray drying at 80-110 deg.C until the water content is less than or equal to 5 wt%.
7. The method for preparing spheroidal nano gamma-alumina according to claim 1, wherein the pulverization manner adopted in the step 6) is as follows: grinding, alligator crushing, roller crushing or airflow crushing, wherein the size of the crushed solid particles is less than 1 mm.
8. The method for preparing spheroidal nano gamma-alumina according to claim 1, wherein the equipment used for calcination in step 7) is a muffle furnace, a tube furnace, a rotary furnace, a crucible resistance furnace, a box furnace, a lift furnace, a shaft furnace, a trolley furnace, a mesh belt furnace, a roller kiln, a pusher kiln, a tunnel furnace, a rotary kiln or a suspension calciner, and the calcination method comprises the following steps:
71) heating the temperature from room temperature to 300 ℃, wherein the heating rate is 0.1-50 ℃/min;
72) raising the temperature from 300 to 600 ℃ at a temperature raising rate of 0.1-50 ℃/min;
73) heating the temperature from 600 to 800 ℃ at a heating rate of 0.1-50 ℃/min;
74) the heat preservation temperature is 700-;
75) cooling with the furnace body or then quickly cooling to obtain the nano alumina.
9. The spheroidal nano gamma-alumina prepared by the method for preparing the spheroidal nano gamma-alumina according to any one of claims 1 to 8.
10. Use of the spheroidal nano-gamma-alumina prepared by the method of any one of claims 1 to 8.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115140756A (en) * | 2022-08-05 | 2022-10-04 | 湖南省产商品质量检验研究院 | Preparation method of sphere-like nano cerium oxide |
| CN117142503A (en) * | 2023-08-28 | 2023-12-01 | 山东奥维新材料科技有限公司 | Composite active alumina powder and preparation method thereof |
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2021
- 2021-12-27 CN CN202111616877.XA patent/CN114105177A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115140756A (en) * | 2022-08-05 | 2022-10-04 | 湖南省产商品质量检验研究院 | Preparation method of sphere-like nano cerium oxide |
| CN117142503A (en) * | 2023-08-28 | 2023-12-01 | 山东奥维新材料科技有限公司 | Composite active alumina powder and preparation method thereof |
| CN117142503B (en) * | 2023-08-28 | 2024-02-23 | 山东奥维新材料科技有限公司 | Composite active alumina powder and preparation method thereof |
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