CN114772620B - Superfine alpha-alumina and preparation method thereof - Google Patents
Superfine alpha-alumina and preparation method thereof Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 49
- 238000010902 jet-milling Methods 0.000 claims abstract description 35
- 238000005119 centrifugation Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 125000004122 cyclic group Chemical group 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 229910001593 boehmite Inorganic materials 0.000 claims description 6
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 6
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 28
- 239000000843 powder Substances 0.000 abstract description 10
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 23
- 238000000635 electron micrograph Methods 0.000 description 17
- 239000004576 sand Substances 0.000 description 15
- 238000003801 milling Methods 0.000 description 12
- 238000000227 grinding Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000009776 industrial production Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The application provides superfine alpha-alumina and a preparation method thereof, and belongs to the technical field of alpha-alumina preparation. The preparation method of the superfine alpha-alumina comprises the following steps: and sequentially carrying out jet milling and centrifugation on the alpha-alumina precursor, taking upper slurry, and sintering. The rotational speed of the jet mill during jet milling is at least 1000r/min. The preparation method of the superfine alpha-alumina utilizes the characteristic that the alpha-alumina can perfectly inherit the performance of a precursor, and before sintering, the alpha-alumina precursor is subjected to jet milling treatment, so that the agglomeration trend of alpha-alumina precursor powder is effectively improved, the alpha-alumina precursor with different particle diameters can be obtained through the jet milling treatment, the upper slurry is obtained after centrifugal separation, and the upper slurry is generally superfine powder which has no special sharp angle and has excellent characteristics, and the superfine alpha-alumina with the primary crystal particles of 50-300 nm can be obtained through sintering.
Description
Technical Field
The application relates to the technical field of alpha-alumina preparation, in particular to superfine alpha-alumina and a preparation method thereof.
Background
The alumina has excellent performances of wear resistance, corrosion resistance, high temperature resistance, high strength and the like, and can be widely applied to the fields of ceramics, polishing, grinding tools, protective coatings, composite materials and the like. The size, morphology and dispersibility of the alumina particles have a decisive effect on the shaping of the product and its use, and even on the properties. The alpha-alumina powder has the characteristics of good fluidity, small granularity, low surface energy, high density and the like, and can be widely applied to precise polishing materials, lithium battery diaphragm materials, transparent ceramics, high-performance ceramics and substrate materials of semiconductors and chips.
In general, the alpha-alumina prepared by conventional industrial production has larger granularity, and few alpha-alumina powder with a diameter of a few microns can be directly prepared.
Disclosure of Invention
The application provides superfine alpha-alumina and a preparation method thereof, which can prepare superfine alpha-alumina with primary crystal particles of 50-300 nm.
Embodiments of the present application are implemented as follows:
in a first aspect, the present examples provide a method for preparing ultrafine α -alumina, comprising: and sequentially carrying out jet milling and centrifugation on the alpha-alumina precursor, taking upper slurry, and sintering.
The alpha-alumina precursor is prepared by calcining an aluminum source.
The rotational speed of the jet mill during jet milling is at least 1000r/min.
In the technical scheme, the preparation method of the superfine alpha-alumina can perfectly inherit the characteristic of the precursor performance of the alpha-alumina, and the alpha-alumina precursor is subjected to jet milling treatment before sintering, so that the agglomeration trend of the alpha-alumina precursor powder is effectively improved, and the subsequent preparation is facilitated. And the alpha-alumina precursors with different particle diameters can be obtained through jet milling treatment, the upper slurry is obtained after centrifugal separation, the upper slurry is generally ultrafine powder which has no special sharp angle and has excellent characteristics, and the superfine alpha-alumina with primary crystal particles of 50-300 nm can be obtained through sintering. Meanwhile, the preparation method of the superfine alpha-alumina is suitable for industrial production.
With reference to the first aspect, in a first possible example of the first aspect of the present application, the rotational speed of the jet mill during jet milling is 1000 to 2500r/min.
In the above example, the particle size of the alpha alumina precursor does not substantially change when the jet mill speed exceeds 2500r/min.
With reference to the first aspect, in a second possible example of the first aspect of the present application, the number of cyclic crushing times in the jet milling process is 1 to 6.
In the above example, the particle size of the α -alumina precursor does not substantially change when the number of cyclic breaks exceeds 6.
With reference to the first aspect, in a third possible example of the first aspect of the present application, the centrifugation includes: mixing the crushed alpha-alumina precursor with a solvent, and then placing the mixture in a centrifugal machine for centrifugal treatment.
With reference to the first aspect, in a fourth possible example of the first aspect of the present application, the mass ratio of the crushed α -alumina precursor to the solvent is 1:1 to 1:5.
Alternatively, the solvent comprises water, ethanol, or a mixture of water and ethanol.
With reference to the first aspect, in a fifth possible example of the first aspect of the present application, the rotational speed of the centrifuge during the centrifugation is 200 to 800r/min, and the time of the centrifugation is 5 to 60min.
In combination with the first aspect, in a sixth possible example of the first aspect of the present application, the calcination temperature is 500 to 1100 ℃ and the calcination time is 2 to 5 hours.
In combination with the first aspect, in a seventh possible example of the first aspect of the present application, the sintering temperature is 1100 to 1450 ℃, and the sintering time is 2 to 5 hours.
With reference to the first aspect, in an eighth possible example of the first aspect of the present application, after sintering is completed, ultra-fine α -alumina is prepared, and the ultra-fine α -alumina is subjected to sanding treatment.
In the above example, the sanding process can refine the particle size of the α -alumina more and round the corners of the α -alumina particles to make them more rounded.
In a second aspect, the present examples provide an ultrafine α -alumina produced according to the above-described process for producing ultrafine α -alumina.
In the technical scheme, the primary crystal particles of the superfine alpha-alumina can reach 50-300 nm.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an electron micrograph of an ultra-fine alpha-alumina precursor after jet milling of example 1 of the present application;
FIG. 2 is an electron micrograph of ultrafine α -alumina obtained in example 1 of the present application;
FIG. 3 is an electron micrograph of an ultra-fine alpha-alumina precursor after jet milling of example 4 of the present application;
FIG. 4 is an electron micrograph of ultrafine α -alumina obtained in example 4 of the present application;
FIG. 5 is an electron micrograph of ultrafine α -alumina obtained in example 21 of the present application;
FIG. 6 is an electron micrograph of ultrafine α -alumina obtained in comparative example 1 of the present application;
FIG. 7 is an electron micrograph of ultrafine α -alumina obtained in comparative example 2 of the present application;
FIG. 8 is an electron micrograph of ultrafine α -alumina obtained in comparative example 3 of the present application;
FIG. 9 is an electron micrograph of an ultrafine α -alumina precursor after jet milling according to comparative example 5 of the present application;
FIG. 10 is an electron micrograph of ultrafine α -alumina obtained in comparative example 5 of the present application.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustration of the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
At present, the preparation of superfine alpha-alumina mainly adopts a chemical method to prepare a precursor thereof, for example, a sol-gel method is adopted to prepare the superfine alpha-alumina, but the method seems to be only remained in a laboratory stage, and is difficult to popularize and apply to industrial production. The methods such as a homogeneous precipitation method, a mechanical ball milling method, a microemulsion method, a plasma spray pyrolysis method, an aerosol decomposition method and the like are more used, but the problems of long production period, low production efficiency, poor powder performance, easy agglomeration, difficult regulation of particle size and the like exist.
The following specifically describes an ultrafine α -alumina and a preparation method thereof according to an embodiment of the present application:
the application provides a preparation method of superfine alpha-alumina, which comprises the following steps: and sequentially carrying out jet milling and centrifugation on the alpha-alumina precursor, taking upper slurry, and sintering.
The rotational speed of the jet mill during jet milling is at least 1000r/min.
Optionally, the rotational speed of the jet mill during jet milling is 1000-2500 r/min.
When the rotating speed of the jet mill exceeds 2500r/min, the granularity of the alpha-alumina precursor is not changed basically, and the rotating speed of the jet mill can be limited to 1000-2500 r/min based on energy saving consideration.
As an example, the rotational speed of the jet mill during jet milling may be 1000r/min, 1200r/min, 1500r/min, 1800r/min, 2000r/min, 2300r/min, or 2500r/min.
The number of cyclic crushing times in the jet milling process is at least 1.
Optionally, the number of cyclic crushing times in the jet milling process is 1 to 6.
When the number of cyclic crushing times exceeds 6 times, the particle size of the alpha-alumina precursor is not substantially changed, and the number of cyclic crushing times can be limited to 1 to 6 times based on energy saving consideration.
As an example, the number of cyclic crushing times in the jet milling process may be 1, 2, 3. 4 times, 5 times or 6 times.
Centrifugation involves mixing the crushed alpha-alumina precursor with a solvent and then placing the mixture in a centrifuge for centrifugation.
Optionally, the mass ratio of the alpha-alumina precursor and the solvent after crushing in the centrifugal treatment is 1:1-1:5.
As an example, the mass ratio of the alpha-alumina precursor to the solvent after pulverization in the centrifugation treatment may be 1:1, 1:2, 1:3, 1:4, or 1:5.
Alternatively, the solvent comprises water, ethanol, or a mixture of water and ethanol.
As an example, the solvent may be water, ethanol, or an aqueous ethanol solution of any ratio.
Optionally, the rotational speed of the centrifuge during the centrifugation process is 200-800 r/min.
As an example, the rotational speed of the centrifuge during the centrifugation process may be 200r/min, 300r/min, 400r/min, 500r/min, 600r/min, 700r/min or 800r/min.
Optionally, the centrifugation time is 5-60 min.
As an example, the time of the centrifugation may be 5min, 10min, 20min, 30min, 40min, 50min, or 60min.
After the centrifugation, the upper slurry should be rapidly taken out to be dried, and the drying method includes oven drying and spray drying.
The drying in the oven comprises the step of putting the upper slurry taken out after centrifugation into the oven and drying for 1-5 h at the temperature of 40-60 ℃.
As an example, the temperature in the oven may be 40 ℃, 40 ℃ or 40 ℃; the oven drying time may be 1h, 2h, 3h, 4h or 5h.
It should be noted that too high a temperature in the oven will cause the alpha-alumina precursor to agglomerate easily.
Spray drying is a process for preparing dry powders from liquids or slurries by flash drying with hot gases.
After the drying is finished, the dried alpha-alumina precursor is placed in a sintering chamber, heated to 1100-1450 ℃ at 5-20 min/DEG C, and sintered for 2-5 h at 1100-1450 ℃.
By way of example, the heating rate may be 5 min/DEG C, 8 min/DEG C, 10 min/DEG C, 13 min/DEG C, 15 min/DEG C, 18 min/DEG C, or 20 min/DEG C; the sintering temperature can be 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃, 1350 ℃, 1400 ℃ or 1450 ℃; the sintering time may be 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h.
After sintering, the superfine alpha-alumina is prepared, wherein the D50 granularity of the superfine alpha-alumina is between 1 and 2.5 mu m, and the superfine alpha-alumina can be further subjected to sanding treatment, so that the granularity of the alpha-alumina can be further thinned and corners of the alpha-alumina particles can be rounded, so that the alpha-alumina particles are more round.
The rotating speed of the sand mill in the sand milling treatment is 1800-2600 r/min, the sand milling treatment time is 0.2-1 h, the mass ratio of superfine alpha-alumina to grinding balls in the sand milling treatment is 1:1-1:3, the grinding balls in the sand milling treatment are made of zirconia or alumina, and no solvent is added in the sand milling treatment.
As an example, the rotational speed of the sand mill in the sanding process may be 1800r/min, 1900r/min, 2000r/min, 2100r/min, 2200r/min, 2300r/min, 2400r/min, 2500r/min, or 2600r/min; the sanding treatment time can be 0.2h, 0.3h, 0.5h, 0.7h or 1h; the mass ratio of the superfine alpha-alumina to the grinding ball in the sanding treatment may be 1:1, 1:2, or 1:3.
The alpha-alumina precursor is prepared by the following method:
the aluminum source is placed in a calcining chamber, the temperature is raised to 500-1100 ℃ at the temperature rising rate of 5-20 min/DEG C, and the heat is preserved for 2-5 h at the temperature of 500-1100 ℃.
By way of example, the heating rate may be 5 min/DEG C, 8 min/DEG C, 10 min/DEG C, 13 min/DEG C, 15 min/DEG C, 18 min/DEG C, or 20 min/DEG C; the calcination temperature may be 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ or 1100 ℃; the calcination time may be 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h.
The aluminum source includes any one or more of aluminum hydroxide, boehmite, and pseudo-boehmite.
As examples, the aluminum source may be aluminum hydroxide, boehmite, or pseudo-boehmite, or a mixture of aluminum hydroxide, boehmite, or a mixture of boehmite, pseudo-boehmite, or a mixture of aluminum hydroxide, boehmite, and pseudo-boehmite.
The preparation method of the superfine alpha-alumina utilizes the characteristic that the alpha-alumina can perfectly inherit the performance of the precursor, and the alpha-alumina precursor is subjected to jet milling treatment before sintering, so that the agglomeration trend of the alpha-alumina precursor powder is effectively improved, and the subsequent preparation is facilitated. And the alpha-alumina precursors with different particle diameters can be obtained through jet milling treatment, the upper slurry is obtained after centrifugal separation, the upper slurry is generally ultrafine powder which has no special sharp angle and has excellent characteristics, and the superfine alpha-alumina with primary crystal particles of 50-300 nm can be obtained through sintering. Meanwhile, the preparation method of the superfine alpha-alumina is suitable for industrial production.
The application also provides an ultrafine alpha-alumina, which is prepared according to the preparation method of the ultrafine alpha-alumina.
The primary crystal particles of the superfine alpha-alumina can reach 50-300 nm.
An ultrafine α -alumina and a method for preparing the same of the present application are described in further detail below with reference to examples.
Example 1
The embodiment of the application provides superfine alpha-alumina and a preparation method thereof, wherein the preparation method comprises the following steps:
s1, preparing superfine alpha-alumina precursor
And (3) placing the aluminum hydroxide in a calcination chamber, heating to 780 ℃ at a heating rate of 10 min/DEG C, and preserving heat for 4 hours at the temperature of 780 ℃ to obtain the superfine alpha-alumina precursor.
S2, jet milling
The superfine alpha-alumina precursor is placed in a jet mill for jet milling treatment, the rotating speed of the jet mill is 1900r/min in the jet milling process, and the cyclic milling times are 3 times in the jet milling process.
S4, centrifuging
Mixing the crushed alpha-alumina precursor with ethanol, then placing the mixture in a centrifuge for centrifugal treatment, and taking upper slurry for spray drying; the mass ratio of the crushed alpha-alumina precursor to the ethanol in the centrifugal treatment is 1:3, the rotating speed of the centrifugal machine in the centrifugal treatment process is 600r/min, and the centrifugal treatment time is 30min.
S5, preparing superfine alpha-alumina
The dried alpha-alumina precursor was placed in a sintering chamber, warmed to 1250 ℃ at 10min/°c, and sintered at 1250 ℃ for 4 hours.
The parameters of examples 2 to 20 and comparative examples 1 to 3 are shown in Table 1, and the other parameters are the same as those of example 1.
Table 1 examples 2 to 20 and comparative examples 1 to 3
Example 21
According to the embodiment of the application, the post-treatment steps of S5 and superfine alpha-alumina are added on the basis of the embodiment 1, the prepared superfine alpha-alumina is added into a sand mill for sand milling treatment, the rotating speed of the sand mill in the sand milling treatment is 2200r/min, the sand milling treatment time is 0.5h, the mass ratio of the spheroid alpha-alumina to the grinding balls in the sand milling treatment is 1:2, the grinding balls in the sand milling treatment are made of alumina, and no solvent is added in the sand milling treatment.
Comparative example 4
Comparative example this application was based on example 1, and after centrifugation, the middle slurry was spray dried, the others being unchanged.
Comparative example 5
Comparative example herein the lower slurry was spray dried after centrifugation, the others being unchanged, based on example 1.
Test example 1
The precursor particle sizes of the ultrafine α -alumina before jet milling, and the specific surface areas and particle sizes of the ultrafine α -alumina obtained in examples 1 to 21 and comparative examples 1 to 5 were measured, respectively, and the results are shown in table 2.
TABLE 2 precursor and ultra-fine alpha-alumina Performance of ultra-fine alpha-alumina of examples 1-21 and comparative examples 1-5
As is clear from the above, the specific surface area of the superfine alpha-alumina prepared by the embodiment of the application without post-treatment sanding is 6.83-14.23 m 2 The particle size of D50 is 1.31-2.53 mu m; the specific surface area of the superfine alpha-alumina prepared by post-treatment sanding in the embodiment of the application can reach 36.73m 2 The D50 particle size is only 0.21. Mu.m.
As is clear from the comparison between comparative example 1 and example 1, the specific surface area of ultrafine alpha-alumina obtained without jet milling and centrifugation is low, 3.31m only 2 The particle size of the component/g, D50, is larger and is 10.74 μm.
As is clear from comparison of comparative example 2 and example 2, the specific surface area of ultrafine alpha-alumina obtained without centrifugation is low, only 7.55m 2 The D50 particle size per gram is relatively large and is 2.67. Mu.m.
As is clear from the comparison between comparative example 3 and example 1, the specific surface area of the ultrafine alpha-alumina obtained by the low rotational speed of the jet mill is low, which is only 5.83m 2 The D50 particle size per gram is relatively large and is 2.75 μm.
As is clear from the comparison between comparative example 4 and example 1, the specific surface area of ultrafine alpha-alumina prepared by using the centrifuged intermediate slurry is low, only 9.02m 2 The D50 particle size per gram is relatively large and is 1.93. Mu.m.
As can be seen from the comparison of comparative example 5 and example 1, the specific surface area of ultrafine alpha-alumina prepared by using the centrifuged lower slurry was relatively largeLow, only 5.83m 2 The D50 particle size per gram is relatively large and is 2.75 μm.
Test example 2
Taking the superfine alpha-alumina precursor after jet milling in the embodiment 1 and the prepared superfine alpha-alumina, wherein the electron micrographs of the superfine alpha-alumina precursor and the prepared superfine alpha-alumina are respectively shown in fig. 1 and 2;
taking the superfine alpha-alumina precursor after jet milling in the embodiment 4 and the prepared superfine alpha-alumina, wherein the electron micrographs of the superfine alpha-alumina precursor and the prepared superfine alpha-alumina are respectively shown in fig. 3 and 4;
taking the superfine alpha-alumina prepared in the example 21, and respectively showing an electron micrograph of the superfine alpha-alumina in FIG. 5;
taking superfine alpha-alumina prepared in comparative example 1, and respectively showing an electron micrograph thereof in FIG. 6;
taking superfine alpha-alumina prepared in comparative example 2, and respectively showing the electron micrographs of the superfine alpha-alumina in FIG. 7;
taking superfine alpha-alumina prepared in comparative example 3, and respectively showing the electron micrographs of the superfine alpha-alumina in FIG. 8;
the superfine alpha-alumina precursor after jet milling of comparative example 5 and the superfine alpha-alumina produced were taken, and the electron micrographs thereof are shown in fig. 9 and 10, respectively.
As can be seen from the comparison of fig. 2 and fig. 6 to 8 and 10, the α -alumina prepared in example 1 of the present application has a smaller particle size than that of comparative examples 1 to 3 and 5.
The foregoing is merely a specific embodiment of the present application and is not intended to limit the present application, and various modifications and variations may be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method for preparing ultrafine alpha-alumina, which is characterized by comprising the following steps: sequentially carrying out jet milling and centrifugation on an alpha-alumina precursor, taking upper slurry, and sintering;
the alpha-alumina precursor is prepared by calcining an aluminum source; the aluminum source comprises any one or more of aluminum hydroxide, boehmite and pseudo-boehmite;
the rotational speed of the jet mill during the jet milling process is at least 1000r/min;
the rotating speed of the centrifugal machine is 200-800 r/min in the centrifugal treatment process, and the centrifugal treatment time is 5-60 min;
after the centrifugation is completed, the upper slurry is quickly taken out for drying treatment, wherein the drying treatment mode comprises oven drying and spray drying; and the drying in the oven comprises the step of placing the upper slurry taken out after centrifugation in the oven and drying for 1-5 h at the temperature of 40-60 ℃.
2. The method for preparing ultrafine alpha-alumina according to claim 1, wherein the rotational speed of the jet mill during the jet milling is 1000-2500 r/min.
3. The method for preparing ultrafine α -alumina according to claim 1, wherein the number of cyclic crushing times in the jet milling process is 1 to 6.
4. The method for preparing ultrafine α -alumina according to claim 1, wherein the centrifuging comprises: mixing the crushed alpha-alumina precursor with a solvent, and then placing the mixture in a centrifuge for centrifugal treatment.
5. The method for preparing ultrafine alpha-alumina according to claim 4, wherein the mass ratio of the crushed alpha-alumina precursor to the solvent is 1:1-1:5.
6. The method for preparing ultrafine α -alumina according to claim 5, wherein the solvent comprises water, ethanol, or a mixture of water and ethanol.
7. The method for preparing ultrafine alpha-alumina according to claim 1, wherein the calcination temperature is 500-1100 ℃, and the calcination time is 2-5 hours.
8. The method for preparing ultrafine alpha-alumina according to claim 1, wherein the sintering temperature is 1100-1450 ℃, and the sintering time is 2-5 hours.
9. The method for preparing ultrafine α -alumina according to claim 1, wherein after the sintering is completed, ultrafine α -alumina is prepared and the ultrafine α -alumina is subjected to a sanding treatment.
10. An ultrafine α -alumina, characterized in that the ultrafine α -alumina is produced according to the production method of ultrafine α -alumina as claimed in any one of claims 1 to 9.
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| CN113247930A (en) * | 2021-06-30 | 2021-08-13 | 上海交通大学 | Alpha-alumina and preparation method thereof |
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