CN115818687B - Superfine alpha-Al2O3Method for preparing nano powder - Google Patents
Superfine alpha-Al2O3Method for preparing nano powder Download PDFInfo
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 29
- IOGARICUVYSYGI-UHFFFAOYSA-K azanium (4-oxo-1,3,2-dioxalumetan-2-yl) carbonate Chemical compound [NH4+].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O IOGARICUVYSYGI-UHFFFAOYSA-K 0.000 claims abstract description 63
- 239000003513 alkali Substances 0.000 claims abstract description 57
- 239000002243 precursor Substances 0.000 claims abstract description 57
- 239000002245 particle Substances 0.000 claims abstract description 25
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims abstract description 22
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 21
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 19
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 44
- 239000000843 powder Substances 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000002572 peristaltic effect Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000001238 wet grinding Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 description 10
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 description 5
- 229940063655 aluminum stearate Drugs 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 229910001593 boehmite Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- -1 aluminum alkoxide Chemical class 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 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
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of superfine alpha-Al 2O3 nano powder, belonging to the technical field of inorganic nonmetallic materials. According to the invention, aluminum chloride hexahydrate and ammonium carbonate solution are used as raw materials, the aluminum chloride hexahydrate solution is slowly dripped into the ammonium carbonate solution to react in high-speed rotation, the alkali aluminum ammonium carbonate precursor suspension obtained by the reaction is filtered, washed and dried, the dispersibility of the dried alkali aluminum ammonium carbonate precursor is increased by wet grinding of a dispersing agent and ethanol, and then the alpha-Al 2O3 nano powder with the particle size of 100-200nm and good dispersibility can be obtained by drying and calcining. The preparation process is energy-saving, environment-friendly, suitable for industrial production and has wide market application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic materials, and particularly relates to a preparation method of superfine alpha-Al 2O3 nanometer powder.
Background
Alpha-Al 2O3 is an important inorganic nonmetallic material and has wide application value, but the common alumina powder is obtained from bauxite, so that the application range is limited due to large particle size, particle morphology, particle distribution and the like. The superfine alpha-Al 2O3 nano powder has the advantages of small granularity, large specific surface area, uniform granularity, large hardness, strong heat stability, corrosion resistance and the like, and is widely applied to a plurality of high and new technical fields, such as: electronic materials, surface protective materials, optical materials, biological materials, ceramic composite materials, and the like, particularly for transparent ceramics. In order to further improve the performance of the alpha-Al 2O3 nano powder, researchers optimize the synthesis process to improve the performances of purity, morphology, particle size distribution, dispersibility and the like.
Currently, the most widely used method for preparing alpha-Al 2O3 nano-powder is (1) sol-gel method; (2) pyrolysis method. The sol-gel method can be divided into inorganic aluminum salt hydrolysis and aluminum alkoxide hydrolysis according to the aluminum salt, the sol is formed after hydrolysis, the sol is aged or evaporated and concentrated to further enable colloidal particles to be condensed, gel with a three-dimensional space network structure is formed, and the gel is dried and heat treated to obtain alpha-Al 2O3 nano powder. U.S. patent document USP7115243B2 discloses a method for preparing ultrafine alpha-Al 2O3 nanometer powder with controllable crystal grains by adding alpha-Al 2O3 crystal seeds or corundum crystal seeds into isopropanol and butanediol serving as raw materials in the hydrolysis process and performing hydrothermal treatment. U.S. patent document USP6464584B1 discloses a method for preparing boehmite sol by adding aluminum nitrate solution into ammonia water for hydrolysis, adding oleic acid to uniformly disperse the boehmite sol, and calcining the boehmite sol in an anaerobic environment at 1000-1100 ℃ to obtain alpha-Al 2O3 powder, wherein the liquid phase process can prepare powder with smaller particle size, but the product has serious agglomeration, long production period and high cost. The pyrolysis method is a method for preparing alpha-Al 2O3 powder by calcining aluminum ammonium carbonate or aluminum ammonium sulfate at high temperature. Chinese patent document CN201310180677.3 discloses an aluminum ammonium sulfate recrystallization, and then the recrystallized aluminum ammonium sulfate is calcined at high temperature to obtain a product, in the patent, a tail gas treatment device is designed, so that the waste emission is reduced, but the process is complex, the period is long, and the method has the advantages that the prepared product has small particle size, but the problem of environmental pollution exists in the calcining process. Aluminum ammonium carbonate pyrolysis is typically synthesized from aluminum salt solutions and ammonium salt solutions, wherein the raw material purity, raw material concentration, temperature, reflected molar ratio, and the like are related. U.S. patent document USP4053579 discloses a method for preparing alpha-Al 2O3 nano powder by pyrolysis of aluminum ammonium carbonate, which selects aluminum chloride hexahydrate or aluminum ammonium sulfate as an aluminum source at 25-70 ℃. Dripping the precursor into ammonium bicarbonate solution, regulating the pH value of the solution to 7.5-9, obtaining an ammonium aluminum carbonate precursor through precipitation and projection, and calcining the precursor at 1250-1300 ℃ to obtain superfine alpha-Al 2O3 nano powder. Although the ammonium aluminum carbonate is utilized to prevent the emission of harmful gases such as sulfur trioxide, the agglomeration phenomenon of the obtained product is serious after high-temperature calcination at a temperature of more than 1200 ℃, the particle size and the dispersibility of the particles are poor, and the energy consumption is high.
Disclosure of Invention
Aiming at the technical problems of poor dispersibility and serious particle size agglomeration of the final product alpha-Al 2O3 powder in the process for preparing the superfine alpha-Al 2O3 powder in the prior art, the invention provides the preparation method of the superfine alpha-Al 2O3 powder, which is energy-saving, environment-friendly and suitable for industrial production.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the superfine alpha-Al 2O3 nanometer powder comprises the following preparation steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor:
a) Respectively preparing aluminum chloride hexahydrate and ammonium carbonate into aqueous solutions, slowly adding the aluminum chloride hexahydrate solution into the ammonium carbonate solution, and reacting for 1-6 hours at 25-55 ℃ to obtain a suspension of an alkali aluminum ammonium carbonate precursor;
b) Carrying out reduced pressure suction filtration on the obtained suspension of the alkali aluminum ammonium carbonate precursor, washing a filter cake with water, washing with alcohol, and drying to obtain alkali aluminum ammonium carbonate precursor powder;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: adding ethanol into alkali aluminum ammonium carbonate precursor powder to prepare slurry with the solid content of 10% -50%, adding a dispersing agent I, performing planetary ball milling for 1-5h, filtering, and drying to obtain ball-milled alkali aluminum ammonium carbonate precursor powder;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: and heating the alkali aluminum ammonium carbonate precursor powder after ball milling to 950-1200 ℃, and preserving heat for 30-180min to obtain the superfine alpha-Al 2O3 nano powder.
Preferably, in step a), the aluminum chloride hexahydrate solution is added by injection or peristaltic method, and the mixing method adopted in the adding process is vigorous stirring; aluminum chloride hexahydrate: the molar ratio of the ammonium carbonate is 1: (3.5-6); wherein, the water consumption ratio of the prepared aluminum chloride hexahydrate solution and the ammonium carbonate solution is 45:13, and the concentration of Al 3+ in the aluminum chloride hexahydrate solution is 0.2M.
More preferably, aluminum chloride hexahydrate: the molar ratio of the ammonium carbonate is 1: (4.5-5).
Preferably, the drying temperature in step b) is 80-100deg.C and the drying time is 8-12h.
Preferably, in the step (2), the dispersing agent I is one or more of oleic acid, stearic acid, tween 60 and Tween 80; according to dispersant I: the addition amount of the dispersing agent I is determined by the mass ratio (0.01-0.3) of the alpha-Al 2O3 powder to 100.
More preferably, in step (2) dispersant I is stearic acid.
Preferably, ball milling balls in the planetary ball milling in the step (2): the mass ratio of the powder is (6-12): 1.
Preferably, the ball milling rotating speed in the planetary ball milling in the step (2) is 100-300rpm, and the ball milling time is 2-5h.
Preferably, the temperature rising rate in the step (3) is 1-10 ℃/min.
Preferably, in the step (3), the temperature is raised to 950-1050 ℃, and the heat preservation time is 30min-2h.
The technical characteristics and the principle of the invention are as follows:
According to the invention, aluminum chloride hexahydrate and ammonium carbonate solution are used as raw materials, the aluminum chloride hexahydrate solution is slowly dripped into the ammonium carbonate solution to react in high-speed rotation, the alkali aluminum ammonium carbonate precursor suspension obtained by the reaction is filtered, washed and dried, the dispersibility of the dried alkali aluminum ammonium carbonate precursor is increased by wet grinding of a dispersing agent and ethanol, and then the alpha-Al 2O3 nano powder with the particle size of 100-200nm and good dispersibility can be obtained by drying and calcining.
After the preparation of the precursor is completed, the precursor powder is subjected to planetary ball milling treatment, and a dispersing agent I added in the ball milling process can react with alkali aluminum ammonium carbonate to form aluminum stearate, and the existence of the aluminum stearate prevents mutual contact among particles, so that the steric effect is enhanced, and agglomeration among particles is inhibited; in addition, the formed agglomerates can be broken up due to mutual collision between the balls and the materials in the ball milling process, so that the dispersion effect is achieved.
Calcining alkali aluminum ammonium carbonate ball-milled by adding a dispersing agent to obtain alpha-Al 2O3 nano powder, and measuring the particle size and volume distribution of the alpha-Al 2O3 nano powder by using a laser particle size distribution instrument, wherein the particle size and volume distribution is as follows: d20 =200 nm, d90=500 nm; the transmission electron microscope shows that the product has regular particle morphology, approximately spherical shape, uniform granularity and good dispersity among particles, and the primary particle size is 100-200nm.
The beneficial effects are that:
1. In the invention, the dispersibility of the alkali aluminum ammonium carbonate is increased by utilizing planetary ball milling wet milling, so that the calcining temperature is reduced, and the energy consumption is reduced;
2. The dispersant I added in the planetary ball grinding process reacts with the alkali aluminum ammonium carbonate to form aluminum stearate, and the formation of the aluminum stearate further increases the dispersibility of the aluminum stearate.
Drawings
FIG. 1 is an XRD pattern of example 1 before and after ACCH ball milling of ammonium aluminum carbonate after addition of dispersant I in step (1);
FIG. 2 is an XRD pattern of ultrafine alpha-Al 2O3 nano powder obtained in the step (1) of example 1;
FIG. 3 is an SEM photograph of ultra-fine α -Al 2O3 nano powder obtained in the step (1) of example 1;
FIG. 4 is a TEM photograph of the ultra fine α -Al 2O3 nano powder obtained in the step (1) of example 1;
FIG. 5 is a graph showing the laser particle size distribution of the ultrafine α -Al 2O3 nano powder obtained in the step (1) of example 1.
Detailed Description
The technical scheme of the present invention is further described below with reference to specific examples, but is not limited thereto.
Example 1
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor:
a) Dissolving 6.05g of aluminum chloride hexahydrate solid in 180ml of water, dissolving 10g of ammonium carbonate in 52ml of water, slowly injecting the aluminum chloride hexahydrate solution into the vigorously stirred ammonium carbonate solution after complete dissolution, and reacting at 45 ℃ for 1 hour to generate alkali aluminum ammonium carbonate precursor suspension;
b) Filtering the obtained alkali aluminum ammonium carbonate precursor suspension, washing a filter cake with water, and drying the filter cake in a vacuum drying oven at 80 ℃ for 10 hours to obtain alkali aluminum ammonium carbonate precursor powder;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor:
Preparing the obtained alkali aluminum ammonium carbonate precursor powder into slurry with the solid content of 12.5% in ethanol, adding 0.05g of stearic acid, performing planetary ball milling for 3 hours at 250rpm, filtering, drying, grinding a ball-milled sample, and obtaining alkali aluminum ammonium carbonate powder after ball milling;
XRD and SEM images of the alkali aluminum ammonium carbonate precursor powder obtained in the step are shown in figures 2-3;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling:
and (3) placing the alkali ammonium aluminum carbonate precursor powder after ball milling in a tube furnace, heating to 950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours to obtain the alpha-Al 2O3 nano powder.
XRD of the α -Al 2O3 nano powder obtained in the step (3) of this example is shown in FIG. 2, SEM is shown in FIG. 3, TEM is shown in FIG. 4, and laser particle size distribution is shown in FIG. 5. As shown in figures 4-5, the alpha-Al 2O3 nano powder has the particle size of 100-200nm, the morphology is similar to a sphere, and the dispersibility is good. As can be seen from fig. 5, the volume distribution of the powder particles is a standard normal distribution, D 50＝200nm,D90 =420 nm, and the particle size distribution is narrow.
Example 2
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1, except that a): 6.05g of aluminum chloride hexahydrate solid was dissolved in 180ml of water, 12g of ammonium carbonate was dissolved in 52ml of water, and reacted at 45℃for 1 hour;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: as described in example 1.
Example 3
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1, except that a): 16g of ammonium carbonate is taken and dissolved in 52ml of water and reacted for 1h at 45 ℃;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: as described in example 1.
Example 4
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1, except that 0.1g of dispersant I stearic acid was added;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: as described in example 1.
Example 5
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1, except that planetary ball milling was performed at 200rpm for 3 hours;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: as described in example 1.
Example 6
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: the procedure is as in example 1, except that the calcination temperature is 1000 ℃.
Example 7
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1, except that 0.1g of dispersant I stearic acid was added;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: the procedure is as in example 1, except that the calcination temperature is 1000 ℃.
Example 8
A preparation method of superfine alpha-Al 2O3 nanometer powder comprises the following steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor: as described in example 1;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: as described in example 1, except that 0.1g of dispersant I stearic acid was added;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: the procedure is as in example 1, except that the calcination temperature is 1050 ℃.
It should be noted that the above-mentioned embodiments are merely some, but not all embodiments of the preferred mode of carrying out the invention. It is evident that all other embodiments obtained by a person skilled in the art without making any inventive effort, based on the above-described embodiments of the invention, shall fall within the scope of protection of the invention.
Claims (7)
1. The preparation method of the superfine alpha-Al 2O3 nanometer powder is characterized by comprising the following preparation steps:
(1) Preparing an alkali aluminum ammonium carbonate precursor:
a) Respectively preparing aluminum chloride hexahydrate and ammonium carbonate into aqueous solutions, slowly adding the aluminum chloride hexahydrate solution into the ammonium carbonate solution, and reacting at 25-55 ℃ for 1-6 h to obtain a suspension of an alkali aluminum ammonium carbonate precursor;
b) Carrying out reduced pressure suction filtration on the obtained suspension of the alkali aluminum ammonium carbonate precursor, washing a filter cake with water, washing with alcohol, and drying to obtain alkali aluminum ammonium carbonate precursor powder;
(2) Ball milling treatment of an alkali aluminum ammonium carbonate precursor: adding ethanol into alkali aluminum ammonium carbonate precursor powder to prepare slurry with the solid content of 10% -50%, adding a dispersing agent I, performing planetary ball milling on the slurry for 1-5 h, filtering and drying the slurry to obtain alkali aluminum ammonium carbonate precursor powder after ball milling;
(3) Calcining an alkali aluminum ammonium carbonate precursor after ball milling: heating the alkali aluminum ammonium carbonate precursor powder after ball milling to 950-1050 ℃, and keeping the temperature for 30 min-2 h to obtain superfine alpha-Al 2O3 nano powder; the particle size of the superfine alpha-Al 2O3 nano powder is 100-200 nm;
In the step (2), the dispersant I is stearic acid; according to dispersant I: finally, the mass ratio of the alpha-Al 2O3 powder is (0.01-0.3): the ratio of 100 determines the amount of dispersant I added.
2. The method for preparing ultrafine α -Al 2O3 nano-powder according to claim 1, wherein in step a), the addition of the aluminum chloride hexahydrate solution is performed by injection or peristaltic method, and the mixing method adopted in the addition process is vigorous stirring; aluminum chloride hexahydrate: the molar ratio of the ammonium carbonate is 1: (3.5-6); wherein, the water consumption volume ratio of the prepared aluminum chloride hexahydrate solution and the ammonium carbonate solution is 45:13; the concentration of Al 3+ in the aluminum chloride hexahydrate solution was 0.2M.
3. The method for preparing ultrafine α -Al 2O3 nano-powder according to claim 2, wherein the aluminum chloride hexahydrate: the molar ratio of the ammonium carbonate is 1: (4.5-5).
4. The method for preparing ultrafine α -Al 2O3 nano-powder according to claim 1, wherein the drying temperature in step b) is 80-100 ℃ and the drying time is 8-12 h.
5. The method for preparing ultrafine alpha-Al 2O3 nano powder according to claim 1, wherein the ball milling ball in the planetary ball milling in the step (2) is: the mass ratio of the powder is (6-12): 1.
6. The method for preparing ultrafine alpha-Al 2O3 nano-powder according to claim 1, wherein the ball milling speed in the planetary ball milling in the step (2) is 100-300 rpm, and the ball milling time is 2-5 h.
7. The method for preparing ultrafine α -Al 2O3 nano-powder according to claim 1, wherein the heating rate in step (3) is 1-10 ℃/min.
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| CN202211420763.2A CN115818687B (en) | 2022-11-11 | 2022-11-11 | Superfine alpha-Al2O3Method for preparing nano powder |
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| CN104891542A (en) * | 2015-06-24 | 2015-09-09 | 山东大学 | Preparation method of ultrafine alpha-Al2O3 powder |
| CN108163876A (en) * | 2017-12-19 | 2018-06-15 | 华北电力大学（保定） | A kind of nanometer of γ-Al2O3The synthetic method of powder |
| CN109534378A (en) * | 2018-11-27 | 2019-03-29 | 东华大学 | A kind of preparation method of anti-hard aggregation nano alumina particles |
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| TWI408104B (en) * | 2005-03-18 | 2013-09-11 | Sumitomo Chemical Co | Process for producing fine α-alumina particles |
| DE102005033393B4 (en) * | 2005-07-16 | 2014-04-03 | Clariant International Limited | Process for the preparation of nanocrystalline α-Al 2 O 3 |
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| CN104891542A (en) * | 2015-06-24 | 2015-09-09 | 山东大学 | Preparation method of ultrafine alpha-Al2O3 powder |
| CN108163876A (en) * | 2017-12-19 | 2018-06-15 | 华北电力大学（保定） | A kind of nanometer of γ-Al2O3The synthetic method of powder |
| CN109534378A (en) * | 2018-11-27 | 2019-03-29 | 东华大学 | A kind of preparation method of anti-hard aggregation nano alumina particles |
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