CN115974112A - Low-sodium submicron alpha-alumina powder and preparation method and application thereof - Google Patents
Low-sodium submicron alpha-alumina powder and preparation method and application 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 105
- 239000011734 sodium Substances 0.000 title claims abstract description 91
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 91
- 239000000843 powder Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 27
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 16
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 239000011777 magnesium Substances 0.000 claims abstract description 15
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 15
- 150000007524 organic acids Chemical class 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 5
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 4
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 4
- NGPGDYLVALNKEG-UHFFFAOYSA-N azanium;azane;2,3,4-trihydroxy-4-oxobutanoate Chemical compound [NH4+].[NH4+].[O-]C(=O)C(O)C(O)C([O-])=O NGPGDYLVALNKEG-UHFFFAOYSA-N 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 4
- 229940075624 ytterbium oxide Drugs 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 229940031958 magnesium carbonate hydroxide Drugs 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052796 boron Inorganic materials 0.000 abstract description 3
- 150000004820 halides Chemical class 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000012071 phase Substances 0.000 description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000019580 granularity Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention provides low-sodium submicron alpha-alumina powder and a preparation method and application thereof, relating to the technical field of powder materials. The invention provides a preparation method of low-sodium submicron alpha-alumina powder, which comprises the following steps: mixing industrial alumina, organic acid, a dispersant and water, and adjusting the pH value of the obtained dispersion liquid to 7-7.5 to obtain slurry; carrying out filter pressing treatment on the slurry to obtain low-sodium industrial alumina powder; and mixing the low-sodium industrial alumina powder with a magnesium-containing compound and a rare earth oxide, and calcining to obtain the low-sodium submicron alpha-alumina powder. The low-sodium submicron alpha-alumina powder prepared by the method has low sodium content and high purity, the primary crystal size is submicron, and the process does not add mineralizers such as boron, halide and the like, realizes the controllable growth of the primary crystal, has no pollution to production equipment, and is convenient for large-scale production.
Description
Technical Field
The invention relates to the technical field of powder materials, in particular to low-sodium submicron alpha-alumina powder and a preparation method and application thereof.
Background
The high-purity submicron alpha-alumina powder has the advantages of stable crystalline phase, high hardness, good size stability and the like, can be widely applied to reinforcement and toughening of various plastics, rubbers and ceramic products, and is particularly remarkable in the aspects of improving the compactness and the mechanical property of ceramics, the wear resistance and the thermal conductivity of polymer material products and the like. Especially in the aspect of preparing high-performance alumina ceramics, the used alpha-alumina powder must meet the requirements of high purity, good dispersibility, narrow particle size distribution, small particle size, high activity, easy sintering and the like.
There are many conventional methods for producing α -alumina powder, such as a solid phase method, a liquid phase method, and a gas phase method. However, the performance of the prepared powder is not satisfactory, the alpha-alumina powder prepared by some methods has high purity, but the particle size distribution is not uniform and the primary crystal size is too large, and the powder prepared by some methods has fine particle size, but the purity is not high and the dispersibility is poor. Among them, calcination using industrial alumina or aluminum hydroxide is the most common method for preparing α -alumina powder. The method removes sodium impurities by adding a mineralizer, and alpha-alumina powder with different shapes and granularities is obtained by calcining at high temperature. However, the addition of mineralizer makes it difficult to control the primary crystal of the powder and to obtain submicron alpha-alumina powder. In addition, the addition of mineralizers such as boron, halides and the like causes pollution and corrosion to production equipment, and increases the production cost of the alpha-alumina powder. Therefore, the development of a low-cost and environment-friendly method for preparing the low-sodium submicron alpha-alumina powder is a hot issue of interest in the industry.
Disclosure of Invention
The invention aims to provide low-sodium submicron alpha-alumina powder and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of low-sodium submicron alpha-alumina powder, which comprises the following steps:
mixing industrial alumina, organic acid, a dispersant and water, and adjusting the pH value of the obtained dispersion liquid to 7-7.5 to obtain slurry;
carrying out filter pressing treatment on the slurry to obtain low-sodium industrial alumina powder;
and mixing the low-sodium industrial alumina powder with a magnesium-containing compound and a rare earth oxide, and calcining to obtain the low-sodium submicron alpha-alumina powder.
Preferably, the sodium content of the industrial alumina is 0.35 to 0.45wt%.
Preferably, the organic acid comprises one or more of glacial acetic acid, citric acid, tartaric acid and oxalic acid; the mass of the organic acid is 0.1-3% of the mass of the industrial alumina.
Preferably, the dispersant comprises one of ammonium citrate, ammonium polyacrylate, ammonium tartrate and ammonium polyphosphate; the mass of the dispersant is 0.1-1.5% of the mass of the industrial alumina.
Preferably, the sodium content of the low-sodium industrial alumina powder is 0.05 to 0.1 weight percent.
Preferably, the magnesium-containing compound comprises one of magnesium oxide, magnesium carbonate and magnesium hydroxide; the mass of the magnesium-containing compound is 0.05-0.2% of the mass of the low-sodium industrial alumina powder.
Preferably, the rare earth oxide comprises one of lanthanum oxide, yttrium oxide, cerium oxide and ytterbium oxide; the mass of the rare earth oxide is 0.1-0.3% of the mass of the low-sodium industrial alumina powder.
Preferably, the calcining temperature is 1100-1300 ℃, and the holding time is 2-5 hours.
The invention provides the low-sodium submicron alpha-alumina powder prepared by the preparation method of the technical scheme, the purity is 99.9-99.99 wt%, the alpha phase content is 96-99%, the primary crystal size is 0.3-0.8 mu m, and the sodium content is 0.01-0.05 wt%.
The invention provides the application of the low-sodium submicron alpha-alumina powder in high-performance ceramics, precision polishing or heat-conducting fillers.
The invention provides a preparation method of low-sodium submicron alpha-alumina powder, which comprises the following steps: mixing industrial alumina, organic acid, a dispersant and water, and adjusting the pH value of the obtained dispersion liquid to 7-7.5 to obtain slurry; carrying out filter pressing treatment on the slurry to obtain low-sodium industrial alumina powder; and mixing the low-sodium industrial alumina powder with a magnesium-containing compound and a rare earth oxide, and calcining to obtain the low-sodium submicron alpha-alumina powder. The purity of the low-sodium submicron alpha-alumina powder prepared by the invention is 99.9-99.99 wt%, the alpha phase content is 96-99%, the primary crystal size is 0.3-0.8 μm, and the sodium content is 0.01-0.05 wt%. According to the invention, sodium impurities are removed by organic acid, and the primary crystal size of the alpha-alumina powder is regulated and controlled by adopting a magnesium-containing compound and rare earth oxide in a calcination stage, so that the prepared low-sodium submicron alpha-alumina powder has low sodium content and high purity, the primary crystal size is submicron, and the process does not add mineralizers such as boron, halide and the like, realizes controllable growth of primary crystals, has no pollution to production equipment, and is convenient for large-scale production.
Drawings
Fig. 1 is an SEM picture of the low sodium submicron alpha alumina powder prepared in example 2.
Detailed Description
The invention provides a preparation method of low-sodium submicron alpha-alumina powder, which comprises the following steps:
mixing industrial alumina, organic acid, a dispersant and water, and adjusting the pH value of the obtained dispersion liquid to 7-7.5 to obtain slurry;
carrying out filter pressing treatment on the slurry to obtain low-sodium industrial alumina powder;
and mixing the low-sodium industrial alumina powder with a magnesium-containing compound and a rare earth oxide, and calcining to obtain the low-sodium submicron alpha-alumina powder.
The industrial alumina, the organic acid, the dispersant and the water are mixed, and the pH value of the obtained dispersion liquid is adjusted to 7-7.5 to obtain the slurry. In the present invention, the water is preferably deionized water. In the present invention, the solid content of the dispersion obtained by mixing the industrial alumina, the organic acid, the dispersant and water is preferably 50 to 80%, more preferably 54 to 70%.
In the present invention, the sodium content of the industrial alumina is preferably 0.35 to 0.45wt%. In the present invention, the particle size of the industrial alumina is preferably 30 to 80 μm.
In the present invention, the organic acid preferably includes one or more of glacial acetic acid, citric acid, tartaric acid and oxalic acid; the mass of the organic acid is preferably 0.1 to 3%, more preferably 0.5 to 2% of the mass of the industrial alumina. In the invention, the organic acid reacts with sodium oxide in industrial alumina to remove sodium impurities.
In the present invention, the dispersant preferably includes one of ammonium citrate, ammonium polyacrylate, ammonium tartrate and ammonium polyphosphate; the mass of the dispersant is preferably 0.1 to 1.5%, more preferably 0.5 to 1%, of the mass of the industrial alumina.
In the present invention, the method of adjusting the pH of the resulting dispersion to 7 to 7.5 preferably comprises: to the dispersion obtained, aqueous ammonia was added, and washed with deionized water. In the present invention, the mass concentration of the ammonia water is preferably 5 to 20wt%. In the present invention, the pH of the dispersion is preferably 2 to 4, more preferably 2.5 to 3.5. In the present invention, the pH of the slurry is 7 to 7.5, preferably 7.1 to 7.3.
After the slurry is obtained, the low-sodium industrial alumina powder is obtained by performing filter pressing treatment on the slurry. In the present invention, the process parameters of the pressure filtration treatment preferably include: the pressure is 0.5MPa, and the pressurizing time is 30min. The invention removes the water in the slurry through filter pressing treatment.
In the invention, the sodium content of the low-sodium industrial alumina powder is preferably 0.05 to 0.1wt%, and more preferably 0.06 to 0.08wt%; the particle size is preferably 30 to 80 μm.
After the low-sodium industrial alumina powder is obtained, the low-sodium industrial alumina powder, a magnesium-containing compound and a rare earth oxide are mixed and calcined to obtain the low-sodium submicron alpha-alumina powder. In the present invention, the magnesium-containing compound preferably includes one of magnesium oxide, magnesium carbonate and magnesium hydroxide; the mass of the magnesium-containing compound is preferably 0.05 to 0.2%, more preferably 0.1 to 0.2% of the mass of the low-sodium industrial alumina powder. In the invention, the magnesium-containing compound has the function of controlling the primary crystal size of alpha-alumina to obtain submicron crystal grains.
In the present invention, the rare earth oxide preferably includes one of lanthanum oxide, yttrium oxide, cerium oxide, and ytterbium oxide; the mass of the rare earth oxide is preferably 0.1 to 0.3 percent of the mass of the low-sodium industrial alumina powder, and more preferably 0.2 percent. In the invention, the rare earth oxide has the function of controlling the primary crystal size of alpha-alumina in combination with a magnesium-containing compound to obtain submicron crystal grains.
In the present invention, the temperature of the calcination is preferably 1100 to 1300 ℃, more preferably 1150 to 1250 ℃; the holding time is preferably 2 to 5 hours, more preferably 3 to 4 hours. In the present invention, the atmosphere of the calcination is air. In the present invention, gamma-alumina is converted to alpha-alumina during the calcination process.
The invention provides the low-sodium submicron alpha-alumina powder prepared by the preparation method of the technical scheme, the purity is 99.9-99.99 wt%, the alpha phase content is 96-99%, the primary crystal size is 0.3-0.8 mu m, and the sodium content is 0.01-0.05 wt%. In the present invention, the α -phase content refers to a mass fraction.
The invention provides the application of the low-sodium submicron alpha-alumina powder in high-performance ceramics, precision polishing or heat-conducting fillers.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
1 kg of industrial alumina, 1 g of citric acid, 1 g of ammonium tartrate and 1 kg of deionized water are mixed to prepare a dispersion liquid, wherein the solid phase content of the dispersion liquid is 50%, and the pH value is 4; adding ammonia water and deionized water into the dispersion liquid for cleaning, and adjusting the pH value to 7; carrying out filter pressing treatment on the obtained slurry to obtain low-sodium industrial alumina powder, wherein the sodium content is 0.1wt%;
1 kg of the low-sodium industrial alumina powder is mixed with 0.5 g of magnesium oxide and 3 g of yttrium oxide, and the mixture is placed in a kiln to be calcined at 1300 ℃ for 5 hours to obtain the low-sodium submicron alpha-alumina powder, wherein the purity is 99.99wt%, the alpha phase content is 99%, the primary crystal size is 0.8 mu m, and the sodium content is 0.05wt%.
Example 2
1 kg of industrial alumina, 25 g of glacial acetic acid, 5 g of citric acid, 15 g of ammonium citrate and 0.45 kg of deionized water are mixed to prepare a dispersion liquid, wherein the solid phase content of the dispersion liquid is 80%, and the pH value is 2; adding ammonia water and deionized water into the dispersion liquid for cleaning, and adjusting the pH value to 7; carrying out filter pressing treatment on the obtained slurry to obtain low-sodium industrial alumina powder, wherein the sodium content is 0.05wt%;
mixing 1 kg of the low-sodium industrial alumina powder with 2 g of magnesium oxide and 1 g of lanthanum oxide, and calcining the mixture in a kiln at 1100 ℃ for 2 hours to obtain the low-sodium submicron alpha-alumina powder with the purity of 99.9wt%, the alpha phase content of 96%, the primary crystal size of 0.3 mu m and the sodium content of 0.01wt%.
Fig. 1 is an SEM picture of the low-sodium submicron α -alumina powder prepared in example 2, and it can be seen from fig. 1 that the primary crystals of the α -alumina powder are uniform and have a submicron size.
Example 3
1 kg of industrial alumina, 20 g of oxalic acid, 10 g of ammonium polyphosphate and 0.55 kg of deionized water are mixed to prepare a dispersion liquid, wherein the solid phase content of the dispersion liquid is 64.5 percent, and the pH value is 2.5; adding ammonia water and deionized water into the dispersion liquid for cleaning, and adjusting the pH value to 7.5; carrying out filter pressing treatment on the obtained slurry to obtain low-sodium industrial alumina powder, wherein the sodium content is 0.06wt%;
mixing 1 kg of the low-sodium industrial alumina powder with 1 g of magnesium hydroxide and 2 g of cerium oxide, and calcining the mixture in a kiln at 1200 ℃ for 2 hours to obtain the low-sodium submicron alpha-alumina powder with the purity of 99.95wt%, the alpha phase content of 98%, the primary crystal size of 0.5 mu m and the sodium content of 0.02wt%.
Example 4
1 kg of industrial alumina, 5 g of tartaric acid, 5 g of ammonium polyacrylate and 0.43 kg of deionized water are mixed to prepare a dispersion liquid, wherein the solid phase content of the dispersion liquid is 70%, and the pH value is 3.5; adding ammonia water and deionized water into the dispersion liquid for cleaning, and adjusting the pH value to 7.3; carrying out filter pressing treatment on the obtained slurry to obtain low-sodium industrial alumina powder, wherein the sodium content is 0.08wt%;
1 kg of the low-sodium industrial alumina powder, 1 g of magnesium hydroxide and 2 g of cerium oxide are mixed and placed in a kiln to be calcined at 1250 ℃ for 3 hours, and the low-sodium submicron alpha-alumina powder with the purity of 99.92wt%, the alpha phase content of 99%, the primary crystal size of 0.7 mu m and the sodium content of 0.04wt% is obtained.
Example 5
1 kg of industrial alumina, 8 g of oxalic acid, 2 g of glacial acetic acid, 10 g of ammonium citrate and 0.85 kg of deionized water are mixed to prepare a dispersion liquid, wherein the solid phase content of the dispersion liquid is 54%, and the pH value is 3; adding ammonia water and deionized water into the dispersion liquid for cleaning, and adjusting the pH value to 7.1; carrying out filter pressing treatment on the obtained slurry to obtain low-sodium industrial alumina powder, wherein the sodium content is 0.07wt%;
mixing 1 kg of the low-sodium industrial alumina powder with 2 g of magnesium hydroxide and 2 g of ytterbium oxide, and calcining the mixture in a kiln at 1150 ℃ for 5 hours to obtain the low-sodium submicron alpha-alumina powder with the purity of 99.93wt%, the alpha phase content of 97%, the primary crystal size of 0.4 mu m and the sodium content of 0.03wt%.
The embodiment shows that the preparation method provided by the invention is simple, the synthesis temperature is low, the cost is low, the purity of the prepared low-sodium submicron alpha-alumina powder is high, the conversion rate is high, the primary crystal size is small, and the application requirements of high-performance ceramics, precision polishing and heat-conducting fillers can be met.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of low-sodium submicron alpha-alumina powder comprises the following steps:
mixing industrial alumina, organic acid, a dispersant and water, and adjusting the pH value of the obtained dispersion liquid to 7-7.5 to obtain slurry;
carrying out filter pressing treatment on the slurry to obtain low-sodium industrial alumina powder;
and mixing the low-sodium industrial alumina powder with a magnesium-containing compound and a rare earth oxide, and calcining to obtain the low-sodium submicron alpha-alumina powder.
2. The method according to claim 1, wherein the sodium content of the industrial alumina is 0.35 to 0.45wt%.
3. The method of claim 1, wherein the organic acid comprises one or more of glacial acetic acid, citric acid, tartaric acid, and oxalic acid; the mass of the organic acid is 0.1-3% of the mass of the industrial alumina.
4. The method of claim 1, wherein the dispersant comprises one of ammonium citrate, ammonium polyacrylate, ammonium tartrate and ammonium polyphosphate; the mass of the dispersant is 0.1-1.5% of the mass of the industrial alumina.
5. The method according to claim 1, wherein the low-sodium industrial alumina powder has a sodium content of 0.05 to 0.1wt%.
6. The production method according to claim 1, wherein the magnesium-containing compound includes one of magnesium oxide, magnesium carbonate, and magnesium hydroxide; the mass of the magnesium-containing compound is 0.05-0.2% of the mass of the low-sodium industrial alumina powder.
7. The production method according to claim 1, wherein the rare earth oxide includes one of lanthanum oxide, yttrium oxide, cerium oxide, and ytterbium oxide; the mass of the rare earth oxide is 0.1-0.3% of the mass of the low-sodium industrial alumina powder.
8. The method of claim 1, wherein the calcining temperature is 1100-1300 ℃ and the holding time is 2-5 hours.
9. The low-sodium submicron alpha-alumina powder prepared by the preparation method of any one of claims 1 to 8 has a purity of 99.9 to 99.99wt%, an alpha phase content of 96 to 99%, a primary crystal size of 0.3 to 0.8 μm, and a sodium content of 0.01 to 0.05wt%.
10. The use of the low sodium submicron alpha alumina powder of claim 9 in high performance ceramics, precision polishing or heat conducting fillers.
Priority Applications (1)
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