CN116002734A - Production process of high-purity high-dispersibility nanoscale alumina - Google Patents
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- CN116002734A CN116002734A CN202310061656.3A CN202310061656A CN116002734A CN 116002734 A CN116002734 A CN 116002734A CN 202310061656 A CN202310061656 A CN 202310061656A CN 116002734 A CN116002734 A CN 116002734A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 221
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 93
- 239000002002 slurry Substances 0.000 claims abstract description 87
- 239000000843 powder Substances 0.000 claims abstract description 85
- 238000010438 heat treatment Methods 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000007787 solid Substances 0.000 claims abstract description 62
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000006185 dispersion Substances 0.000 claims abstract description 36
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000002244 precipitate Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 15
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 12
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 11
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 39
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 17
- 239000004202 carbamide Substances 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 12
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 11
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 claims description 11
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 11
- 239000001099 ammonium carbonate Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002105 nanoparticle Substances 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- -1 aluminum dipentaerythritol Chemical compound 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 claims description 2
- UAEJRRZPRZCUBE-UHFFFAOYSA-N trimethoxyalumane Chemical compound [Al+3].[O-]C.[O-]C.[O-]C UAEJRRZPRZCUBE-UHFFFAOYSA-N 0.000 claims description 2
- OBROYCQXICMORW-UHFFFAOYSA-N tripropoxyalumane Chemical compound [Al+3].CCC[O-].CCC[O-].CCC[O-] OBROYCQXICMORW-UHFFFAOYSA-N 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 3
- 238000007670 refining Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 13
- 238000011010 flushing procedure Methods 0.000 abstract description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a production process of high-purity and high-dispersibility nanoscale alumina, which comprises the following steps: hydrolyzing aluminum salt to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, regulating the pH of the system to be alkaline, and performing ultrasonic dispersion to obtain hydrated alumina slurry; carrying out high-temperature high-pressure hydrothermal refinement on the hydrated alumina slurry to obtain nano hydrated alumina slurry, cooling, aging, carrying out solid-liquid separation, putting the nano hydrated alumina slurry obtained by washing and filtering into ethylene glycol solution, heating, adding a dispersing agent B into the ethylene glycol solution, and carrying out ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; separating solid and liquid to obtain nano alumina hydrate dispersion slurry, washing, filtering and drying to obtain nano alumina hydrate solid powder; and (3) carrying out opposite flushing and vacuum roasting by using high-pressure nitrogen or carbon dioxide to obtain the nano-scale alumina powder. The nano-scale alumina prepared by the method has the characteristics of good dispersibility and high purity, and can be used for preparing alumina ceramic substrates.
Description
Technical Field
The invention belongs to the technical field of ceramic powder preparation, and particularly relates to a production process of high-purity and high-dispersibility nanoscale alumina.
Background
Nano alumina has many excellent characteristics such as high heat conductivity, high insulation, high hardness, high temperature resistance, corrosion resistance, wear resistance and the like. The nano alumina powder is mainly used as raw material powder of an alumina ceramic substrate, and the alumina ceramic substrate is mainly used for chip resistor LED encapsulation. The main methods for preparing nano alumina at present are an aluminum alkoxide method, a pyrolysis method, an amorphous crystallization method, a sol-gel method, a liquid phase precipitation method and the like, wherein the aluminum alkoxide method is the most widely used alumina preparation method in the industry at present.
The purity and dispersion performance of the nano alumina powder influence the quality of the prepared alumina ceramic substrate, and the preparation of the ceramic substrate generally requires high-purity nano alumina powder with the purity of more than 99.7 percent, and meanwhile, the requirements on the dispersibility and the uniformity of the particle size distribution of the nano alumina are extremely high. The electric ceramic substrate obtained by sintering the nano alumina powder with high purity and good dispersibility has more excellent heat conduction coefficient, thermal expansion coefficient, bending strength mechanical property and the like, and because the alumina powder with smaller size particle diameter can be pressed and sintered to obtain a more compact electric ceramic substrate, the electric ceramic substrate has lower heating growth amount, is more suitable for being used as a high-temperature resistant insulating material, and has fewer defects such as pores among alumina phases. The existing aluminum alkoxide method is less ideal in dispersibility of the aluminum oxide powder, and the particle size distribution of the aluminum oxide powder is not concentrated. In order to prepare the nano alumina powder with high purity, high dispersibility and concentrated particle size distribution so as to meet the sintering preparation of the electric ceramic substrate with high heat conduction coefficient, low thermal expansion coefficient and high bending strength, the current nano alumina production process needs to be improved.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a process for producing high purity, high dispersibility nano-scale alumina, comprising:
firstly, hydrolyzing aluminum salt to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, adjusting the pH value of the system to be alkaline after dispersing, and obtaining hydrated alumina slurry after ultrasonic dispersion;
carrying out high-temperature high-pressure hydrothermal refinement on the hydrated alumina slurry to obtain nano hydrated alumina slurry, cooling, aging, carrying out solid-liquid separation, putting the washed and filtered nano hydrated alumina slurry into a glycol solution with the weight of 2-12%, heating, and adding a dispersing agent B into the glycol solution for ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, and washing, filtering and drying to obtain nano hydrated alumina solid powder; the nano hydrated alumina solid powder is hedged by high-pressure nitrogen or carbon dioxide, and then the nano alumina powder is obtained through vacuum roasting.
Preferably, in the first step, the aluminum salt is one of aluminum isopropoxide, aluminum ethoxide, aluminum methoxide, aluminum propoxide, aluminum hexanoxide and aluminum dipentaerythritol.
Preferably, the dispersing agent A in the first step is a mixed dispersing agent composed of polyethylene glycol, citric acid and tetramethyl disilazane according to a mass ratio of 3:1:1-2, and the dosage of the dispersing agent A is 0.4-12% of the mass of the aluminum salt.
Preferably, in the first step, after adding the dispersing agent A, stirring for 15-40 min at a rotating speed of 300-450 r/min; the method for regulating the pH value of the system to be alkaline is to add sodium hydroxide into the system to regulate the pH value to 8-10; the ultrasonic dispersion frequency is 45-80 kHz, and the dispersion time is 35-55 min.
Preferably, in the second step, the method for obtaining nano hydrated alumina slurry by carrying out high-temperature high-pressure hydrothermal refinement on the hydrated alumina slurry comprises the following steps: heating the hydrated alumina slurry to 60-95 ℃ at a heating rate of 5-8 ℃/min, stirring at a speed of 600-800 r/min for 10-15 min, and then preserving heat for 1-2 h; adding ammonium bicarbonate into a reaction kettle, wherein the adding amount is 4-10% of the mass of aluminum salt, heating to 180-225 ℃ at the heating rate of 10-15 ℃/min, pressurizing the reaction kettle to 2-3.6 Mpa, and maintaining constant pressure and temperature for 2-4 h to obtain the nano hydrated alumina slurry.
Preferably, the aging temperature in the second step is 25-32 ℃ and the aging time is 5-20 h.
Preferably, in the second step, the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200, and the dosage of the dispersant B is 5-10% of the mass of aluminum salt; the preparation method of the dispersant B comprises the following steps: weighing 12-25 parts by weight of polyvinyl alcohol, heating 60-80 parts by weight of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 0.5-2 parts by weight of urea, stirring and dissolving, and preserving heat for 20-60 min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, adding 1.5-4 parts of polyethylene glycol-200, stirring and dissolving, and standing for 1-2 hours to obtain a dispersing agent solution; and in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B.
Preferably, in the third step, ethanol is used to wash the nano-alumina hydrate dispersion slurry, and the drying temperature is 120-140 ℃.
Preferably, in the third step, the specific method for hedging the nano alumina hydrate solid powder by using high-pressure nitrogen or carbon dioxide is as follows: two ejectors which are horizontally arranged oppositely are adopted, wherein one ejector ejects high-pressure nitrogen or carbon dioxide, the other ejector ejects nano-alumina hydrate solid powder, and the nano-alumina hydrate solid powder is further atomized and dispersed through the high-pressure nitrogen or the carbon dioxide; wherein, the pressurization of the injector for nitrogen and carbon dioxide is 30-40 kPa, and the pressurization for nano-alumina hydrate solid powder is 10-15 kPa.
Preferably, in the third step, the roasting temperature of the nano-scale alumina powder obtained by vacuum roasting is 500-800 ℃, and the vacuum degree during roasting is less than 2.5X10 ﹣4 Pa, and roasting time is 1-3 h.
The invention at least comprises the following beneficial effects: the nano-scale alumina prepared by the method has the characteristics of good dispersibility, high purity and concentrated particle size distribution, and can be used as raw material powder of an alumina ceramic substrate.
In the process of preparing the nano-alumina powder, an aluminum alkoxide method is used, no impurities are introduced in the processes of hydrolysis, dispersion hedging, roasting and the like, all the used reagents can be dissolved in deionized water or ethanol, and the reagents can be removed in a slurry in a washing way, so that the purity of the finally prepared nano-alumina powder is high, and can reach more than 99.7%.
In the whole process of preparing the nano-scale alumina powder, the dispersibility of the hydrated alumina slurry is maintained, and the hydrated alumina precipitate obtained by hydrolysis is subjected to dispersion treatment by using the dispersant A in the early stage; when the nano hydrated alumina slurry is obtained through high-temperature high-pressure hydrothermal refinement, ammonium bicarbonate is added into the system, ammonia gas and carbon dioxide released by the thermal decomposition of the ammonium bicarbonate act on the hydrated alumina slurry, so that the reaction is more sufficient, meanwhile, a dispersing effect is formed on the hydrated alumina slurry, and the dispersibility of the hydrated alumina slurry in the hydrothermal refinement process is ensured; carrying out high-temperature high-pressure hydrothermal refinement on the hydrated alumina slurry to obtain nano hydrated alumina slurry, and then carrying out dispersion treatment on the slurry by using ethanol and a dispersing agent B; when the nano-scale alumina powder is finally prepared, high-pressure nitrogen and carbon dioxide are used for carrying out opposite flushing with the nano-scale alumina solid powder, compared with the conventional liquid opposite flushing, the high-pressure gaseous opposite flushing has higher pressure, the flushing effect on the nano-scale alumina solid powder is better, and meanwhile, the solid-liquid separation, washing and drying operations are not required for the later-stage nano-scale alumina solid powder, so that the process flow is simplified, and the production cost is reduced; finally, dehydrating the nano hydrated alumina solid powder by using a vacuum roasting mode to obtain nano alumina powder.
Wherein the dispersing agent A is slurry with polyethylene glycol, citric acid and tetramethyl disilazane as main raw materials and the dispersing agent B is slurry with the surface being subjected to dispersion treatment of the dispersing agent B by blending modified polyvinyl alcohol, urea and polyethylene glycol-200, so that the agglomeration of nano hydrated alumina in the slurry is greatly reduced, and the dispersion of the nano hydrated alumina is improved; the dispersing agent A and the dispersing agent B are easy to dissolve in water and are easy to separate from slurry, so that impurities are not brought to the product, and the purity of the nano alumina is ensured.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention by reference to the specification.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
The embodiment provides a production process of high-purity and high-dispersibility nanoscale alumina, which comprises the following steps of:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 15min at a rotating speed of 300r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 8, and performing ultrasonic dispersion at a frequency of 45kHz for 35min to obtain hydrated alumina slurry; wherein dispersant A comprises 2.4g polyethylene glycol, 0.8g citric acid and 0.8g tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 60 ℃ at a heating rate of 5 ℃/min, stirring at a speed of 600r/min for 10min, and then preserving heat for 1h; adding 40g of ammonium bicarbonate into a reaction kettle, heating to 180 ℃ at a heating rate of 10 ℃/min, pressurizing the reaction kettle to 2Mpa, maintaining constant pressure and temperature for 2h to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 5h, performing solid-liquid separation, putting the nano hydrated alumina slurry obtained by washing and filtering into 2%wt of glycol solution, heating, adding 50g of dispersing agent B into the glycol solution, and performing ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; wherein the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200; the preparation method of the dispersing agent B comprises the following steps: weighing 120g of polyvinyl alcohol according to parts by weight, heating 600g of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 5g of urea, stirring and dissolving, and preserving the temperature for 20min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, 15g of polyethylene glycol-200 is added, stirred and dissolved, and the mixture is kept stand for 1h to obtain a dispersing agent solution; in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, washing with ethanol, filtering, and drying at 120 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is subjected to opposite flushing by using high-pressure nitrogen, specifically, two ejectors which are horizontally arranged in opposite mode are adopted, wherein one ejector ejects the high-pressure nitrogen, the other ejector ejects the nanometer hydrated alumina solid powder, and the nanometer hydrated alumina solid powder is further atomized and dispersed by the high-pressure nitrogen; wherein, the pressurization of the injector for nitrogen is 30kPa, and the pressurization for nano-alumina hydrate solid powder is 10kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 500 deg.C, and the vacuum degree is less than 2.5X10 when roasting ﹣4 Pa, and roasting time of 1h.
Example 2
The embodiment provides a production process of high-purity and high-dispersibility nanoscale alumina, which comprises the following steps of:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 20min at a rotating speed of 350r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 8, and performing ultrasonic dispersion at a frequency of 50kHz for 40min to obtain hydrated alumina slurry; wherein the dispersant A comprises 6g of polyethylene glycol, 2g of citric acid and 2g of tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 70 ℃ at a heating rate of 6 ℃/min, stirring at a speed of 600r/min for 10min, and then preserving heat for 1h; adding 50g of ammonium bicarbonate into a reaction kettle, heating to 200 ℃ at a heating rate of 12 ℃/min, pressurizing the reaction kettle to 2.2Mpa, maintaining constant pressure and temperature for 2h to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 6h, performing solid-liquid separation, putting the washed and filtered nano hydrated alumina slurry into 5%wt ethylene glycol solution, heating, adding 60g of dispersing agent B into the ethylene glycol solution, and performing ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; wherein the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200; the preparation method of the dispersing agent B comprises the following steps: weighing 150g of polyvinyl alcohol according to parts by weight, heating 700g of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 10g of urea, stirring and dissolving, and preserving the temperature for 30min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, adding 20g of polyethylene glycol-200, stirring and dissolving, and standing for 1h to obtain a dispersing agent solution; in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, washing with ethanol, filtering, and drying at 130 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is subjected to high-pressure opposite flushing, specifically, two ejectors which are horizontally arranged in opposite mode are adopted, wherein one ejector ejects high-pressure nitrogen, the other ejector ejects the nanometer hydrated alumina solid powder, and the nanometer hydrated alumina solid powder is further atomized and dispersed through the high-pressure nitrogen; wherein, the pressurization of the injector for nitrogen is 32kPa, and the pressurization for nano-alumina hydrate solid powder is 10kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 600 deg.C, and the vacuum degree is less than 2.5×10 when roasting ﹣4 Pa, and roasting time of 1h.
Example 3
The embodiment provides a production process of high-purity and high-dispersibility nanoscale alumina, which comprises the following steps of:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 30min at a rotating speed of 400r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 9, and performing ultrasonic dispersion at a frequency of 70kHz for 50min to obtain hydrated alumina slurry; wherein the dispersant A comprises 30g of polyethylene glycol, 20g of citric acid and 20g of tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 90 ℃ at a heating rate of 7 ℃/min, stirring at a speed of 700r/min for 10min, and then preserving heat for 2h; adding 80g of ammonium bicarbonate into a reaction kettle, heating to 210 ℃ at a heating rate of 14 ℃/min, pressurizing the reaction kettle to 3.0Mpa, maintaining constant pressure and temperature for 3 hours to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 6 hours, performing solid-liquid separation, putting the washed and filtered nano hydrated alumina slurry into an ethylene glycol solution with the weight of 8%, heating, adding 80g of dispersing agent B into the ethylene glycol solution, and performing ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; wherein the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200; the preparation method of the dispersing agent B comprises the following steps: weighing 200g of polyvinyl alcohol according to parts by weight, heating 700g of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 15g of urea, stirring and dissolving, and preserving the temperature for 40min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, 25g of polyethylene glycol-200 is added, stirred and dissolved, and the mixture is kept stand for 2 hours to obtain a dispersing agent solution; in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, washing with ethanol, filtering, and drying at 130 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is heduled by high-pressure carbon dioxide, specifically, two ejectors which are horizontally arranged oppositely are adopted, wherein one ejector ejects high-pressure nitrogen, the other ejector ejects the nanometer hydrated alumina solid powder, and the nanometer hydrated alumina solid powder is further atomized and dispersed by the high-pressure nitrogen; wherein, the pressurization of the injector for nitrogen is 36kPa, and the pressurization for nano-alumina hydrate solid powder is 13kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 700 deg.C, and the vacuum degree is less than 2.5×10 when roasting ﹣4 Pa, and roasting time is 2h.
Example 4
The embodiment provides a production process of high-purity and high-dispersibility nanoscale alumina, which comprises the following steps of:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 40min at the rotating speed of 450r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 10, and performing ultrasonic dispersion for 55min at the frequency of 80kHz to obtain hydrated alumina slurry; wherein the dispersant A comprises 72g of polyethylene glycol, 48g of citric acid and 48g of tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 95 ℃ at a heating rate of 8 ℃/min, stirring at a speed of 800r/min for 15min, and then preserving heat for 2h; adding 100g of ammonium bicarbonate into a reaction kettle, heating to 225 ℃ at a heating rate of 15 ℃/min, pressurizing the reaction kettle to 3.6Mpa, maintaining constant pressure and temperature for 4 hours to obtain nano hydrated alumina slurry, cooling, aging at 32 ℃ for 20 hours, performing solid-liquid separation, putting the washed and filtered nano hydrated alumina slurry into 12%wt ethylene glycol solution, heating, adding 100g of dispersing agent B into the ethylene glycol solution, and performing ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; wherein the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200; the preparation method of the dispersing agent B comprises the following steps: weighing 250g of polyvinyl alcohol according to parts by weight, heating 800g of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 20g of urea, stirring and dissolving, and preserving the temperature for 60min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, 40g of polyethylene glycol-200 is added, stirred and dissolved, and the mixture is kept stand for 2 hours to obtain a dispersing agent solution; in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, washing with ethanol, filtering, and drying at 140 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is opposite flushed by high pressure carbon dioxide, in particular to a horizontal relative methodTwo ejectors are arranged, wherein one ejector ejects high-pressure nitrogen, the other ejector ejects nano-alumina hydrate solid powder, and the nano-alumina hydrate solid powder is further atomized and dispersed by the high-pressure nitrogen; wherein, the pressurization of the injector for nitrogen is 40kPa, and the pressurization for nano-alumina hydrate solid powder is 15kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 800 ℃, and the vacuum degree during roasting is less than 2.5 multiplied by 10 ﹣4 Pa, and roasting time is 3h.
Comparative example 1
The comparative example provides a production process of high-purity nanoscale aluminum oxide, which comprises the following steps:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 15min at a rotating speed of 300r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 8, and performing ultrasonic dispersion at a frequency of 45kHz for 35min to obtain hydrated alumina slurry; wherein dispersant A comprises 2.4g polyethylene glycol, 0.8g citric acid and 0.8g tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 60 ℃ at a heating rate of 5 ℃/min, stirring at a speed of 600r/min for 10min, and then preserving heat for 1h; adding 40g of ammonium bicarbonate into a reaction kettle, heating to 180 ℃ at a heating rate of 10 ℃/min, pressurizing the reaction kettle to 2Mpa, maintaining constant pressure and temperature for 2h to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 5h, performing solid-liquid separation, washing, and filtering to obtain nano hydrated alumina slurry;
step three, washing the nano hydrated alumina slurry with ethanol, filtering, and drying at 120 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is subjected to opposite flushing by using high-pressure nitrogen, specifically, two ejectors which are horizontally arranged in opposite mode are adopted, wherein one ejector ejects the high-pressure nitrogen, the other ejector ejects the nanometer hydrated alumina solid powder, and the nanometer hydrated alumina solid powder is further atomized and dispersed by the high-pressure nitrogen; wherein, the pressurization of the injector for nitrogen is 30kPa, and the injector is used for nano hydrated alumina solid powderThe final pressurization is 10kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 500 deg.C, and the vacuum degree is less than 2.5X10 when roasting ﹣4 Pa, and roasting time of 1h.
Comparative example 2
The comparative example provides a production process of high-purity nanoscale aluminum oxide, which comprises the following steps:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 20min at a rotating speed of 350r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 8, and performing ultrasonic dispersion at a frequency of 50kHz for 40min to obtain hydrated alumina slurry; wherein the dispersant A comprises 6g of polyethylene glycol, 2g of citric acid and 2g of tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 70 ℃ at a heating rate of 6 ℃/min, stirring at a speed of 600r/min for 10min, and then preserving heat for 1h; adding 50g of ammonium bicarbonate into a reaction kettle, heating to 200 ℃ at a heating rate of 12 ℃/min, pressurizing the reaction kettle to 2.2Mpa, maintaining constant pressure and temperature for 2h to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 6h, performing solid-liquid separation, washing, and filtering to obtain nano hydrated alumina slurry
Step three, washing the obtained nano hydrated alumina slurry by using ethanol, filtering, and drying at 130 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is subjected to opposite flushing by using high-pressure nitrogen, specifically, two ejectors which are horizontally arranged in opposite mode are adopted, wherein one ejector ejects the high-pressure nitrogen, the other ejector ejects the nanometer hydrated alumina solid powder, and the nanometer hydrated alumina solid powder is further atomized and dispersed by the high-pressure nitrogen; wherein, the pressurization of the injector for nitrogen is 32kPa, and the pressurization for nano-alumina hydrate solid powder is 10kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 600 deg.C, and the vacuum degree is less than 2.5×10 when roasting ﹣4 Pa, roasting time of 1h
Comparative example 3
The comparative example provides a production process of high-purity nanoscale aluminum oxide, which comprises the following steps:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 15min at a rotating speed of 300r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 8, and performing ultrasonic dispersion at a frequency of 45kHz for 35min to obtain hydrated alumina slurry; wherein dispersant A comprises 2.4g polyethylene glycol, 0.8g citric acid and 0.8g tetramethyl disilazane;
step two, raising the temperature of the hydrated alumina slurry to 60 ℃, stirring at 600r/min for 10min, and then preserving heat for 1h; heating to 180 ℃, pressurizing the reaction kettle to 2Mpa, maintaining constant pressure and temperature for 2h to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 5h, performing solid-liquid separation, putting the nano hydrated alumina slurry obtained by washing and filtering into 2%wt of glycol solution, heating, adding 50g of dispersing agent B into the glycol solution, and performing ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; wherein the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200; the preparation method of the dispersing agent B comprises the following steps: weighing 120g of polyvinyl alcohol according to parts by weight, heating 600g of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 5g of urea, stirring and dissolving, and preserving the temperature for 20min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, 15g of polyethylene glycol-200 is added, stirred and dissolved, and the mixture is kept stand for 1h to obtain a dispersing agent solution; in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, washing with ethanol, filtering, and drying at 120 ℃ to obtain nano hydrated alumina solid powder; the nanometer hydrated alumina solid powder is subjected to opposite flushing by using high-pressure nitrogen, specifically, two ejectors which are horizontally arranged in opposite mode are adopted, wherein one ejector ejects the high-pressure nitrogen, the other ejector ejects the nanometer hydrated alumina solid powder, and the nanometer hydrated alumina solid powder is further atomized by the high-pressure nitrogenAnd (5) flushing and dispersing; wherein, the pressurization of the injector for nitrogen is 30kPa, and the pressurization for nano-alumina hydrate solid powder is 10kPa; then vacuum roasting to obtain nano-scale alumina powder, the vacuum roasting temperature is 500 deg.C, and the vacuum degree is less than 2.5X10 when roasting ﹣4 Pa, and roasting time of 1h.
Comparative example 4
The comparative example provides a production process of high-purity nanoscale aluminum oxide, which comprises the following steps:
firstly, hydrolyzing 1kg of aluminum isopropoxide to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, stirring for 15min at a rotating speed of 300r/min, adding sodium hydroxide into a system after dispersion to adjust the pH of the system to 8, and performing ultrasonic dispersion at a frequency of 45kHz for 35min to obtain hydrated alumina slurry; wherein dispersant A comprises 2.4g polyethylene glycol, 0.8g citric acid and 0.8g tetramethyl disilazane;
step two, heating the hydrated alumina slurry to 60 ℃ at a heating rate of 5 ℃/min, stirring at a speed of 600r/min for 10min, and then preserving heat for 1h; adding 40g of ammonium bicarbonate into a reaction kettle, heating to 180 ℃ at a heating rate of 10 ℃/min, pressurizing the reaction kettle to 2Mpa, maintaining constant pressure and temperature for 2h to obtain nano hydrated alumina slurry, cooling, aging at 25 ℃ for 5h, performing solid-liquid separation, putting the nano hydrated alumina slurry obtained by washing and filtering into 2%wt of glycol solution, heating, adding 50g of dispersing agent B into the glycol solution, and performing ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry; wherein the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200; the preparation method of the dispersing agent B comprises the following steps: weighing 120g of polyvinyl alcohol according to parts by weight, heating 600g of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 5g of urea, stirring and dissolving, and preserving the temperature for 20min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, 15g of polyethylene glycol-200 is added, stirred and dissolved, and the mixture is kept stand for 1h to obtain a dispersing agent solution; in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, washing with ethanol, filtering, and drying at 120 ℃ to obtain nano hydrated alumina solid powder; the nano-scale alumina powder is obtained through vacuum roasting, the vacuum roasting temperature is 500 ℃, and the vacuum degree during roasting is less than 2.5 multiplied by 10 ﹣4 Pa, and roasting time of 1h.
The high purity, high dispersibility nano-sized alumina powder obtained in example 1-example 4, the average particle diameter D50 of the high purity nano-sized alumina powder obtained in comparative example 1-comparative example 4, and the heat conduction coefficient, the heat expansion coefficient, and the bending strength of the power package substrate samples obtained by sintering the nano-sized alumina powder of example 1-example 4, comparative example 1-comparative example 4 were each measured, wherein the sintering temperature of each sample was 1600 ℃, and the time after heat preservation was 6 hours, respectively, to obtain the following table:
from the above table, it can be seen that the nano-scale alumina ceramics prepared by the production process of the high-purity and high-dispersibility nano-scale alumina provided by the invention in the embodiment 1-embodiment 4 have smaller particle size and better dispersibility, so that defects such as bulk pores in the sintered power ceramic substrate are fewer, and the powder of the sintered power ceramic substrate is more compact, thereby having higher heat conduction coefficient, lower thermal expansion coefficient and higher bending strength.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use for which the invention is suited, and further modifications may be readily made by one skilled in the art, and the invention is therefore not to be limited to the particular details and examples shown and described herein, without departing from the general concepts defined by the claims and the equivalents thereof.
Claims (10)
1. The production process of the high-purity high-dispersibility nanoscale alumina is characterized by comprising the following steps of:
firstly, hydrolyzing aluminum salt to prepare hydrated alumina precipitate, adding a dispersing agent A into the hydrated alumina precipitate, adjusting the pH value of the system to be alkaline after dispersing, and obtaining hydrated alumina slurry after ultrasonic dispersion;
carrying out high-temperature high-pressure hydrothermal refinement on the hydrated alumina slurry to obtain nano hydrated alumina slurry, cooling, aging, carrying out solid-liquid separation, putting the washed and filtered nano hydrated alumina slurry into a glycol solution with the weight of 2-12%, heating, adding a dispersing agent B into the glycol solution, and carrying out ultrasonic dispersion to obtain nano hydrated alumina dispersion slurry;
step three, separating solid and liquid to obtain nano hydrated alumina dispersion slurry, and washing, filtering and drying to obtain nano hydrated alumina solid powder; the nano hydrated alumina solid powder is hedged by high-pressure nitrogen or carbon dioxide, and then the nano alumina powder is obtained through vacuum roasting.
2. The process for producing high purity, high dispersibility nano-sized alumina according to claim 1, wherein in the first step, the aluminum salt is one of aluminum isopropoxide, aluminum ethoxide, aluminum methoxide, aluminum propoxide, aluminum hexanoxide and aluminum dipentaerythritol.
3. The process for producing high-purity and high-dispersibility nano-scale alumina according to claim 1, wherein the dispersant A in the first step is a mixed dispersant comprising polyethylene glycol, citric acid and tetramethyl disilazane according to a mass ratio of 3:1:1-2, and the amount of the dispersant A is 0.4-12% of the mass of the aluminum salt.
4. The process for producing high purity, high dispersibility nano-scale alumina according to claim 1, wherein in the first step, after adding dispersant a, stirring at a rotational speed of 300-450 r/min for 15-40 min; the method for regulating the pH value of the system to be alkaline is to add sodium hydroxide into the system to regulate the pH value to 8-10; the ultrasonic dispersion frequency is 45-80 kHz, and the dispersion time is 35-55 min.
5. The process for producing high purity, high dispersibility nano-scale alumina according to claim 1, wherein in the second step, the method for obtaining nano-alumina hydrate slurry by high temperature and high pressure hydrothermal refining of the alumina hydrate slurry comprises: heating the hydrated alumina slurry to 60-95 ℃ at a heating rate of 5-8 ℃/min, stirring at a speed of 600-800 r/min for 10-15 min, and then preserving heat for 1-2 h; adding ammonium bicarbonate into a reaction kettle, wherein the adding amount is 4-10% of the mass of aluminum salt, heating to 180-225 ℃ at the heating rate of 10-15 ℃/min, pressurizing the reaction kettle to 2-3.6 Mpa, and maintaining constant pressure and temperature for 2-4 h to obtain the nano hydrated alumina slurry.
6. The process for producing high purity, high dispersibility nano-sized alumina according to claim 1, wherein the aging temperature in the second step is 25 to 32 ℃ and the aging time is 5 to 20 hours.
7. The process for producing high-purity and high-dispersibility nano-scale alumina according to claim 1, wherein in the second step, the dispersant B is a blending modified dispersant of polyvinyl alcohol, urea and polyethylene glycol-200, and the amount of the dispersant B is 5-10% of the mass of aluminum salt; the preparation method of the dispersant B comprises the following steps: weighing 12-25 parts by weight of polyvinyl alcohol, heating 60-80 parts by weight of deionized water to above 95 ℃, then adding the polyvinyl alcohol, stirring until the polyvinyl alcohol is completely dissolved, cooling the solution to 40 ℃, adding 0.5-2 parts by weight of urea, stirring and dissolving, and preserving heat for 20-60 min to obtain a mixed solution; after the temperature of the mixed solution is reduced to 25 ℃, adding 1.5-4 parts of polyethylene glycol-200, stirring and dissolving, and standing for 1-2 hours to obtain a dispersing agent solution; and in a nitrogen atmosphere, heating and evaporating deionized water in the complete dispersing agent solution to obtain a dispersing agent B.
8. The process for producing high purity, high dispersibility nano-sized alumina according to claim 1, wherein in the third step, the nano-sized alumina hydrate dispersion slurry is washed with ethanol, and the drying temperature is 120 to 140 ℃.
9. The process for producing high purity, high dispersibility nano-scale alumina according to claim 1, wherein in the third step, the specific method for using high pressure nitrogen or carbon dioxide for hedging the nano-alumina hydrate solid powder is as follows: two ejectors which are horizontally arranged oppositely are adopted, wherein one ejector ejects high-pressure nitrogen or carbon dioxide, the other ejector ejects nano-alumina hydrate solid powder, and the nano-alumina hydrate solid powder is further atomized and dispersed through the high-pressure nitrogen or the carbon dioxide; wherein, the pressurization of the injector for nitrogen and carbon dioxide is 30-40 kPa, and the pressurization for nano-alumina hydrate solid powder is 10-15 kPa.
10. The process for producing high purity and high dispersibility nano-sized alumina according to claim 1, wherein in said step three, the firing temperature of the nano-sized alumina powder obtained by vacuum firing is 500 to 800 ℃, and the degree of vacuum upon firing is less than 2.5X10 ﹣4 Pa, and roasting time is 1-3 h.
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