CN115340113B - Preparation method of gas-phase nanometer alumina - Google Patents
Preparation method of gas-phase nanometer alumina Download PDFInfo
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- CN115340113B CN115340113B CN202211134491.XA CN202211134491A CN115340113B CN 115340113 B CN115340113 B CN 115340113B CN 202211134491 A CN202211134491 A CN 202211134491A CN 115340113 B CN115340113 B CN 115340113B
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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 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 230000002776 aggregation Effects 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000004220 aggregation Methods 0.000 claims abstract description 12
- 238000010791 quenching Methods 0.000 claims abstract description 12
- 230000000171 quenching effect Effects 0.000 claims abstract description 12
- 239000012798 spherical particle Substances 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 230000005284 excitation Effects 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005054 agglomeration Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 15
- 239000000843 powder Substances 0.000 abstract description 9
- 239000011858 nanopowder Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000007921 spray Substances 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 238000002485 combustion reaction Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910000761 Aluminium amalgam Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 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 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- -1 aluminum alkoxide Chemical class 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
- C01F7/422—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature
- C01F7/424—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature using a plasma
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- Nanotechnology (AREA)
- Plasma & Fusion (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A preparation method of nanometer alumina by a gas phase method, which relates to the technical field of nanometer material preparation. Firstly, preprocessing the alumina sol to obtain high-purity alumina sol, then utilizing a high-temperature plasma reactor to instantaneously react, finally cooling through a quenching system, and utilizing a grading collection system to obtain the gas-phase nanometer alumina. The invention realizes the preparation of the high-purity alumina nano powder, has the advantages of simple and convenient process, low cost, high product purity and the like, and can be used for large-scale production. The prepared alumina is in the form of spherical particles with the diameter of 10-50 nm, no aggregation and in the form of monodispersion. The invention abandons the defect of feeding the traditional powder material, firstly proposes that the alumina sol enters the reaction chamber in a spray mode, can realize uniform reaction, can realize effective control of particle size by controlling the feeding flow, and is beneficial to preparing the monodisperse form of the alumina nano powder.
Description
Technical Field
The invention relates to the technical field of nano powder material preparation, in particular to a preparation method of alumina, and especially relates to a preparation method of gas-phase nano alumina.
Background
Alumina has high melting point, high hardness and high chemical stability, and is widely used in the industries of paint, plastics, paper making, printing ink, chemical fiber, rubber, cosmetics and the like. At present, the preparation method of the alumina mainly comprises the following steps: firstly, preparing hydrated alumina, and then further processing the hydrated alumina into activated alumina. The hydrated alumina is prepared by using sodium metaaluminate, aluminum hydroxide, aluminum sulfate, aluminum chloride, aluminum isopropoxide, aluminum amalgam and the like which are obtained by processing bauxite as raw materials, and using an aluminum alkoxide method, an aluminum amalgam method, an alkaline method (or called acid precipitation method) and an acid method (or called alkali precipitation method).
With plasma technologyThe development of plasma processes for the production of alumina has been ongoing and has been reported in some documents or patents. Chinese patent application CN 112723399A discloses a plasma arc flame combustion reaction system and preparing high purity gamma-Al using the same 2 O 3 Through a novel designed plasma arc flame combustion reaction system, the method can realize high-purity gamma-Al 2 O 3 Fast preparation of nano powder, and fast synthesis of nano gamma-Al with high purity and large specific surface area by one-step ionic arc combustion 2 O 3 . The method mainly adopts the method that the high-purity pseudo-boehmite coarse powder (the purity is generally up to 99.9 percent) is treated by using a dispersion grinding device to obtain the high-purity pseudo-boehmite fine powder, which is more beneficial to the plasma arc flame combustion reaction, and the prepared high-purity gamma-Al 2 O 3 The nano powder can be obtained without secondary grinding.
However, the reaction system mainly utilizes carrier gas to carry high-purity pseudo-boehmite fine powder into a plasma arc flame combustion chamber, and the conveying flow of powder materials is difficult to control. Compared with powder materials, sol in colloid form is easier to spray into a combustion chamber, the feeding flow is controllable, and the preparation of alumina materials with uniform morphology can be realized.
Disclosure of Invention
Aiming at the defects of the related technology existing in the preparation of alumina powder, the invention provides a preparation method of gas-phase nanometer alumina, which comprises the steps of firstly preprocessing alumina sol to obtain high-purity alumina sol, then utilizing a high-temperature plasma reactor to instantaneously react, finally cooling through a quenching system, and utilizing a grading collection system to obtain the gas-phase nanometer alumina.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the preparation process of nanometer alumina in gas phase includes the following steps:
(1) purifying the crude product of the alumina sol to prepare high-purity alumina sol;
(2) spraying the mixture into a high-temperature plasma reactor by adopting a high-pressure spraying method to instantaneously react to prepare nano alumina;
(3) cooling the quenching system;
(4) and a grading collection system, so as to prepare the gas phase nanometer alumina.
As a preferable technical scheme of the invention, the step (1) of preparing the high-purity alumina sol by using the crude alumina sol comprises the following steps:
(1) Evaporating the crude aluminum sol slurry under the condition of vacuum heating until the water content reaches 15-30%, and cooling to room temperature;
(2) Adding absolute ethyl alcohol into the slurry, uniformly dispersing by ultrasonic, then adding a silane coupling agent KH550, heating to 50-60 ℃ and stirring for 1-3 h; the adding weight ratio of the slurry to the absolute ethyl alcohol to the silane coupling agent KH550 is 1:1.5 to 2.5:0.3 to 0.6;
(3) Evaporating again under the condition of vacuum heating until the water-ethanol content reaches 5-10%, and cooling to room temperature to obtain the high-purity aluminum sol.
As a preferable technical scheme of the invention, the specific steps in the step (2) are as follows:
the high-pressure spraying method is adopted, high-purity alumina sol is sprayed into a reaction cavity of a high-temperature plasma reactor by a pump, plasma excitation gas of the high-temperature plasma reactor is nitrogen or argon, and the alumina sol is instantaneously vaporized when contacting high temperature, and is cracked, depolymerized and polymerized into nano alumina particles.
It is further preferred that the jet velocity of the high purity aluminum sol in the high temperature plasma reactor is 300 to 500g/min.
As a preferable technical scheme of the invention, the specific steps in the steps (3) and (4) are as follows:
the nano alumina particles generated in the reaction cavity of the high-temperature plasma reactor rapidly fall, are cooled by a quenching system to avoid aggregation of nano particles, reduce aggregation, and finally pass through a grading collection system to prepare the gas-phase nano alumina.
Preferably, the temperature of the plasma flame flow in the high-temperature plasma reactor is adjustable at 1500-2500 ℃, the reaction time is lower than 1s, and the power of the high-temperature plasma reactor is adjustable at 50-85 kW.
Preferably, the flow rate of the plasma excitation gas of the high temperature plasma reactor is 100 to 200sccm.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention realizes the preparation of the high-purity alumina nano powder, has the advantages of simple process, low cost, high product purity and the like, can be used for large-scale production, and can obviously reduce the reaction temperature and the production energy consumption.
2) In a plasma reaction system, the reaction is finished instantly and can reach millisecond level, and the prepared product has small particle size and no hard agglomeration, which has a critical influence on the formation of low-particle-size nano powder.
3) The alumina prepared by the invention is in the form of spherical particles with the diameter of 10-50 nm, has no aggregation and is in a monodisperse form.
4) The invention abandons the defect of feeding the traditional powder material, firstly proposes that the alumina sol is fed into the reaction chamber in a spray mode by using the pump, the uniform reaction can be realized, the effective control of the particle size can be realized by controlling the feeding flow, and the preparation of the monodisperse form of the alumina nano powder is facilitated.
Drawings
FIG. 1 is an SEM image of crude alumina sol (a) and high purity alumina sol (b).
Figure 2 is an XRD pattern of the product prepared in example 1.
Fig. 3 is an SEM image of the product prepared in example 1.
FIG. 4 is an SEM image of the product of comparative example (a corresponds to a jet velocity of 100g/min, and b corresponds to a jet velocity of 1500 g/min).
Detailed Description
The invention provides a preparation method of nanometer alumina by a gas phase method, and the method of the invention is further described in detail below by using examples and drawings.
Example 1
The preparation process of nanometer alumina in gas phase includes the following steps:
(1) and purifying the crude product of the alumina sol to prepare the high-purity alumina sol.
(1) Evaporating the crude aluminum sol slurry under the condition of vacuum heating until the water content reaches 25%, and cooling to room temperature.
(2) And adding absolute ethyl alcohol into the slurry, uniformly dispersing by ultrasonic, then adding a silane coupling agent KH550, heating to 55 ℃ and stirring for 2h. The adding weight ratio of the slurry to the absolute ethyl alcohol to the silane coupling agent KH550 is 1:2:0.5.
(3) Evaporating again under vacuum heating until the water-ethanol content reaches 10%, and cooling to room temperature to obtain high-purity aluminum sol.
As can be seen from FIG. 1, the crude product of the aluminum sol is a cotton-like aggregate, and the morphology is unevenly distributed. The high-purity aluminum sol prepared by purification treatment is obviously more uniformly distributed and has high uniformity of appearance.
(2) Spraying the mixture into a high-temperature plasma reactor by adopting a high-pressure spraying method to instantaneously react to prepare the nano alumina.
The high-pressure spraying method is adopted, high-purity alumina sol is sprayed into a reaction cavity of a high-temperature plasma reactor by a pump, plasma excitation gas of the high-temperature plasma reactor is nitrogen or argon, and the alumina sol is instantaneously vaporized when contacting high temperature, and is cracked, depolymerized and polymerized into nano alumina particles.
Wherein the temperature of the plasma flame flow in the high-temperature plasma reactor is 2000 ℃, the reaction time is lower than 1s, and the jet flow speed of the high-purity aluminum sol is 400g/min.
(3) Cooling the quenching system and collecting by a grading collecting system.
The nano alumina particles generated in the reaction cavity of the high-temperature plasma reactor rapidly fall, are cooled by a quenching system to avoid aggregation of nano particles, reduce aggregation, and finally pass through a grading collection system to prepare the gas-phase nano alumina.
Fig. 2 is an SEM image of the product prepared in example 1, and fig. 3 is an SEM image of the product prepared in example 1. As can be seen from the figure, the prepared alumina is in the form of dispersed nearly spherical particles, the diameter of the alumina is 20-50 nm, and the alumina is nearly spherical and has no hard agglomeration. The product produced was found to be alumina when compared to a standard PDF card (46-1131) in conjunction with the XRD pattern shown in fig. 2. Through detection, the purity of the prepared nano alumina powder reaches more than 99.9 percent.
Comparative examples
The preparation method is similar to that of example 1, except that the jet flow rate of the high-purity alumina sol is adjusted to be 100g/min and 1500g/min respectively.
As can be seen from FIG. 4, with the change of the jet flow rate, the morphology of the prepared product is greatly affected, and particularly as shown in FIG. 4b, when the jet flow rate is too high, the agglomeration phenomenon of the prepared product is serious, and the alumina in a monodisperse form cannot be prepared.
Example 2
The preparation process of nanometer alumina in gas phase includes the following steps:
(1) and purifying the crude product of the alumina sol to prepare the high-purity alumina sol.
(1) Evaporating the crude aluminum sol slurry under the condition of vacuum heating until the water content reaches 30%, and cooling to room temperature.
(2) And adding absolute ethyl alcohol into the slurry, uniformly dispersing by ultrasonic, then adding a silane coupling agent KH550, heating to 55 ℃ and stirring for 3h. The adding weight ratio of the slurry to the absolute ethyl alcohol to the silane coupling agent KH550 is 1:2.5:0.4.
(3) Evaporating again under vacuum heating until the water-ethanol content reaches 8%, and cooling to room temperature to obtain high-purity aluminum sol.
(2) Spraying the mixture into a high-temperature plasma reactor by adopting a high-pressure spraying method to instantaneously react to prepare the nano alumina.
The high-pressure spraying method is adopted, high-purity alumina sol is sprayed into a reaction cavity of a high-temperature plasma reactor by a pump, plasma excitation gas of the high-temperature plasma reactor is nitrogen or argon, and the alumina sol is instantaneously vaporized when contacting high temperature, and is cracked, depolymerized and polymerized into nano alumina particles.
Wherein the plasma flame flow temperature in the high-temperature plasma reactor is 1800 ℃, the reaction time is lower than 1s, and the jet flow speed of the high-purity aluminum sol is 350g/min.
(3) Cooling the quenching system and collecting by a grading collecting system.
The nano alumina particles generated in the reaction cavity of the high-temperature plasma reactor rapidly fall, are cooled by a quenching system to avoid aggregation of nano particles, reduce aggregation, and finally pass through a grading collection system to prepare the gas-phase nano alumina.
Example 3
The preparation process of nanometer alumina in gas phase includes the following steps:
(1) and purifying the crude product of the alumina sol to prepare the high-purity alumina sol.
(1) Evaporating the crude aluminum sol slurry under the condition of vacuum heating until the water content reaches 20%, and cooling to room temperature.
(2) And adding absolute ethyl alcohol into the slurry, uniformly dispersing by ultrasonic, then adding a silane coupling agent KH550, heating to 60 ℃ and stirring for 2 hours. The adding weight ratio of the slurry to the absolute ethyl alcohol to the silane coupling agent KH550 is 1:2:0.6.
(3) Evaporating again under vacuum heating until the water-ethanol content reaches 5%, and cooling to room temperature to obtain high-purity aluminum sol.
(2) Spraying the mixture into a high-temperature plasma reactor by adopting a high-pressure spraying method to instantaneously react to prepare the nano alumina.
The high-pressure spraying method is adopted, high-purity alumina sol is sprayed into a reaction cavity of a high-temperature plasma reactor by a pump, plasma excitation gas of the high-temperature plasma reactor is nitrogen or argon, and the alumina sol is instantaneously vaporized when contacting high temperature, and is cracked, depolymerized and polymerized into nano alumina particles.
Wherein, the temperature of the plasma flame flow in the high-temperature plasma reactor is 2200 ℃ and adjustable, the reaction time is lower than 1s, and the jet flow speed of the high-purity aluminum sol is 450g/min.
(3) Cooling the quenching system and collecting by a grading collecting system.
The nano alumina particles generated in the reaction cavity of the high-temperature plasma reactor rapidly fall, are cooled by a quenching system to avoid aggregation of nano particles, reduce aggregation, and finally pass through a grading collection system to prepare the gas-phase nano alumina.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (1)
1. The preparation method of the gas phase nanometer alumina is characterized by comprising the following steps:
(1) purifying the crude product of the aluminum sol to prepare high-purity aluminum sol:
evaporating the crude aluminum sol slurry under the condition of vacuum heating until the water content reaches 15-30%, and cooling to room temperature; adding absolute ethyl alcohol into the slurry, uniformly dispersing by ultrasonic, then adding a silane coupling agent KH550, heating to 50-60 ℃ and stirring for 1-3 h; the adding weight ratio of the slurry to the absolute ethyl alcohol to the silane coupling agent KH550 is 1:1.5 to 2.5:0.3 to 0.6; evaporating under vacuum heating until the water-ethanol content reaches 5-10%, and cooling to room temperature to obtain high-purity aluminum sol;
(2) spraying the nano alumina into a high-temperature plasma reactor by adopting a high-pressure spraying method for instantaneous reaction to prepare nano alumina:
spraying high-purity aluminum sol into a reaction cavity of a high-temperature plasma reactor by using a pump, wherein plasma excitation gas of the high-temperature plasma reactor is nitrogen or argon, and the aluminum sol is instantaneously vaporized when contacting high temperature, and is cracked, depolymerized and polymerized into monodisperse nano aluminum oxide particles;
the jet flow speed of the high-purity aluminum sol in the high-temperature plasma reactor is 300-500 g/min, the plasma flame flow temperature in the high-temperature plasma reactor is 1500-2500 ℃, the reaction time is lower than 1s, the power of the reactor is 50-120 kW, and the flow rate of plasma excitation gas is 100-200 sccm;
(3) cooling the quenching system and grading the collecting system to prepare the gas phase nanometer alumina:
monodisperse nano alumina particles generated in a reaction cavity of a high-temperature plasma reactor rapidly fall, are cooled by a quenching system to avoid nanoparticle aggregation, reduce agglomeration, and finally are prepared by a grading collection system to obtain gas-phase nano alumina;
the prepared gas phase nanometer alumina is in spherical particle form, the diameter of the nanometer alumina is 10-50 nm, aggregation is avoided, and the nanometer alumina is in monodisperse form.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531009A (en) * | 2010-12-28 | 2012-07-04 | 上海华明高技术（集团）有限公司 | Nanoscale high-purity aluminum oxide preparation method |
| CN103043692A (en) * | 2012-12-27 | 2013-04-17 | 西安迈克森新材料有限公司 | Preparation method for high-purity aluminum oxide powder material |
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