CN111170345A - preparation method of nano α phase aluminum oxide material - Google Patents
preparation method of nano α phase aluminum oxide material Download PDFInfo
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- CN111170345A CN111170345A CN202010042490.7A CN202010042490A CN111170345A CN 111170345 A CN111170345 A CN 111170345A CN 202010042490 A CN202010042490 A CN 202010042490A CN 111170345 A CN111170345 A CN 111170345A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
- C01F7/023—Grinding, deagglomeration or disintegration
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- B82—NANOTECHNOLOGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
the invention discloses a preparation method of a nanometer α phase alumina material, which comprises the following steps of S1 weighing an alumina raw material and performing sanding operation to obtain nano alumina, S2 rapidly heating to 1200 ℃ in a roasting furnace, keeping the temperature for 5-15 min, and then rapidly cooling to obtain alumina powder containing alpha-phase alumina microcrystals, S3 re-heating to 850-950 ℃, keeping the temperature constant in the temperature range for 2-6 h, and then cooling to obtain alpha-phase alumina with the conversion rate of more than 90%, and S4 dispersing the alpha-phase alumina in carrier liquid to obtain alpha-phase alumina suspension, crushing the alpha-phase alumina suspension under the high-speed collision condition through high-speed collision equipment, repeatedly circulating for many times, and preparing the ultra-pure nanometer α phase alumina in batches.
Description
Technical Field
the invention relates to the technical field of nano material preparation, in particular to a preparation method of an ultra-pure nano α phase alumina material.
Background
the α phase alumina has low specific surface, high temperature resistance, high heat resistance, stable crystal phase, high hardness and high size stability, and may be used widely in reinforcing and toughening various plastic, rubber, ceramic, refractory material and other products, especially in raising the compactness, smoothness, cold and hot fatigue, fracture toughness and creep resistance of ceramic and in raising the wear resistance of polymer material.
the existing preparation method of the nano alpha-phase aluminum oxide material generally adopts Al (OH)3the method has the advantages of strong corrosion to equipment, low crystal form conversion efficiency and incapability of preparing the nano α -phase alumina material in batches, reduces the production cost and the pollution to the environment in the production process, and realizes the green preparation of the ultra-pure nano α -phase alumina powder, which is the key for further wide application of the nano powder.
Disclosure of Invention
in view of the defects of the prior art, the invention provides the preparation method of the nanometer α phase alumina material, which does not introduce any process impurity, has green and environment-friendly preparation process and is particularly suitable for batch production and preparation of ultra-pure nanometer α phase alumina.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a preparation method of a nano α phase alumina material comprises the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 5-15 min, and then rapidly cooling to obtain alumina powder containing α -phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 850-950 ℃, keeping the temperature constant in the temperature range for 2-6 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
The alumina raw material is gamma-phase alumina or theta-phase alumina.
In the step S2, the rapid temperature-raising rate is set to 10-15 ℃/min, and the rapid temperature-lowering rate is set to 10-15 ℃/min.
in the step S2, the content of α phase alumina crystallites in the alumina powder is 0.1 to 0.5 wt%.
In the step S3, the temperature rising rate is set to 5-12 ℃/min, and the temperature lowering rate is set to 15-20 ℃/min.
In step S4, the carrier liquid is at least one of water, ethanol, and ethylene glycol.
More preferably, the carrier fluid is a mixed solution obtained by mixing at least one of water, ethanol and ethylene glycol with calixarene, and the mass ratio of the carrier fluid to the calixarene is 6-18: 1. the lower edge of the calixarene is modified with hydroxyl, and the upper edge of the calixarene is modified with a long-chain alkane group of C6-C10.
The calixarene has the characteristic of forming a host-guest inclusion complex with ions and neutral molecules, the modified group has strong water compatibility, and is beneficial to improving the uniform dispersion of solid particles in suspension, and the calixarene can be easily separated from the prepared nano particles under the action of high pressure due to good thermal stability and chemical stability, so that the purity of the nano material is further improved.
the particle size of the nanometer α phase alumina is 20-50 nm.
The high-speed collision device includes:
the first liquid storage tank is used for storing the prepared suspension liquid;
the inlet of the pressure pump is connected to the first liquid storage tank, and is used for pressurizing the suspension liquid to a high-pressure state and distributing the suspension liquid to the first high-pressure liquid tank and the second high-pressure liquid tank, and the first high-pressure liquid tank and the second high-pressure liquid tank are respectively connected with the inlet ends of the first nozzle and the second nozzle;
the reaction kettle is used for carrying out high-speed collision on the suspension in the reaction kettle, and the first nozzle and the second nozzle extend to the upper part of the inner cavity of the reaction kettle and are arranged oppositely;
and the second liquid storage tank is connected to the lower part of the inner cavity of the reaction kettle and is used for storing the nano material prepared after collision is finished.
The pressure of the liquid cavities in the first high-pressure liquid tank and the second high-pressure liquid tank is required to be more than 100 Mpa.
The spraying speed of the fluid in the first nozzle and the second nozzle is 20-40 m/s.
The invention has the beneficial effects that:
the preparation method of the nanometer α phase alumina material does not introduce any process impurities, has green and environment-friendly preparation process, is particularly suitable for batch production and preparation of the nanometer α phase alumina, and the purity of the prepared nano material reaches more than 99.99 percent.
Drawings
FIG. 1 is a schematic view of a high speed collision device in an embodiment of the present invention;
the device comprises a first liquid storage tank 1, a pressure pump 2, a first high-pressure liquid tank 3, a second high-pressure liquid tank 4, a reaction kettle 5, a second liquid storage tank 6, a first nozzle 31 and a second nozzle 41.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1
the preparation method of the nano α phase alumina material comprises the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 10min, and then rapidly cooling to obtain alumina powder containing α phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 900 ℃ again, keeping the temperature constant in the temperature range for 4 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
The raw material of the alumina is gamma-phase alumina.
In step S2, the rate of rapid temperature increase is set to 12 ℃/min, and the rate of rapid temperature decrease is set to 12 ℃/min.
in the step S2, the content of α -phase alumina crystallites in the alumina powder is 0.3 wt%.
In step S3, the temperature increase rate is set to 8 ℃/min and the temperature decrease rate is set to 18 ℃/min.
In step S4, the carrier liquid is water.
the particle size of the nanometer α phase alumina is 40 nm.
As shown in fig. 1, the high-speed collision device includes:
a first liquid storage tank 1 for storing the prepared suspension;
the inlet of the pressure pump 2 is connected to the first liquid storage tank 1, so that the suspension is pressurized to a high-pressure state and is divided into a first high-pressure liquid tank 3 and a second high-pressure liquid tank 4, and the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 are respectively connected with the inlet ends of the first nozzle 31 and the second nozzle 41;
the reaction kettle 5 is used for carrying out high-speed collision on the suspension in the reaction kettle 5, and the first nozzle 31 and the second nozzle 41 extend to the upper part of the inner cavity of the reaction kettle 5 and are oppositely arranged;
and the second liquid storage tank 6 is connected to the lower part of the inner cavity of the reaction kettle 5 and is used for storing the nano material prepared after collision is finished.
The pressure of the liquid chambers in the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 is 110 Mpa.
The fluid ejection speed in the first nozzle 31 and the second nozzle 41 is 30 m/s.
The purity of the prepared nano material reaches 99.990%.
Example 2
the preparation method of the nano α phase alumina material comprises the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 5min, and then rapidly cooling to obtain alumina powder containing α phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 850 ℃, keeping the temperature constant in the temperature range for 6 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
The alumina raw material is theta-phase alumina.
In step S2, the rate of rapid temperature increase is set to 10 ℃/min, and the rate of rapid temperature decrease is set to 15 ℃/min.
in the step S2, the content of α -phase alumina crystallites in the alumina powder is 0.1 wt%.
In step S3, the temperature increase rate is set to 5 ℃/min and the temperature decrease rate is set to 15 ℃/min.
In step S4, the carrier liquid is ethanol.
the particle size of the nanometer α phase alumina is 20 nm.
As shown in fig. 1, the high-speed collision device includes:
a first liquid storage tank 1 for storing the prepared suspension;
the inlet of the pressure pump 2 is connected to the first liquid storage tank 1, so that the suspension is pressurized to a high-pressure state and is divided into a first high-pressure liquid tank 3 and a second high-pressure liquid tank 4, and the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 are respectively connected with the inlet ends of the first nozzle 31 and the second nozzle 41;
the reaction kettle 5 is used for carrying out high-speed collision on the suspension in the reaction kettle 5, and the first nozzle 31 and the second nozzle 41 extend to the upper part of the inner cavity of the reaction kettle 5 and are oppositely arranged;
and the second liquid storage tank 6 is connected to the lower part of the inner cavity of the reaction kettle 5 and is used for storing the nano material prepared after collision is finished.
The pressure of the liquid chambers in the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 is 100 Mpa.
The fluid ejection speed in the first nozzle 31 and the second nozzle 41 is 20 m/s.
The purity of the prepared nano material reaches 99.988%.
Example 3
the preparation method of the nano α phase alumina material comprises the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 15min, and then rapidly cooling to obtain alumina powder containing α phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 950 ℃ again, keeping the temperature constant in the temperature range for 6 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
The raw material of the alumina is gamma-phase alumina.
In step S2, the rate of rapid temperature increase is set to 15 ℃/min, and the rate of rapid temperature decrease is set to 15 ℃/min.
in the step S2, the content of α -phase alumina crystallites in the alumina powder is 0.5 wt%.
In step S3, the temperature increase rate is set to 12 ℃/min and the temperature decrease rate is set to 20 ℃/min.
In step S4, the carrier liquid is ethylene glycol.
the particle size of the nanometer α phase alumina is 50 nm.
As shown in fig. 1, the high-speed collision device includes:
a first liquid storage tank 1 for storing the prepared suspension;
the inlet of the pressure pump 2 is connected to the first liquid storage tank 1, so that the suspension is pressurized to a high-pressure state and is divided into a first high-pressure liquid tank 3 and a second high-pressure liquid tank 4, and the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 are respectively connected with the inlet ends of the first nozzle 31 and the second nozzle 41;
the reaction kettle 5 is used for carrying out high-speed collision on the suspension in the reaction kettle 5, and the first nozzle 31 and the second nozzle 41 extend to the upper part of the inner cavity of the reaction kettle 5 and are oppositely arranged;
and the second liquid storage tank 6 is connected to the lower part of the inner cavity of the reaction kettle 5 and is used for storing the nano material prepared after collision is finished.
The pressure of the liquid chambers in the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 is 120 Mpa.
The fluid velocity in the first nozzle 31 and the second nozzle 41 was 40 m/s.
The purity of the prepared nano material reaches 99.991%.
Example 4
the preparation method of the nano α phase alumina material comprises the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 5min, and then rapidly cooling to obtain alumina powder containing α phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 850 ℃, keeping the temperature constant in the temperature range for 2 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
The raw material of the alumina is gamma-phase alumina.
In step S2, the rate of rapid temperature increase is set to 15 ℃/min, and the rate of rapid temperature decrease is set to 15 ℃/min.
in the step S2, the content of α -phase alumina crystallites in the alumina powder is 0.1 wt%.
In step S3, the temperature increase rate is set to 7 ℃/min and the temperature decrease rate is set to 20 ℃/min.
In step S4, the carrier liquid is a mixed solution obtained by mixing ethanol and calixarene, and the mass ratio of the two is 8: 1.
the particle size of the nanometer α phase alumina is 40 nm.
As shown in fig. 1, the high-speed collision device includes:
a first liquid storage tank 1 for storing the prepared suspension;
the inlet of the pressure pump 2 is connected to the first liquid storage tank 1, so that the suspension is pressurized to a high-pressure state and is divided into a first high-pressure liquid tank 3 and a second high-pressure liquid tank 4, and the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 are respectively connected with the inlet ends of the first nozzle 31 and the second nozzle 41;
the reaction kettle 5 is used for carrying out high-speed collision on the suspension in the reaction kettle 5, and the first nozzle 31 and the second nozzle 41 extend to the upper part of the inner cavity of the reaction kettle 5 and are oppositely arranged;
and the second liquid storage tank 6 is connected to the lower part of the inner cavity of the reaction kettle 5 and is used for storing the nano material prepared after collision is finished.
The pressure of the liquid cavities in the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 is 110 Mpa.
The fluid ejection speed in the first nozzle 31 and the second nozzle 41 is 30 m/s.
The purity of the prepared nano material reaches 99.998%.
Example 5
the preparation method of the nano α phase alumina material comprises the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 15min, and then rapidly cooling to obtain alumina powder containing α phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 950 ℃ again, keeping the temperature constant in the temperature range for 6 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
The alumina raw material is theta-phase alumina.
In step S2, the rate of rapid temperature increase is set to 10 ℃/min, and the rate of rapid temperature decrease is set to 15 ℃/min.
in the step S2, the content of α -phase alumina crystallites in the alumina powder is 0.2 wt%.
In step S3, the temperature increase rate is set to 10 ℃/min and the temperature decrease rate is set to 16 ℃/min.
In step S4, the carrier liquid is a mixed solution obtained by mixing water and calixarene, and the mass ratio of the two is 15: 1.
the particle size of the nanometer α phase alumina is 20 nm.
As shown in fig. 1, the high-speed collision device includes:
a first liquid storage tank 1 for storing the prepared suspension;
the inlet of the pressure pump 2 is connected to the first liquid storage tank 1, so that the suspension is pressurized to a high-pressure state and is divided into a first high-pressure liquid tank 3 and a second high-pressure liquid tank 4, and the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 are respectively connected with the inlet ends of the first nozzle 31 and the second nozzle 41;
the reaction kettle 5 is used for carrying out high-speed collision on the suspension in the reaction kettle 5, and the first nozzle 31 and the second nozzle 41 extend to the upper part of the inner cavity of the reaction kettle 5 and are oppositely arranged;
and the second liquid storage tank 6 is connected to the lower part of the inner cavity of the reaction kettle 5 and is used for storing the nano material prepared after collision is finished.
The pressure of the liquid chambers in the first high-pressure liquid tank 3 and the second high-pressure liquid tank 4 is 100 Mpa.
The fluid ejection speed in the first nozzle 31 and the second nozzle 41 is 20 m/s.
The purity of the prepared nano material reaches 99.999 percent.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a nano α -phase alumina material is characterized by comprising the following steps:
s1: weighing an alumina raw material, and performing sanding operation to obtain nano alumina;
s2, rapidly heating the nano-alumina obtained in the step S1 to 1200 ℃ in a roasting furnace, keeping the temperature for 5-15 min, and then rapidly cooling to obtain alumina powder containing α -phase alumina microcrystals;
s3, heating the alumina powder containing the α -phase alumina microcrystal obtained in the step S2 to 850-950 ℃, keeping the temperature constant in the temperature range for 2-6 hours, and then cooling to obtain α -phase alumina with the conversion rate of more than 90%;
and S4, dispersing the α -phase alumina obtained in the step S3 in carrier liquid to obtain α -phase alumina suspension, crushing the α -phase alumina suspension under a high-speed collision condition through high-speed collision equipment, and repeatedly circulating for many times to prepare the ultrahigh-purity nano α -phase alumina in batches.
2. the method of preparing a nano α -phase alumina material according to claim 1, wherein the alumina raw material is γ -phase alumina or θ -phase alumina.
3. the method of preparing a nano α -phase alumina material according to claim 1, wherein in the step S2, the rapid temperature increase rate is set to 10 to 15 ℃/min and the rapid temperature decrease rate is set to 10 to 15 ℃/min.
4. the method of preparing a nano α -phase alumina material according to claim 1, wherein in the step S2, the α -phase alumina fine powder contains 0.1 to 0.5wt% of the α -phase alumina fine crystals.
5. the method of preparing a nano α -phase alumina material according to claim 1, wherein in the step S3, the temperature rising rate is set to 5 to 12 ℃/min and the temperature lowering rate is set to 15 to 20 ℃/min.
6. the method of manufacturing a nano α -phase alumina material according to claim 1, wherein in the step S4, the carrier liquid is at least one of water, ethanol, and ethylene glycol.
7. the method of preparing a nano α -phase alumina material according to claim 1, wherein the nano α -phase alumina has a particle size of 20 to 50 nm.
8. the method of preparing a nano α phase alumina material according to claim 1, wherein the high speed collision device comprises:
the first liquid storage tank is used for storing the prepared suspension liquid;
the inlet of the pressure pump is connected to the first liquid storage tank, and is used for pressurizing the suspension liquid to a high-pressure state and distributing the suspension liquid to the first high-pressure liquid tank and the second high-pressure liquid tank, and the first high-pressure liquid tank and the second high-pressure liquid tank are respectively connected with the inlet ends of the first nozzle and the second nozzle;
the reaction kettle is used for carrying out high-speed collision on the suspension in the reaction kettle, and the first nozzle and the second nozzle extend to the upper part of the inner cavity of the reaction kettle and are arranged oppositely;
and the second liquid storage tank is connected to the lower part of the inner cavity of the reaction kettle and is used for storing the nano material prepared after collision is finished.
9. the method for preparing nano alpha-phase alumina material according to claim 8, wherein the pressure requirement of the liquid chambers in the first high-pressure liquid tank and the second high-pressure liquid tank is more than 100 Mpa.
10. the method for preparing a nano α phase alumina material according to claim 8, wherein the fluid spraying speed in the first nozzle and the second nozzle is 20 to 40 m/s.
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| CN103816970A (en) * | 2014-01-27 | 2014-05-28 | 上海应用技术学院 | Preparing device and preparing method for liquid nano solution |
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| CN105540574A (en) * | 2016-01-28 | 2016-05-04 | 成都新柯力化工科技有限公司 | Method for preparing graphene micro-sheets by using counter-jet jet mill |
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