CN1565973A - Process for preparing high purity superfine Al2O3 powder - Google Patents
Process for preparing high purity superfine Al2O3 powder Download PDFInfo
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- CN1565973A CN1565973A CN 03148830 CN03148830A CN1565973A CN 1565973 A CN1565973 A CN 1565973A CN 03148830 CN03148830 CN 03148830 CN 03148830 A CN03148830 A CN 03148830A CN 1565973 A CN1565973 A CN 1565973A
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Abstract
The invention discloses a process for preparing high purity superfine aluminium oxide powder which comprises the steps of, (1) mixing aluminum powder and water by a finite proportion, charging in a purpose made ball grinder for grinding, (2) taking out the prepared aluminum hydroxide from the ball-grinding tank, proceeding dewatering dehydration and phase inversion.
Description
Technical Field
The invention relates to a method for preparing high-purity oxide powder by a mechanical ball milling method, in particular to a method for preparing high-purity superfine Al by a mechanical ball milling method2O3And (3) powder.
Background
The high-purity ultrafine alumina powder exhibits excellent properties that conventional alumina materials do not have due to its high purity and small particle size. Currently, the current practice is. As one of the advanced materials, it has been widely used in many fields such as optics, chemical engineering, and special ceramics, for example: three-primary-color fluorescent powder, a high-pressure sodium lamp tube, a catalyst carrier, a high-efficiency grinding material, an artificial joint and the like. Due to the rapid development of modern science and technology, the demand for high-purity ultrafine alumina powder materials is rapidly increasing.
The preparation of the high-purity ultrafine alumina powder mainly adopts a sol-gel method, an ammonium aluminum sulfate pyrolysis method, an ammonium aluminum carbonate pyrolysis method, an aluminum isopropoxide hydrolysis method, a mercury chloride activation hydrolysis method, a plasma method, a hydrothermal method, an improved Bayer method, an active high-purity aluminum powder direct hydrolysis method and the like, and the methods have advantages and disadvantages. At present, the domestic large-scale production mainly adopts an ammonium aluminum carbonate pyrolysis method, an aluminum isopropoxide hydrolysis method and an active high-purity aluminum powder direct hydrolysis method. The existing publications report that metal oxide is mixed and then ball-milled to obtain a metal oxide mixture, or elemental metal powder is ball-milled to obtain elemental metal powder, and no report that the elemental metal is ball-milled and hydrolyzed to obtain metal oxide powder is provided, and a hydrolysis reaction is accompanied. Aluminum generally has high activity, and the aluminum in an active state can generate hydrolysis reaction when meeting water. In the conventional powder preparation process, an oxide film is quickly formed due to the oxidation of the surface of the powder to passivate the powder, and the surface layer of the passivated aluminum powder cannot be hydrolyzed under the protection of the oxide film.
Disclosure of Invention
The invention provides a novel method for preparing a high-purity superfine alumina powder material, which can overcome the problem of an oxide film on the surface layer of the aluminum powder.
The method comprises the following specific process steps: (1) mixing aluminum powder and water according to a certain proportion, and then putting the mixture into a ball mill for ball milling; (2) and taking the prepared aluminum hydroxide out of the ball milling tank, and carrying out dehydration drying and phase inversion treatment. The aluminum powder has the purity of 99.9-99.999% and the granularity of-100 meshes. The weight ratio of the aluminum powder to the water is 1: 2, namely Al: H2O is 1: 2. The ball mill is provided with an exhaust pipeline and a heat-insulating interlayer, and hot water at about 90 ℃ is introduced into the heat-insulating interlayer in the reaction process. The ball mill has ball milling tank lining and ZrO for ball2、Al2O3The material is made of (corundum) ceramic materials or other wear-resistant and high-temperature-resistant organic materials, and the purity of the material is equivalent to that of a final product. The invention can also be prepared by selecting raw materials with different purities, different preparation process conditions and different phase inversion temperatures, and a series of high-purity superfine Al with different purities, different particle sizes and different phase states can be obtained2O3And (3) powder.
The purity of the lining material used in the invention is different according to different purity requirements of the manufactured products. The lining material is generally required to be of the same purity as the final product, and the spheres are made of the same material, so that more impurities are prevented from being brought in during the ball milling process.
The method adopts common aluminum powder as raw material and prepares high-purity superfine Al by common ball milling or high-energy ball milling technology2O3And (3) powder. The principle is as follows: due to the action of mechanical ball milling, an oxide film on the surface of the powder can be firstly damaged, meanwhile, due to the action of mechanical ball milling, the crystal lattice of the powder is distorted and a plurality of defects are caused, so that the powder is in a high-energy state, and the powder in the high-energy state can be subjected to hydrolysis reaction when meeting water. This is actually due to a mechanical force-induced chemical reaction, commonly referred to as a mechanochemical reaction.
The invention skillfully applies a mechanical ball milling method, namely a chemical reaction triggered by mechanical force, so that aluminum powder is prepared during the ball milling processThe oxide film on the surface is continuously destroyed, so that the fresh metal aluminum surface is exposed to be contacted with water, meanwhile, the surface energy and the internal energy of the powder are increased in the ball milling process, the hydrolysis reaction of the activated aluminum in water is initiated, and the reaction equation is as follows:
the surface layer of the metal particles is continuously stripped along with the progress of the hydrolysis reaction, the particles are continuously refined and are accompanied with a large amount of hydrogen gas to be discharged, and the final product of the hydrolysis reaction is nano-scale metal hydrate primary particles, namely, the mixture of high-purity and superfine aluminum hydroxide Al (OH) and boehmite AlO (OH) is obtained as a result of the hydrolysis reaction. The high-purity superfine Al with different phase states can be obtained by subsequent dehydration and phase inversion treatment2O3And (3) powder. The method is characterized in that the raw material is high-purity aluminum powder, the aluminum powder is activated by ball milling, and then the high-purity superfine Al with different phase states can be obtained by hydrolysis, drying and phase inversion treatment2O3And (3) powder. The process of preparing the powder has short flow, low cost and no pollution, and can be used for large-scale production. The invention has the advantages of obvious technical progress and outstanding substantive characteristics, and can generate good economic and social benefits.
EXAMPLE 1 preparation of α -Al for Artificial Crystal2O3Production of powder
High-purity aluminum powder with the purity of 99.999 percent is used as a raw material, a mixture of aluminum powder with the purity of-100 meshes and water is put into a special ball mill for ball milling through screening, hot water with the temperature of about 90 ℃ is filled into a heat-insulating interlayer of the ball mill, the aluminum powder and the water react in the ball milling process, hydrogen is discharged at the same time, the hydrolysis reaction of the aluminum powder can be completed after ball milling is carried out for about 24 hours, the ball milling is stopped, the temperature is reduced, then the reaction product is put into a centrifuge for dehydration, drying treatment is carried out at the temperature of below 200 ℃, phase inversion treatment is carried out at the temperature of 1200 and 1300 ℃, and α -Al with the purity of 99.995 percent and the average grain diameter of2O3And (3) powder.
EXAMPLE 2 α -Al for three primary colors phosphor2O3Production of powder
The purity of the alumina powder used for preparing the phosphor powder with three primary colors is required to be more than 99.99 percent, therefore, the purity of the selected-100-mesh aluminum powder is more than 99.995 percent, the ball milling reaction process is basically the same as that of the first embodiment, α -Al which is usually selected for preparing the phosphor powder with three primary colors is adopted2O3The average particle size of the powder is about 5 μm, and the narrower the particle size distribution, the better. Thus, thereaction product obtained is subjected toAfter dehydration, drying and phase inversion, the final α -Al with purity not less than 99.99% and average grain size of about 5 μm can be obtained by classification treatment2O3And (3) powder.
Example 3: Gamma-Al for catalyst carrier2O3Preparation of powder
The alumina powder used for the catalyst carrier has low requirements on purity and granularity, but needs to be active, so that the final product is gamma-Al2O3And (3) powder. During preparation, aluminum powder with the purity of 99.99 percent is selected as a raw material to carry out ball milling reaction, a reaction product is dehydrated and dried, and then phase inversion treatment is carried out at the temperature of 600-2O3And (3) powder. Final product gamma-Al2O3The purity of the powder can be controlled to be more than 99.9 percent. The average particle size is less than 10 μm.
Claims (6)
1. Preparation of high-purity superfine Al2O3Method for the production of a powder, characterised in that it comprises the following process steps: (1) mixing aluminum powder and water according to a certain proportion, and then putting the mixture into a ball mill for ball milling; (2) and taking the prepared aluminum hydroxide out of the ball milling tank, and carrying out dehydration drying and phase inversion treatment.
2. The method of claim 1 for preparing high purity ultra fine Al2O3A method of powdering, characterized by: the aluminum powder has the purity of 99.9-99.999% and the granularity of-100 meshes.
3. The method of claim 1 for preparing a high purity ultra-fineFine Al2O3A method of powdering, characterized by: the weight ratio of the aluminum powder to the water is 1: 2, namely Al: H2O＝1∶2。
4. The method of claim 1 for preparing high purity ultra fine Al2O3A method of powdering, characterized by: the ball mill is provided with an exhaust pipeline and a heat-insulating interlayer, and hot water at about 90 ℃ is introduced into the heat-insulating interlayer in the reaction process.
5. The method of preparing high purity ultra fine Al according to claims 1 to 42O3A method of powdering, characterized by: the ball mill has ball milling tank lining and ZrO for ball2、Al2O3The material is made of (corundum) ceramic materials or other wear-resistant and high-temperature-resistant organic materials, and the purity of the material is equivalent to that of a final product.
6. Preparation of high-purity superfine Al2O3A method of powdering, characterized by: by selecting raw materials with different purities, different preparation process conditions and different phase inversion temperatures, a series of high-purity superfine Al with different purities, different particle sizes and different phase states can be obtained2O3And (3) powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03148830 CN1286724C (en) | 2003-06-13 | 2003-06-13 | Process for preparing high purity superfine Al2O3 powder |
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| CN 03148830 CN1286724C (en) | 2003-06-13 | 2003-06-13 | Process for preparing high purity superfine Al2O3 powder |
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| CN1565973A true CN1565973A (en) | 2005-01-19 |
| CN1286724C CN1286724C (en) | 2006-11-29 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008100903A (en) * | 2006-09-19 | 2008-05-01 | Sumitomo Chemical Co Ltd | Alpha-alumina powder |
| CN101829607A (en) * | 2010-05-17 | 2010-09-15 | 昆明珀玺金属材料有限公司 | Method for preparing catalyst carrier Al2O3 powder by activating and hydrolyzing metallic aluminium under ultrasound-electric field coupling |
| CN102190324A (en) * | 2010-03-09 | 2011-09-21 | 住友化学株式会社 | Alph alumina for the production of sapphire single crystal and method for producing the same |
| CN101516782B (en) * | 2006-09-19 | 2011-11-16 | 住友化学株式会社 | Alpha-alumina powder |
| CN102701248A (en) * | 2012-05-19 | 2012-10-03 | 鸿福晶体科技(安徽)有限公司 | Production process of high-purity aluminum oxide |
| CN103539178A (en) * | 2012-07-13 | 2014-01-29 | 蒋明学 | Production method of high-purity alumina |
| CN103606661A (en) * | 2013-11-11 | 2014-02-26 | 南京工业大学 | Method for synthesizing lithium ion battery cathode material by mechanochemical method |
| CN106573449A (en) * | 2014-08-14 | 2017-04-19 | 株式会社Lg化学 | Hydrophobic substrate and method for manufacturing same |
| CN108602686A (en) * | 2016-09-09 | 2018-09-28 | 住友化学株式会社 | Alumina powder, alumina slurry, the coating containing aluminium oxide, stacking seperation film and secondary cell |
| CN109092515A (en) * | 2018-07-26 | 2018-12-28 | 武汉科技大学 | A kind of high-purity corundum powder and preparation method thereof |
| CN109179466A (en) * | 2018-10-09 | 2019-01-11 | 湖南工业大学 | A kind of metallic aluminium prepares the method and production system of ultra-fine schmigel |
| CN115196658A (en) * | 2022-05-18 | 2022-10-18 | 陕西煤业化工技术研究院有限责任公司 | High-purity alumina powder prepared rapidly through autocatalysis and preparation method |
-
2003
- 2003-06-13 CN CN 03148830 patent/CN1286724C/en not_active Expired - Fee Related
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101516782B (en) * | 2006-09-19 | 2011-11-16 | 住友化学株式会社 | Alpha-alumina powder |
| US8163266B2 (en) | 2006-09-19 | 2012-04-24 | Sumitomo Chemical Company, Limited | Alpha-alumina powder |
| JP2008100903A (en) * | 2006-09-19 | 2008-05-01 | Sumitomo Chemical Co Ltd | Alpha-alumina powder |
| TWI415980B (en) * | 2006-09-19 | 2013-11-21 | Sumitomo Chemical Co | Α Aluminum oxide powder |
| CN102190324B (en) * | 2010-03-09 | 2014-11-19 | 住友化学株式会社 | Alph alumina for the production of sapphire single crystal and method for producing the same |
| CN102190324A (en) * | 2010-03-09 | 2011-09-21 | 住友化学株式会社 | Alph alumina for the production of sapphire single crystal and method for producing the same |
| CN101829607A (en) * | 2010-05-17 | 2010-09-15 | 昆明珀玺金属材料有限公司 | Method for preparing catalyst carrier Al2O3 powder by activating and hydrolyzing metallic aluminium under ultrasound-electric field coupling |
| CN102701248A (en) * | 2012-05-19 | 2012-10-03 | 鸿福晶体科技(安徽)有限公司 | Production process of high-purity aluminum oxide |
| CN102701248B (en) * | 2012-05-19 | 2013-12-25 | 鸿福晶体科技(安徽)有限公司 | Production process of high-purity aluminum oxide |
| CN103539178A (en) * | 2012-07-13 | 2014-01-29 | 蒋明学 | Production method of high-purity alumina |
| CN103606661A (en) * | 2013-11-11 | 2014-02-26 | 南京工业大学 | Method for synthesizing lithium ion battery cathode material by mechanochemical method |
| CN103606661B (en) * | 2013-11-11 | 2016-02-10 | 南京工业大学 | Method for synthesizing lithium ion battery cathode material by mechanochemical method |
| CN106573449A (en) * | 2014-08-14 | 2017-04-19 | 株式会社Lg化学 | Hydrophobic substrate and method for manufacturing same |
| US10763510B2 (en) | 2016-09-09 | 2020-09-01 | Sumitomo Chemical Company, Limited | Alumina powder, alumina slurry, alumina-containing coating layer, multilayer separation membrane and secondary battery |
| CN108602686A (en) * | 2016-09-09 | 2018-09-28 | 住友化学株式会社 | Alumina powder, alumina slurry, the coating containing aluminium oxide, stacking seperation film and secondary cell |
| CN109092515A (en) * | 2018-07-26 | 2018-12-28 | 武汉科技大学 | A kind of high-purity corundum powder and preparation method thereof |
| CN109092515B (en) * | 2018-07-26 | 2020-04-10 | 武汉科技大学 | High-purity corundum powder and preparation method thereof |
| CN109179466A (en) * | 2018-10-09 | 2019-01-11 | 湖南工业大学 | A kind of metallic aluminium prepares the method and production system of ultra-fine schmigel |
| CN109179466B (en) * | 2018-10-09 | 2021-09-28 | 湖南工业大学 | Method for preparing superfine corundum powder from metal aluminum |
| CN115196658A (en) * | 2022-05-18 | 2022-10-18 | 陕西煤业化工技术研究院有限责任公司 | High-purity alumina powder prepared rapidly through autocatalysis and preparation method |
| CN115196658B (en) * | 2022-05-18 | 2023-11-21 | 陕西煤业化工技术研究院有限责任公司 | High-purity alumina powder prepared rapidly through self-catalysis and method |
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| CN1286724C (en) | 2006-11-29 |
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