CN1919737A - Method of preparing good dispersion and high-purity ultra-fine alpha-Al2O3 - Google Patents
Method of preparing good dispersion and high-purity ultra-fine alpha-Al2O3 Download PDFInfo
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- CN1919737A CN1919737A CN 200510096756 CN200510096756A CN1919737A CN 1919737 A CN1919737 A CN 1919737A CN 200510096756 CN200510096756 CN 200510096756 CN 200510096756 A CN200510096756 A CN 200510096756A CN 1919737 A CN1919737 A CN 1919737A
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- aluminium
- ammonium
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Abstract
The invention discloses a preparing method of excellent dispersing high-pure ultra-fine alpha-Al2O3, which comprises the following steps: adopting analytic pure aluminium-alcohol salt hydrating reaction; balling; drying; sintering; adding one carboxyl acid or surface activator in the dehydrating course; adding alpha-Al2O3 seed and additive ammonium salt in the balling course.
Description
Technical field
That the present invention relates to is a kind of α-Al
2O
3The preparation method, particularly a kind of good dispersion, high-purity superfine alpha-Al
2O
3The preparation method.
Background technology
High-purity superfine alumina powder has demonstrated the light that conventional material did not have, electricity, magnetic, heat and mechanical characteristics because of its purity height, particle diameter are little, thereby it is widely used in a plurality of fields such as optics, chemical industry and special cermacis as a kind of new function material.But the Liquid preparation methods of usefulness is alumina powder jointed usually, needs at high temperature just can be converted into α-Al
2O
3, and presoma is easily reunited after high-temperature calcination, and specific area sharply descends, and average grain diameter sharply rises, and is difficult to make the high-quality superfine powder of good dispersion, therefore how to reduce alumina powder jointed phase inversion temperature, becomes the focus of people's research.The aluminium-alcohol salt preparing alumina by hydrolysis is a kind of in the liquid phase method, produces the focus that advantages such as aluminum oxide purity height, cost are lower become domestic and international research owing to it has.Chinese patent " the aluminium alcoholates hydrolysis method prepares the high-purity superfine alumina powder technology ", application number: 00105215.2, and Chinese patent " preparation method of high-purity nanoaluminium oxide ", application number: 01121545.3.The method of these two parts of patent disclosures implements more convenient, and can prepare high-purity grade of product, but hydrolysis of alkoxide forms hydrogen bond easily in this method production process, thereby produces hard aggregation, and the alumina precursor that generates needs at high temperature calcination just can be converted into α-Al
2O
3, hard aggregation also very easily takes place in the calcination process, be difficult to make the high-quality ultra-fine α-Al of good dispersion
2O
3Powder.This there are many researchs control the reunion of powder, Chinese patent " high purity super fine dispersing ball Al by the hydrolytic process of improving aluminium-alcohol salt
2O
3The preparation method of powder ", application number: 95111112.4, utilize steam to improve the dynamic conditions of aluminium-alcohol salt hydrolysis, make hydrolysis rate relatively low, thereby make the aluminium-hydroxide powder of dispersion, Japan Patent " continuous process for preparing aluminum hydroxide ", application number: 93119973.5, by shortening the time of aluminium-alcohol salt hydrolysis, and add the hydrolysising condition that a certain amount of additive improves aluminium-alcohol salt in hydrolytic process, thereby obtain evenly, the aluminium hydroxide that disperses, but the improvement of these technologies all is the improvement to the aluminium-alcohol salt hydrolytic process, ignored aluminium hydroxide and in the calcination process, equally hard aggregation can take place, and technology is relatively complicated.
Summary of the invention
The present invention seeks in hydrolytic process, to add carboxylic acid or surfactant, suppress the formation of hydrogen bond in the hydrolytic process, thereby obtain alumina precursor relatively more even, that disperse, in the calcination process, add and the mutually isomorphous α-Al of product simultaneously
2O
3Powder and organic or inorganic ammonium salt reduce in the calcination process θ to the mutually transformation activation energy of a phase, thus reduction α-Al
2O
3Phase inversion temperature, calcination just can obtain α-Al under lower temperature
2O
3Powder has overcome the hard aggregation that high temperature sintering causes, makes high-purity superfine alpha-Al that good dispersion, particle diameter are evenly distributed
2O
3Powder.
Technical process of the present invention as shown in Figure 1
Be achieved in that specifically the aluminium-alcohol salt that will analyze pure level is dissolved in the solvent of proper proportion, add a certain amount of additive, with the deionized water of certain speed adding behind solvent dilution, after being hydrolyzed, wearing out, filtering, obtain hydrolysate then, namely obtain alumina precursor.
In alumina precursor, add a certain amount of α-Al
2O
3As crystal seed and ammonium salt as additive, take deionized water or absolute alcohol as decentralized medium, the high purity aluminium oxide ball is as ball-milling medium, in high speed ball mill ball milling 3-12 hour, crystal seed and ammonium salt are evenly dispersed in the presoma, 200 mesh sieves were ground in oven dry at a certain temperature then, and powder in 1000-1100 ℃ of calcination, is obtained the α-Al of loose white
2O
3Powder.
In the present invention, alcohol is preferably low-carbon alcohol in the used aluminium-alcohol salt, and carbon number is that 2-4 is advisable, i.e. ethanol, Virahol and sec-butyl alcohol, and the solvent of using as hydrolysis is preferably the alcohol that constitutes aluminium-alcohol salt, so that the solvent recuperation during continuous production.
In the present invention, hydrolysis is elected 1: 1 to 6: 1 as with the mol ratio of deionized water and aluminium-alcohol salt, more preferably from about 2: 1 to 5: 1, when mol ratio during less than 1: 1, hydrolysis can not be fully, therefore a large amount of unreacted alkoxyl groups is retained in the alumina precursor of generation, productive rate descends, when mol ratio during greater than 6: 1, though hydrolysis is complete, but water concentration is too big in the slurry that reaction generates, and influences the quality of alumina precursor.
In the present invention, the additive that adds in the hydrolytic process is following a kind of compound at least, and carboxylic acid is as stearic acid, lauric acid, Glacial acetic acid, citric acid, oxalic acid etc.; Tensio-active agent as: polyoxyethylene glycol (molecular weight is below 1000), Diisopropylamine, tween-80 etc., the mol ratio of hydrolysis additives and aluminium-alcohol salt was at least 1: 30, was preferably 1: 20 to 1: 10.
In the present invention, hydrolysising reacting temperature in 40-90 ℃, is preferably 50-75 ℃ usually, digestion time be 6-12 hour preferable.
In the present invention, in alumina precursor, add α-Al
2O
3Powder is as crystal seed, its average grain diameter should be in 100 nanometers, its addition is usually in 1-10% (by the mass percent of theoretical gained aluminium oxide), be preferably 1-6%, ammonium salt can be organic ammonium salt or inorganic ammonium salt, be at least a kind of in the following compound, and organic ammonium salt is such as ammonium oxalate, ammonium citrate, ammonium acetate.Inorganic ammonium salt is as volatile salt, bicarbonate of ammonia, and ammonium nitrate etc., add-on is 10-40% (by the mass percent of theoretical gained aluminum oxide).
In the present invention, used ball mill can be various planetary high speed ball mills, its ball milling speed is at least 500 rev/mins, the ball milling time is 3-12 hour, be preferably 4-8 hour, in order to obtain high-purity alumina product, ball-milling medium adopts the high purity aluminium oxide ball, and dispersion medium can be deionized water or dehydrated alcohol.
In the present invention, do not decompose in order to make the ammonium salt in the ball milling, the bake out temperature of the aluminium hydroxide behind the ball milling is below 80 ℃, be preferably 50-80 ℃, the too low water evaporates of temperature gets too slow, affects production efficiency, the too high ammonium salt that adds might decompose, impact calcination technology thereafter.
In the present invention, the calcination of aluminium hydroxide can be at box-type furnace or tunnel type kiln, and calcination temperature is 1000-1100 ℃, and calcination time is 2-8 hour, is preferably 4-6 hour.
Compared with prior art, method of the present invention can make high-purity superfine alpha-Al that good dispersion, particle diameter are evenly distributed
2O
3Powder.
Description of drawings
Fig. 1 is the process chart of preparation high-purity ultra-fine alumina.
Embodiment
Raw materials used aluminium-alcohol salt is the analytical pure level among the embodiment.
Embodiment one: in 1 liter there-necked flask, adding mass concentration is the aqueous isopropanol 500g of 50% aluminum isopropylate, place 70 ℃ water-bath, add the 20g lauric acid while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds simultaneously 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium citrate of 20g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 70 ℃ of oven dry, with the 1050 ℃ of calcinations 5 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 110nm.
Embodiment two: in 1 liter there-necked flask, adding mass concentration is the aqueous isopropanol 500g of 50% aluminum isopropylate, place 70 ℃ water-bath, add the 20g Macrogol 200 while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium carbonate of 20g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 60 ℃ of oven dry, with the 1050 ℃ of calcinations 5 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 120nm.
Embodiment three: in 1 liter there-necked flask, adding mass concentration is the aqueous isopropanol 500g of 50% aluminum isopropylate, place 70 ℃ water-bath, add the 20g tween-80 while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium nitrate of 20g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 75 ℃ of oven dry, with the 1050 ℃ of calcinations 6 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 120nm.
Embodiment four: in 1 liter there-necked flask, adding mass concentration is the aqueous isopropanol 500g of 50% aluminum isopropylate, place 70 ℃ water-bath, add the 20g citric acid while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium citrate of 20g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 70 ℃ of oven dry, with the 1050 ℃ of calcinations 4 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 130nm.
Embodiment five: in 1 liter there-necked flask, adding mass concentration is the aqueous isopropanol 500g of 50% aluminum isopropylate, place 70 ℃ water-bath, add the 15g Diisopropylamine while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium acetate of 20g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 70 ℃ of oven dry, with the 1100 ℃ of calcinations 4 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 150nm.
Embodiment six: in 1 liter there-necked flask, adding mass concentration is the aqueous isopropanol 500g of 50% aluminum isopropylate, place 70 ℃ water-bath, add the 20g lauric acid while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 3.5g a-Al
2O
3As crystal seed and the analytically pure ammonium citrate of 20g as additive, add simultaneously an amount of absolute ethyl alcohol as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then oven dry in about 70 ℃ in baking oven, with the 1000 ℃ of calcinations 6 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 100nm.
Embodiment seven: in 1 liter there-necked flask, adding mass concentration is the ethanolic soln 500g of 50% 3 aluminum ethylate, place 70 ℃ water-bath, add the 20g lauric acid while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 1.8g a-Al
2O
3As crystal seed and the analytically pure ammonium citrate of 20g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 70 ℃ of oven dry, with the 1100 ℃ of calcinations 6 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 160nm.
Embodiment eight: in 1 liter there-necked flask, adding mass concentration is the ethanolic soln 500g of 50% 3 aluminum ethylate, place 70 ℃ water-bath, add the 10g lauric acid while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium citrate of 20g as additive, add simultaneously an amount of absolute ethyl alcohol as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then oven dry in about 70 ℃ in baking oven, with the 1050 ℃ of calcinations 5 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 150nm.
Embodiment nine: in 1 liter there-necked flask, adding mass concentration is the ethanolic soln 500g of 50% aluminium secondary butylate, place 70 ℃ water-bath, add the 20g lauric acid while stirring as additive, continue to stir thorough mixing, when stirring, splash into the aqueous isopropanol 80g that mass concentration is 75% deionized water then, left standstill 10 hours after reaction finishes, filter standby.The alumina precursor that obtains after filtration places the ball milling cylinder, adds 2.5g a-Al
2O
3As crystal seed and the analytically pure ammonium citrate of 10g as additive, add simultaneously an amount of deionized water as decentralized medium and high purity aluminium oxide ball as ball-milling medium, ball milling 5 hours, then in baking oven in 60 ℃ of oven dry, with the 1100 ℃ of calcinations 4 hours in batch-type furnace of the aluminium hydroxide after the oven dry, namely obtain a-Al
2O
3Powder, its average grain diameter are 170nm.
Claims (3)
1, a kind of good dispersion, high-purity superfine alpha-Al of preparing
2O
3Method, adopt the aluminium-alcohol salt hydrolysis, it is characterized in that may further comprise the steps:
(1) in the aluminium-alcohol salt hydrolytic process, adds hydrolysis additives: a kind of in carboxylic acid or the tensio-active agent; Aging through 40～90 ℃ of hydrolysis, 6～12 hours, obtain alumina precursor after filtering; Raw material aluminium-alcohol salt purity is the analytical pure level;
(2) in alumina precursor, add α-Al of average grain diameter＜100nm of 1～10%
2O
3As crystal seed and 10-40% ammonium salt additive, add deionized water simultaneously or absolute alcohol is done decentralized medium, the high purity aluminium oxide ball is done ball-milling medium, in high speed ball mill ball milling 3-12 hour;
(3) alumina precursor behind the ball milling again through 1000～1100 ℃ of calcinations, namely obtains a-Al 40～80 ℃ of lower oven dry
2O
3Powder;
Carboxylic acid in the hydrolysis additives that adds in the described hydrolytic process is stearic acid, lauric acid, Glacial acetic acid, citric acid, oxalic acid; Tensio-active agent is polyoxyethylene glycol, Diisopropylamine, tween-80, wherein molecular weight polyethylene glycol＜1000; The mol ratio of hydrolysis additives and aluminium-alcohol salt is 1: 10～30; The ratio of aluminium-alcohol salt and deionized water is 1: 1～6;
Described ammonium salt additive is a kind of in volatile salt, bicarbonate of ammonia, ammonium acetate, ammonium oxalate, ammonium citrate, ammonium nitrate, ammonium tartrate, the ammonium hydrogen tartrate.
2, a kind of good dispersion, high-purity superfine alpha-Al of preparing according to claim 1
2O
3Method, when it is characterized in that in the aluminium-alcohol salt hydrolytic process adding hydrolysis additives, the mol ratio of hydrolysis additives and aluminium-alcohol salt is 1: 10～20; The ratio of aluminium-alcohol salt and deionized water is 1: 2～5; Hydrolysis temperature is 50～75 ℃.
3, a kind of good dispersion, high-purity superfine alpha-Al of preparing according to claim 1
2O
3Method, it is characterized in that described in high speed ball mill the time of ball milling be 4～8 hours.
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| CN102070165A (en) * | 2010-12-07 | 2011-05-25 | 邹平金刚新材料有限公司 | High temperature production process of alpha-aluminum oxide |
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| US5455019A (en) * | 1992-12-25 | 1995-10-03 | Chemical Company, Limited Sumitomo | Continuous process for preparing aluminum hydroxide |
| JP3744006B2 (en) * | 1993-04-13 | 2006-02-08 | 住友化学株式会社 | α-Alumina powder and method for producing the same |
| CN1031396C (en) * | 1993-07-20 | 1996-03-27 | 浙江大学 | Method for preparing alpha-alumina particles with nanometers size |
| TW200503953A (en) * | 2003-06-12 | 2005-02-01 | Showa Denko Kk | Method for producing particulate alumina and composition containing particulate alumina |
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| CN102249275A (en) * | 2011-05-12 | 2011-11-23 | 大连理工大学 | Method for preparing photoelectric-grade high-purity alumina with high sintering activity |
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