CN101659547A - Preparation method of high-purity super fine alumina - Google Patents
Preparation method of high-purity super fine alumina Download PDFInfo
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- CN101659547A CN101659547A CN200910031927A CN200910031927A CN101659547A CN 101659547 A CN101659547 A CN 101659547A CN 200910031927 A CN200910031927 A CN 200910031927A CN 200910031927 A CN200910031927 A CN 200910031927A CN 101659547 A CN101659547 A CN 101659547A
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Abstract
The invention discloses a preparation method of high-purity super fine alumina, which is characterized by comprising the following steps: carrying out the hydrolysis reaction on high-purity organic aluminum alkoxide in the presence of organic or inorganic acids at 40-95 DEG C, mixing for 3-8 hours, aging for 10-20 hours, then filtering the feed liquid, washing with deionized water to generate aluminium hydroxide as an intermediate product; drying the aluminium hydroxide at 110 DEG C, roasting the aluminium hydroxide at 1000-1300 DEG C, keeping the temperature for 1-4 hours, and controlling thesize of the generated particles to be between 50nm and 200nm. By adopting the preparation method, the size of the particles of the product is even, the product purity is above 99.9%, and the conversion ratio of the alpha-Al2O3 crystal form is above 90%.
Description
Technical field
The present invention relates to a kind of preparation method of nano aluminium oxide, relate in particular to a kind of control method of nano aluminium oxide particle diameter.
Background technology
Generally, people product purity greater than 99.9% the high purity product that calls; The call nanometer materials of diameter less than 100nm; Particle diameter be 0.1 μ m-1 μ m call the submicron order material; Is particle diameter calling of 1 μ m-10 μ m to be the treasured book material; Usually micron order, submicron order and nano level material are referred to as ultra tiny material.
We know, high-purity super fine alumina at home and abroad has broad prospects on the market as a kind of emerging high-tech product, yet, common complete processing can not satisfy the requirement of preparation high-purity super fine alumina, so finding out various energy, people satisfy the method for preparing high-purity super fine alumina, mainly contain: the exsiccated ammonium alum pyrolysis method is the tschermigite pyrolysis method, alkoxide hydrolysis, low-carbon alkyl aluminium hydrolysis method, chloroethanol method, crystal aluminum chloride pyrolysis method, the improvement Bayer process, spark-discharge method etc., all there is certain defective in these methods to the requirement of modern high-purity super fine alumina, and for example size distribution is inhomogeneous, particle diameter is excessive etc.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-purity super fine, control by maturing temperature and soaking time, it is even to obtain the product grains size, the purity height, and between 50-200nm, satisfy the high-purity and narrow requirement of size distribution of modern high technology product between the particle of alumina product to aluminum oxide.
Solution of the present invention is: a kind of preparation method of high-purity super fine, under 40-95 ℃ of temperature, in the environment that organic acid or mineral acid exist, with the reaction that is hydrolyzed of the organic aluminium alcoholates of high purity, stirred 3-8 hour, aging after 10-20 hour, feed liquid is filtered, use deionized water wash, generate intermediate product aluminium hydroxide; Aluminium hydroxide is dry under 110 ℃ of temperature, 1000-1300 ℃ roasting temperature also is incubated 1-4 hour, and the grain-size that control generates is between the 50-200nm.
Described organic aluminium alcoholates is aluminum ethylate or aluminum isopropylate.
Described mineral acid is sulfuric acid and hydrochloric acid.
Described organic acid is formic acid, acetate, butyric acid, citric acid, lactic acid, toxilic acid or oxysuccinic acid.
Usefulness of the present invention is:
1. the nano aluminium oxide purity of this present invention preparation is more than 99.9%, and α-Al
2O
3The transformation efficiency of crystal formation is more than 90%.
2, the grain-size homogeneous of product of the present invention uses U.S. PSS laser particle analyzer particle tested particle size dispersion degree less than 0.2.
3, product purity height of the present invention, help protecting environment, the component of the raw material aluminium alcoholates that adopts in the invention is C, H, O, Al, does not have NH
3, SO
2Deng composition, under 1000-1300 ℃ maturing temperature, when obtaining high-purity alpha-alumina, liquid does not have a large amount of NH
3, SO
2Deng the discharging of corrosive gases or liquid, not only help protecting plant and instrument, and do not pollute the environment, influence the healthy of people, thereby have good benefits in environment.
4, the production technique of the present invention's employing is simple, and reduced investment is with low cost, is easy to realize industrialization.
Embodiment
Embodiment 1:
With aluminum ethylate 90g, deionized water 50ml, the 3ml concentrated hydrochloric acid mixes, under 65 ℃, and stirring reaction 5h, aging after 10 hours, feed liquid is filtered, use deionized water wash, 100 ℃ of oven dry; 1100 ℃ of following roastings, soaking time is controlled at 2.5h then.Obtain α-Al20330.1g, purity 99.9%, particle grain size is tested with U.S. PSS laser particle analyzer, and particle diameter is 80nm, dispersity 0.18.
Embodiment 2:
With aluminum isopropylate 100g, deionized water 60ml, the 5ml vitriol oil mixes, under 65 ℃, and stirring reaction 5h, aging after 10 hours, feed liquid is filtered, use deionized water wash, 100 ℃ of oven dry; 1250 ℃ of following roastings, soaking time is controlled at 3h then.Obtain α-Al20330.1g, purity 99.9%, particle grain size is tested with U.S. PSS laser particle analyzer, and particle diameter is 90nm, dispersity 0.15.
Claims (4)
1, a kind of preparation method of high-purity super fine, it is characterized in that: under 40-95 ℃ of temperature, in the environment that organic acid or mineral acid exist, with the reaction that is hydrolyzed of the organic aluminium alcoholates of high purity, stirred 3-8 hour, aging after 10-20 hour, feed liquid is filtered, use deionized water wash, generate intermediate product aluminium hydroxide; Aluminium hydroxide is dry under 110 ℃ of temperature, 1000-1300 ℃ roasting temperature also is incubated 1-4 hour, and the grain-size that control generates is between the 50-200nm.
2, preparation method of high-purity super fine according to claim 1 is characterized in that: described organic aluminium alcoholates is aluminum ethylate or aluminum isopropylate.
3, preparation method of high-purity super fine according to claim 1 is characterized in that: described mineral acid is sulfuric acid or hydrochloric acid.
4, preparation method of high-purity super fine according to claim 1 is characterized in that: described organic acid is formic acid, acetate, butyric acid, citric acid, lactic acid, toxilic acid or oxysuccinic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910031927A CN101659547A (en) | 2009-07-03 | 2009-07-03 | Preparation method of high-purity super fine alumina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910031927A CN101659547A (en) | 2009-07-03 | 2009-07-03 | Preparation method of high-purity super fine alumina |
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| CN101659547A true CN101659547A (en) | 2010-03-03 |
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| CN200910031927A Pending CN101659547A (en) | 2009-07-03 | 2009-07-03 | Preparation method of high-purity super fine alumina |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560521A (en) * | 2012-01-14 | 2012-07-11 | 新疆哥兰德新能源有限公司 | Method for electrochemically preparing high-purity aluminum oxide |
| CN102943280A (en) * | 2012-10-18 | 2013-02-27 | 成都华泽晶体材料有限公司 | Method for preparing high-purity aluminium hydroxide powder by electrochemical method |
| CN103011216A (en) * | 2012-12-20 | 2013-04-03 | 大连理工大学 | Recovery method for ageing liquid in process of preparing high sintering activated aluminum oxide |
| CN103304223A (en) * | 2013-06-13 | 2013-09-18 | 景德镇陶瓷学院 | Preparation method of high-purity aluminum oxide ceramic |
-
2009
- 2009-07-03 CN CN200910031927A patent/CN101659547A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560521A (en) * | 2012-01-14 | 2012-07-11 | 新疆哥兰德新能源有限公司 | Method for electrochemically preparing high-purity aluminum oxide |
| CN102943280A (en) * | 2012-10-18 | 2013-02-27 | 成都华泽晶体材料有限公司 | Method for preparing high-purity aluminium hydroxide powder by electrochemical method |
| CN102943280B (en) * | 2012-10-18 | 2016-01-06 | 成都华泽晶体材料有限公司 | A kind of method of electrochemical production Two-step purifying body |
| CN103011216A (en) * | 2012-12-20 | 2013-04-03 | 大连理工大学 | Recovery method for ageing liquid in process of preparing high sintering activated aluminum oxide |
| CN103304223A (en) * | 2013-06-13 | 2013-09-18 | 景德镇陶瓷学院 | Preparation method of high-purity aluminum oxide ceramic |
| CN103304223B (en) * | 2013-06-13 | 2014-12-17 | 景德镇陶瓷学院 | Preparation method of high-purity aluminum oxide ceramic |
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Open date: 20100303 |