CN1903728A - Preparation method of high purity aluminium oxide powder - Google Patents
Preparation method of high purity aluminium oxide powder Download PDFInfo
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- CN1903728A CN1903728A CN 200510028367 CN200510028367A CN1903728A CN 1903728 A CN1903728 A CN 1903728A CN 200510028367 CN200510028367 CN 200510028367 CN 200510028367 A CN200510028367 A CN 200510028367A CN 1903728 A CN1903728 A CN 1903728A
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- alumina powder
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- high purity
- purity alumina
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Abstract
The present invention relates to a preparation method of high-purity aluminium oxide powder body. It is characterized by that it adopts aluminium sheet whose purity is 99.9999% and organic alkal; and makes them be mutually reacted in hot water bath to obtain the precipitate of aluminium hydroxide, then the precipitate is calcined at 1100-1200deg.C and ground so as to obtain high-purity ultrafine aluminium oxide powder body. The described organic alkal; includes any one of choline, hexamethohydrotetramine and dopamine.
Description
Technical field
The present invention relates to a kind of preparation method of high purity alumina powder.More specifically, the present invention relates to a kind of aluminium hydroxide [Al (OH) that adopts metal aluminium flake and organic bases preparation to exist with the gibbsite form
33H
2O], prepare the preparation method of high purity alumina powder then through special processing.Belong to alumina powder jointed preparation field.
Background technology
Al
2O
3Pottery is aspect multi-chip type packaging ceramic multilayer electronic baseplate material, transparent window material, fluor carrier, ceramic sensor, biological ceramics, fixed enzyme vector and other function ceramics and structural ceramics, important role is arranged, Al
2O
3Fine ceramics is considered to formula and leads to one of base mateiral of 21 century high-tech sector, and is more and more higher to raw-material requirement along with the continuous development of new and high technology, as the super-refinement of granularity, particulate homogenizing, the high purifying of component, low sintering temperature or the like.Nano material is exactly to be divided into down this, and flourish, peculiar characteristics such as its surface effects quantum size effect and volume effect will make the material field enter a brand-new stage.
High purity aluminium oxide has many important use.Produce metallic aluminium or, generally can from mining bauxite, obtain aluminum oxide as the basis and the insulating material in electronic industry district and optics industry district.Yet naturally occurring bauxite can not satisfy specification of quality in many purposes.High-performance new ceramics, especially transparent alumina need the high purity aluminium oxide raw material to prepare, and require to reach more than 99.999% or higher purity.
Active A l
2O
3The preparation method of powder is more, and wherein modal is sol-gel method, and this method utilizes organic alkoxide of Al as raw material,, adds a spot of dispersion agent under certain condition, makes its hydrolysis, gelation, and through vacuum-drying, the control pyrolysis temperature finally makes Al
2O
3Powder.The advantage of this method is the nano-powder that can make, but cost of material is higher, and technical process is longer.
Also have high pure metal aluminium is transformed into exsiccated ammonium alum (NH
4Al (SO
4)
212H
2O), exsiccated ammonium alum is soluble in water under the temperature that suits, and solution carries out recrystallization or redeposition after filtering and purifying, then, and through low temperature calcination, the high-purity aluminum oxide of decomposition preparation.The somebody is to adopt the sol-gel technology preparation with salt decomposition methods such as organoaluminum hydrolysis or aluminum bromide preparation, the another kind of technology of producing high-purity powder.At present, high purity aluminium oxide generally adopts the method for chemosynthesis to obtain.Wherein sophisticated technology of preparing is to prepare high purity aluminium oxide by the calcining exsiccated ammonium alum, but this method can produce a large amount of SO in the process of preparation aluminum oxide
3, ecotope is caused disadvantageous effect.
Based on this, the inventor attempts to have prepared Al (OH) by adopting high pure metal aluminium and the reaction of organic bases in hot water
3Precipitation has prepared high-purity nm Al through calcining
2O
3Powder
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high purity aluminium oxide, it is characterized in that adopting high pure metal aluminium and organic bases in hot water, to react, preparation high purity nanometer alumina powder.In the process of reaction, do not produce deleterious gas.
The principle that the present invention prepares the high purity nanometer alumina powder is:
The raw material that the present invention uses is high-purity aluminium flake, organic alkali, hydrochloric acid.
The preparation technology of high purity aluminium hydroxide provided by the invention, calcining process, technologies such as the preparation of aluminum oxide.Its preparation technology is characterised in that:
1, adopting content is that 99.9999% high-purity aluminium flake and water carry out hydration reaction and prepares high purity aluminium hydroxide.
2, at first high-purity aluminium flake is put into hot water bath, then an amount of organic alkali is added in the water-bath, mixture is boiled to is convenient to reaction, reaction makes soluble aluminum hydrochlorate and hydrogen.Employed organic bases is any one in choline, six first hydrogen tetramines, the Dopamine HCL; Its usage quantity is the mole ratio after the balance shown in the equation (1), boiling temperature 〉=80 ℃, boiling time 40-50 minute.
3, then temperature is cooled to room temperature, with solution and mixed in hydrochloric acid, regulates the pH value between 7～8, the precipitation of preparation oxyhydroxide.
4, promptly obtain the aluminium hydroxide that exists with the gibbsite form behind the drying and dehydrating.
5, the above-mentioned aluminium hydroxide that makes can be obtained aluminum oxide in 5-10 hour in 1000 ℃～1200 ℃ following processing in process furnace.
6, place airflow milling to pulverize, sieve in this aluminum oxide again.Make high-purity, size is single alumina powder jointed.
The preparation technology's of high purity alumina powder provided by the invention characteristics are:
1, product has chemical purity height (〉=99.999%), the low (Na of sodium content
2O ≯ 0.0001%), thin (0.1-0.5 μ m), α-Al of particle
2O
3Content height (α phase ≮ 99%), the big (≮ 3.96g/cm of true density
3) etc. property,
2, in alumina powder jointed preparation process, there is not generation poisonous, obnoxious flavour.
3, product is applicable to electron trade, transparent alumina industry, fluorescent material industry.
Embodiment
Embodiment 1
Adopt high-purity aluminium ingot and water to carry out hydration reaction and prepare high purity aluminium hydroxide, at first high-purity aluminium flake is put into hot water bath, then an amount of choline is added in the water-bath, with mixture boiled to 80 ℃, make it reaction, boiling time 50 minutes, the soluble aluminum hydrochlorate and the hydrogen of reaction system.Then temperature is cooled to room temperature, with solution and mixed in hydrochloric acid, regulates the pH value about 7.5, the precipitation of preparation oxyhydroxide promptly obtains the aluminium hydroxide with the gibbsite form behind the drying and dehydrating.The above-mentioned aluminium hydroxide that makes can be obtained aluminum oxide in 8 hours in 1100 ℃ of following processing in retort furnace, place airflow milling to pulverize, sieve in this aluminum oxide again.Make high-purity, size is single alumina powder jointed.
The performance of the powder that obtains:
Chemical purity height (〉=99.999%),
Particle thin (≈ 0.1 μ m),
α-Al
2O
3Content height (α phase ≈ 99%),
Big (the ≈ 3.96g/cm of true density
3)
Embodiment 2
Adopt high-purity aluminium ingot and water to carry out hydration reaction and prepare high purity aluminium hydroxide, at first high-purity aluminium flake is put into hot water bath, then an amount of hexamethylenetetramine is added in the water-bath, with mixture boiled to 85 ℃, boiling time 40 minutes, make it reaction, the soluble aluminum hydrochlorate and the hydrogen of reaction system.Then temperature is cooled to room temperature, with solution and mixed in hydrochloric acid, regulates the pH value about 7, the precipitation of preparation oxyhydroxide promptly obtains the aluminium hydroxide with the gibbsite form behind the drying and dehydrating.Is to handle in the heating element process furnace can obtain aluminum oxide in 8 hours under 1150 ℃ with the above-mentioned aluminium hydroxide that makes at Fe-Cr-Al wire, places airflow milling to pulverize in this aluminum oxide again.The system high-purity, size is single alumina powder jointed.
The performance of the powder that obtains:
Chemical purity height (〉=99.999%),
Particle thin (≈ 0.2 μ m),
α-Al
2O
3Content height (α phase ≈ 99.5%),
Big (the ≈ 3.96g/cm of true density
3)
Embodiment 3
Adopt high-purity aluminium ingot and water to carry out hydration reaction and prepare high purity aluminium hydroxide, at first high-purity aluminium flake is put into hot water bath, then an amount of Dopamine HCL is added in the water-bath, with mixture boiled to 80 ℃, seething with excitement made it reaction in 45 minutes, the soluble aluminum hydrochlorate and the hydrogen of reaction system.Then temperature is cooled to room temperature, with solution and mixed in hydrochloric acid, regulates the pH value about 8, the precipitation of preparation oxyhydroxide promptly obtains the aluminium hydroxide with the gibbsite form behind the drying and dehydrating.The above-mentioned aluminium hydroxide that makes can be obtained aluminum oxide in 10 hours in 1100 ℃ of following processing in retort furnace, place airflow milling to pulverize in this aluminum oxide again.The system high-purity, size is single alumina powder jointed.
The performance of the powder that obtains:
Chemical purity height (〉=99.999%),
Particle thin (≈ 0.15 μ m),
α-Al
2O
3Content height (α phase ≈ 100%),
Big (the ≈ 3.96g/cm of true density
3)
Embodiment 4
Adopt high-purity aluminium ingot and water to carry out hydration reaction and prepare high purity aluminium hydroxide, at first high-purity aluminium flake is put into hot water bath, then an amount of choline is added in the water-bath, with mixture boiled to 90 ℃, seething with excitement made it reaction in 40 minutes, the soluble aluminum hydrochlorate and the hydrogen of reaction system.Then temperature is cooled to room temperature, with solution and mixed in hydrochloric acid, regulates the pH value about 7.5, the precipitation of preparation oxyhydroxide promptly obtains the aluminium hydroxide with the gibbsite form behind the drying and dehydrating.The above-mentioned aluminium hydroxide that makes can be obtained aluminum oxide in 5 hours in 1200 ℃ of following processing in the globars process furnace, place airflow milling to pulverize in this aluminum oxide again.The system high-purity, size is single alumina powder jointed.
The performance of the powder that obtains:
Chemical purity height (〉=99.999%),
Particle thin (≈ 0.5 μ m),
α-Al
2O
3Content height (α phase ≈ 99%),
Big (the ≈ 3.96g/cm of true density
3).
Claims (8)
1, a kind of preparation method of high purity alumina powder is characterized in that adopting high-purity aluminium flake and water to carry out hydration reaction and prepares aluminium hydroxide, and dry then back is calcined in process furnace and made, and concrete processing step is:
(1) high-purity aluminium flake is put into hot water bath, in water-bath, add an amount of organic bases then, the mixture boiling is reacted, make soluble aluminum hydrochlorate and hydrogen;
(2) be cooled to room temperature then, solution and mixed in hydrochloric acid are regulated pH between 7-8, make precipitation of hydroxide;
(3) the sedimentary oxyhydroxide drying and dehydrating of step (2) is promptly got aluminium hydroxide;
(4) at last aluminium hydroxide is made it decomposition and obtains high-purity α-Al in 1000-1200 ℃ of heating in process furnace
2O
3Block;
(5) alumina block with step (4) gained places the airflow milling pulverizing, sieving obtains high purity alumina powder.
2, by the preparation method of the described high purity alumina powder of claim 1, the purity that it is characterized in that employed high-purity aluminium flake is 99.9999%.
3,, it is characterized in that described organic bases is any one in choline, six first hydrogen tetramines, the Dopamine HCL by the preparation method of the described high purity alumina powder of claim 1.
4, by the preparation method of the described high purity alumina powder of claim 1, it is characterized in that the ratio of high-purity aluminium flake and organic bases, press
Mole ratio after the equation balance, R is the gene of organic bases in the formula.
5, by the preparation method of the described high purity alumina powder of claim 1, it is characterized in that making mixture boiling temperature 〉=80 ℃, boiling time is 40-50 minute.
6, by the preparation method of the described high purity alumina powder of claim 1, it is characterized in that its purity of prepared high purity alumina powder 〉=99.9999%, particle diameter is 0.1-0.5 μ m, and true density is 3.96g/cm
3, α phase 99-100%; Na
2O ≯ 0.0001%.
7, by the preparation method of the described high purity alumina powder of claim 1, it is characterized in that described aluminum hydroxide precipitation is the aluminium hydroxide of gibbsite form.
8, by the preparation method of the described high purity alumina powder of claim 1, it is characterized in that described process furnace be retort furnace, silicon carbide rod furnace, Fe-Cr-Al wire be in the resistance furnace of heating element any one.
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|---|---|---|---|
| CN 200510028367 CN1903728A (en) | 2005-07-29 | 2005-07-29 | Preparation method of high purity aluminium oxide powder |
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| CN 200510028367 CN1903728A (en) | 2005-07-29 | 2005-07-29 | Preparation method of high purity aluminium oxide powder |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153116A (en) * | 2011-02-22 | 2011-08-17 | 马庆忠 | Alumina crystalline material and preparation method and application |
| WO2012055323A1 (en) * | 2010-10-29 | 2012-05-03 | 大连路明发光科技股份有限公司 | Method for preparing na-β"-al2o3 powder |
| CN102583466A (en) * | 2012-02-16 | 2012-07-18 | 山东晶鑫晶体科技有限公司 | High-purity aluminum oxide with small primary crystal and production method of high-purity aluminum oxide |
| CN103214013A (en) * | 2013-04-27 | 2013-07-24 | 昆明冶金研究院 | Preparation method of high-purity alumina powder |
| CN103241756A (en) * | 2012-02-03 | 2013-08-14 | 上海飞凯光电材料股份有限公司 | Preparation method for alumina solid |
| CN104030330A (en) * | 2014-06-14 | 2014-09-10 | 中国科学院过程工程研究所 | Method for preparing high-purity aluminum hydroxide through induced crystallization |
| CN104220373A (en) * | 2012-04-10 | 2014-12-17 | 住友化学株式会社 | Method for producing alumina |
| CN104787794A (en) * | 2015-03-26 | 2015-07-22 | 昆明理工大学 | Self-suction hydrolysis reaction device for preparing high-purity aluminum oxide and application |
| WO2016069743A1 (en) * | 2014-10-28 | 2016-05-06 | Shanghai Phichem Material Co. Ltd. | Methods of preparing high purity aluminum hydroxide and high purity aluminum oxide |
| CN107089676A (en) * | 2017-05-23 | 2017-08-25 | 苏州纳迪微电子有限公司 | A kind of preparation method of high-purity boehmite |
| US10315927B2 (en) | 2014-01-17 | 2019-06-11 | Shanghai Phichem Material Co. Ltd. | Methods and processes of preparing aluminum hydroxide and aluminum oxide |
| CN113382964A (en) * | 2019-04-16 | 2021-09-10 | 斐源有限公司 | Production of high purity alumina and co-product using spent electrolyte from metal-air batteries |
| 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 |
-
2005
- 2005-07-29 CN CN 200510028367 patent/CN1903728A/en active Pending
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012055323A1 (en) * | 2010-10-29 | 2012-05-03 | 大连路明发光科技股份有限公司 | Method for preparing na-β"-al2o3 powder |
| CN102153116A (en) * | 2011-02-22 | 2011-08-17 | 马庆忠 | Alumina crystalline material and preparation method and application |
| CN103241756A (en) * | 2012-02-03 | 2013-08-14 | 上海飞凯光电材料股份有限公司 | Preparation method for alumina solid |
| CN102583466A (en) * | 2012-02-16 | 2012-07-18 | 山东晶鑫晶体科技有限公司 | High-purity aluminum oxide with small primary crystal and production method of high-purity aluminum oxide |
| CN102583466B (en) * | 2012-02-16 | 2014-06-11 | 山东晶鑫晶体科技有限公司 | High-purity aluminum oxide with small primary crystal and production method of high-purity aluminum oxide |
| CN104220373B (en) * | 2012-04-10 | 2016-12-14 | 住友化学株式会社 | The manufacture method of aluminium oxide |
| CN104220373A (en) * | 2012-04-10 | 2014-12-17 | 住友化学株式会社 | Method for producing alumina |
| CN103214013A (en) * | 2013-04-27 | 2013-07-24 | 昆明冶金研究院 | Preparation method of high-purity alumina powder |
| CN103214013B (en) * | 2013-04-27 | 2015-08-05 | 昆明冶金研究院 | A kind of preparation method of high purity alumina powder |
| US10315927B2 (en) | 2014-01-17 | 2019-06-11 | Shanghai Phichem Material Co. Ltd. | Methods and processes of preparing aluminum hydroxide and aluminum oxide |
| CN104030330A (en) * | 2014-06-14 | 2014-09-10 | 中国科学院过程工程研究所 | Method for preparing high-purity aluminum hydroxide through induced crystallization |
| CN104030330B (en) * | 2014-06-14 | 2017-01-18 | 中国科学院过程工程研究所 | Method for preparing high-purity aluminum hydroxide through induced crystallization |
| WO2016069743A1 (en) * | 2014-10-28 | 2016-05-06 | Shanghai Phichem Material Co. Ltd. | Methods of preparing high purity aluminum hydroxide and high purity aluminum oxide |
| CN104787794B (en) * | 2015-03-26 | 2016-06-22 | 昆明理工大学 | A kind of self-priming hydrolysis reaction device preparing high purity aluminium oxide and application |
| CN104787794A (en) * | 2015-03-26 | 2015-07-22 | 昆明理工大学 | Self-suction hydrolysis reaction device for preparing high-purity aluminum oxide and application |
| CN107089676A (en) * | 2017-05-23 | 2017-08-25 | 苏州纳迪微电子有限公司 | A kind of preparation method of high-purity boehmite |
| CN107089676B (en) * | 2017-05-23 | 2018-11-27 | 苏州纳迪微电子有限公司 | A kind of preparation method of high-purity boehmite |
| CN113382964A (en) * | 2019-04-16 | 2021-09-10 | 斐源有限公司 | Production of high purity alumina and co-product using spent electrolyte from metal-air batteries |
| 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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Open date: 20070131 |