CN100457629C - Process for preparing high purity flake alpha-Al2O3 and its super fine powder - Google Patents
Process for preparing high purity flake alpha-Al2O3 and its super fine powder Download PDFInfo
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- CN100457629C CN100457629C CNB2006101460417A CN200610146041A CN100457629C CN 100457629 C CN100457629 C CN 100457629C CN B2006101460417 A CNB2006101460417 A CN B2006101460417A CN 200610146041 A CN200610146041 A CN 200610146041A CN 100457629 C CN100457629 C CN 100457629C
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- high purity
- al2o3
- alpha
- gum
- purity flake
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Abstract
The process of preparing high purity flaky alpha-Al2O3 and its superfine powder includes the following steps: 1. mixing analytic pure aluminum nitrate nonahydrate and water soluble polymer in the same weight, and grinding at room temperature to homogenize; 2. heating the mixture in a dryer at 150 deg.C for 30 min to obtain puffed yellow product; 3. maintaining at 1000-1200 deg.C for 1-2 hr to obtain high purity flaky alpha-Al2O3; and 4. mixing high purity flaky alpha-Al2O3 in 100 weight and anhydrous alcohol in 500-800 weight portions, ball milling for 24-48 hr, stoving at 80-100 deg.C to obtain superfine high purity flaky alpha-Al2O3 powder of 0.17-0.8 micron average particle size. The present invention has low cost, simple technological process, and high product purity.
Description
Technical field
That the present invention relates to is a kind of high purity flake alpha-Al
2O
3The preparation method of superfine powder.
Background technology
Tabular alumina has resistance to acids and bases, and is high temperature resistant, hardness height, fusing point height, the high and high a lot of good performances of resistivity of thermal conductivity; Also have in addition the not available good hear resistance of other flaky powder and high mechanical strength.Therefore, can be widely used in numerous areas such as pigment, coating, makeup, automobile finish, printing ink, filler and abrasive material.
Preparing the most frequently used method of tabular alumina is hydro-thermal or pure thermal synthesis method.The tabular alumina of Hydrothermal Preparation is characterised in that it has thin plate-like structure, and the shape homogeneous; Can keep stable dispersion state to such an extent as in solution, have good orientation.But under hydrothermal condition, α-Al
2O
3The phase transition temperature of crystal higher (＞400 ℃), in order to reduce hydrothermal temperature, people again with KBr and carbon number greater than 4 glycol as reaction medium, with the Al (OH) of new preparation
3Colloid is predecessor, adopts pure thermal response, under 300 ℃ temperature, has prepared the tabular α-Al of hexagonal
2O
3Powder.In addition, the method for preparing tabular alumina also has ball milled and coating method etc.
The CN1092381A (application number 94100796.0) of Sai Ersi R Xibe spy, the special magnificent L Ge Lawen of love and Jr application has wherein introduced a kind of method that adopts the Prepared by Ball Milling tabular alumina.
Hydro-thermal or alcohol heat and established law technology more complicated, ball-milling method is difficult to prepare highly purified sheet α-Al
2O
3
Summary of the invention
The object of the present invention is to provide preparation high purity flake alpha-Al that a kind of cost is low, technical process simple, easily produce
2O
3The preparation method of superfine powder, and prepared sheet α-Al
2O
3Purity only depend on the purity of used raw material.
Concrete steps of the present invention are as follows:
(1) quality such as analytically pure nine water aluminum nitrates and water-soluble polymer are mixed, and grind under the room temperature evenly;
(2) will grind uniform material directly put into 150 ℃ of drying boxes heating 30 minutes yellow puffy product;
(3) yellow puffy product is incubated 1～2 hour at 1000 ℃～1200 ℃, obtains high purity flake alpha-Al
2O
3
(4) with the high purity flake alpha-Al of 100 mass parts
2O
3, add the absolute ethyl alcohol of 500～800 mass parts, with general milling machine ball milling 24～48 hours, slurry 80 ℃～100 ℃ directly dry by the fire in, obtain average grain diameter between high pure and ultra-fine sheet α-Al of 0.17 μ m～0.8 μ m
2O
3
Above-mentioned water-soluble polymer is one or more composite in starch, starch derivative, agar-agar, gum arabic, tragacanth gum, locust bean gum, tamarind seed polysaccharide glue, sesbania gum, guar gum, carrageenin, pectin and the polyvinyl alcohol.
Description of drawings
Fig. 1 is the embodiment of the invention 1 sheet α-Al
2O
3Sem photograph.
Fig. 2 is the embodiment of the invention 1 sheet α-Al
2O
3Cross-sectional scans Electronic Speculum figure.
Embodiment
Embodiment 1:
(1) quality such as analytically pure nine water aluminum nitrates and Zulkovsky starch are mixed, and grind under the room temperature evenly;
(2) will grind uniform material directly put into 150 ℃ of drying boxes heating 30 minutes yellow puffy product;
(3) yellow puffy product is incubated 2 hours at 1000 ℃, obtains high purity flake alpha-Al
2O
3
(4) with the high purity flake alpha-Al of the above-mentioned gained of 100 mass parts
2O
3, add the absolute ethyl alcohol of 500 mass parts, with general milling machine ball milling 24 hours; Slurry is 80 ℃ of directly oven dry, and obtaining average grain diameter is high pure and ultra-fine sheet α-Al of 0.35 μ m
2O
3
Embodiment 2:
(1) quality such as analytically pure nine water aluminum nitrates and tapioca (flour) are mixed, and grind under the room temperature evenly;
(2) will grind uniform material directly put into 150 ℃ of drying boxes heating 30 minutes yellow puffy product;
(3) yellow puffy product is incubated 1 hour at 1200 ℃, obtains high purity flake alpha-Al
2O
3
(4) with the high purity flake alpha-Al of the above-mentioned gained of 100 mass parts
2O
3, add the absolute ethyl alcohol of 600 mass parts, with general milling machine ball milling 24 hours; Slurry is 80 ℃ of directly oven dry, and obtaining average grain diameter is high pure and ultra-fine sheet α-Al of 0.5 μ m
2O
3
Embodiment 3:
(1) quality such as analytically pure nine water aluminum nitrates and gum arabic are mixed, and grind under the room temperature evenly;
(2) will grind uniform material directly put into 150 ℃ of drying boxes heating 30 minutes yellow puffy product;
(3) yellow puffy product is incubated 2 hours at 1000 ℃, obtains high purity flake alpha-Al
2O
3
(4) with the high purity flake alpha-Al of the above-mentioned gained of 100 mass parts
2O
3, add the absolute ethyl alcohol of 500 mass parts, with general milling machine ball milling 24 hours; Slurry is 80 ℃ of directly oven dry, and obtaining average grain diameter is high pure and ultra-fine sheet α-Al of 0.4 μ m
2O
3
Claims (1)
1. high purity flake alpha-Al
2O
3The preparation method of superfine powder is characterized in that concrete steps are:
(1) quality such as composite of one or more in analytically pure nine water aluminum nitrates and water-soluble polymer starch, starch derivative, agar-agar, gum arabic, tragacanth gum, locust bean gum, tamarind seed polysaccharide glue, sesbania gum, guar gum, carrageenin, pectin and the polyvinyl alcohol is mixed, and grinds under the room temperature evenly;
(2) will grind uniform material directly put into 150 ℃ of drying boxes heating 30 minutes yellow puffy product;
(3) yellow puffy product is incubated 1～2 hour at 1000 ℃～1200 ℃, obtains high purity flake alpha-Al
2O
3
(4) with the high purity flake alpha-Al of 100 mass parts
2O
3, the absolute ethyl alcohol of adding 500～800 mass parts, ball milling 24～48 hours, slurry obtains average grain diameter between high pure and ultra-fine sheet α-Al of 0.17 μ m～0.8 μ m 80 ℃～100 ℃ directly oven dry
2O
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101460417A CN100457629C (en) | 2006-10-31 | 2006-10-31 | Process for preparing high purity flake alpha-Al2O3 and its super fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101460417A CN100457629C (en) | 2006-10-31 | 2006-10-31 | Process for preparing high purity flake alpha-Al2O3 and its super fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1944262A CN1944262A (en) | 2007-04-11 |
| CN100457629C true CN100457629C (en) | 2009-02-04 |
Family
ID=38043946
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101460417A Expired - Fee Related CN100457629C (en) | 2006-10-31 | 2006-10-31 | Process for preparing high purity flake alpha-Al2O3 and its super fine powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100457629C (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1083537A (en) * | 1965-07-16 | 1967-09-13 | Allied Chem | Process for decomposing aluminium nitrate nonahydrate |
| EP1148028A2 (en) * | 2000-04-17 | 2001-10-24 | Ykk Corporation | Flake-like alpha-alumina particles and method for producing the same |
| CN1435371A (en) * | 2003-03-12 | 2003-08-13 | 北京科技大学 | Method for preparing aluminium nitride powder |
| JP2005082441A (en) * | 2003-09-08 | 2005-03-31 | Sakai Chem Ind Co Ltd | Flaky aluminum oxide, its production method, cosmetic, coating material, ink and plastic composition |
-
2006
- 2006-10-31 CN CNB2006101460417A patent/CN100457629C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1083537A (en) * | 1965-07-16 | 1967-09-13 | Allied Chem | Process for decomposing aluminium nitrate nonahydrate |
| EP1148028A2 (en) * | 2000-04-17 | 2001-10-24 | Ykk Corporation | Flake-like alpha-alumina particles and method for producing the same |
| CN1435371A (en) * | 2003-03-12 | 2003-08-13 | 北京科技大学 | Method for preparing aluminium nitride powder |
| JP2005082441A (en) * | 2003-09-08 | 2005-03-31 | Sakai Chem Ind Co Ltd | Flaky aluminum oxide, its production method, cosmetic, coating material, ink and plastic composition |
Non-Patent Citations (1)
| Title |
|---|
| 超细a－Al2O3的低温燃烧合成及其烧结特性的研究. 王志强，马铁成，蔡英骥，吕秉玲.硅酸盐通报，第5期. 2000 * |
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| Publication number | Publication date |
|---|---|
| CN1944262A (en) | 2007-04-11 |
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Owner name: LIANYUNGANG LIANLIAN CHEMICAL CO., LTD. Free format text: FORMER OWNER: GUILIN UNIVERSITY OF TECHNOLOGY Effective date: 20100818 |
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Free format text: CORRECT: ADDRESS; FROM: 541004 NO.12, JIANGAN ROAD, GUILIN CITY, GUANGXI ZHUANG AUTONOMOUS REGION TO: 222200 SOUTH OF WEIQI ROAD, LINGANG INDUSTRY DISTRICT, GUANYUN COUNTY, JIANGSU PROVINCE, WEST SIDE OF JINGSI ROAD |
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Effective date of registration: 20100818 Address after: 222200, Guanyun County, Jiangsu Province, Lingang Industrial Zone, seven South Road, west side of four road Patentee after: Lianyungang Lianlian Chemicals Co., Ltd. Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: Guilin University of Technology |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090204 Termination date: 20091130 |