CN104787786A - Alpha-alumina preparation method - Google Patents
Alpha-alumina preparation method Download PDFInfo
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- CN104787786A CN104787786A CN201510084063.4A CN201510084063A CN104787786A CN 104787786 A CN104787786 A CN 104787786A CN 201510084063 A CN201510084063 A CN 201510084063A CN 104787786 A CN104787786 A CN 104787786A
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- Prior art keywords
- alumina
- aluminum oxide
- temperature
- alpha
- ramp
- Prior art date
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 25
- 238000010792 warming Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 159000000013 aluminium salts Chemical class 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 206010020843 Hyperthermia Diseases 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- FOJJCOHOLNJIHE-UHFFFAOYSA-N aluminum;azane Chemical compound N.[Al+3] FOJJCOHOLNJIHE-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000012738 dissolution medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention discloses an alpha-alumina preparation method, which comprises: 1) heating alumina to a temperature of 1200-1220 DEG C within 1-6 h; 2) adjusting the temperature to 1220-1260 DEG C, and maintaining the temperature and carrying out calcination for 2-5 h; and 3) cooling to a temperature of 100-200 DEG C within 2-4 h. The alpha-alumina obtained according to the method of the present invention has high purity and does not contain other crystal phases of the alumina, wherein the particle size is 5.0-7.0 [mu]m, and the purity is 100%..
Description
Technical field
The invention belongs to metal oxide preparation field, be specifically related to a kind of preparation method of Alpha-alumina.
Background technology
Alpha-alumina is a kind of form of low-temperature oxidation aluminium, and the aluminium hydroxide hyperthermia drying that it adopts purity high is usually formed.Alpha-alumina is generally obtained by calcinations of aluminum hydroxide or alumina preparation, but could all be converted into gamma oxidation aluminium powder when needing sintering oven to reach 1400 DEG C, and required power consumption is large, and cost increases, and is unfavorable for large-scale production.And this process is strict to temperature control requirement, otherwise not only also have part θ phase containing γ phase in product, very large impact is existed for subsequent processes.
It is dissolution medium that patent documentation CN1065255 discloses with hydrochloric acid, the aluminum-containing mineral through calcination process is added hydrochloric acid and reacts, obtain alkaline aluminium salt, through being separated desiliconization.Alkaline aluminium salt after being separated is carried out inspissation, roasting to 700 ~ 800 DEG C, produces gama-alumina, obtain product Alpha-alumina by 1100 DEG C of calcinings.But the method only can obtain the aluminum oxide of technical purity, cannot meet the preparation of more highly purified aluminum oxide.
Patent documentation CN103241754A discloses a kind of production method of high-purity alpha-alumina, comprise and prepare exsiccated ammonium alum, exsiccated ammonium alum recrystallization, produce the regeneration of high purity aluminium oxide and exhaust collection and ammonium sulfate, it is first by aluminium hydroxide and sulfuric acid extracting sulfuric acid aluminium ammonium, again recrystallization high purity exsiccated ammonium alum is carried out to exsiccated ammonium alum, then generate γ-Al by low temperature dewatering and middle temperature decomposing and calcining
2o
3, decompose to deviate from whole ammonia, sulphur trioxide and water vapour, then by γ-Al
2o
3screening after broken, send High Temperature Furnaces Heating Apparatus to sinter and obtains α-Al after the die-filling die mould of forming press
2o
3.
At present, the transformation of crystalline phase when preparing aluminum oxide for aluminium hydroxide, there is not unified viewpoint in academia.As " hydrated aluminum oxide crystalline phase change at different temperatures prepared by the precipitator method " thinks that the temperature that exists of gama-alumina is 800-900 DEG C, there is temperature and be then more than 1000 DEG C in Alpha-alumina, and other people research shows that gama-alumina occurs after 500 or 600 DEG C, but it should be noted that aluminum oxide have 8 kinds of crystal form: χ-, η-, γ-, δ-, κ-, θ-, ρ-, α-Al
2o
3.Industrially as catalyzer use aluminum oxide mainly porous aluminum oxide (as η-, γ-, θ-Al
2o
3) one or its mixture.Prepare except by special approach, commercial alumina seldom have single crystal form (as η-, γ-Al
2o
3in just normal containing θ-Al
2o
3), the phase transformation between different aluminum oxide is not only relevant with temperature, also affects by foreign matter content.
It is generally acknowledged η-Al
2o
3turn θ-Al
2o
3temperature is 480 DEG C; χ-Al
2o
3turn κ-Al
2o
3for ~ 500 DEG C; γ-Al
2o
3turn δ-Al
2o
3it is 820 DEG C; δ-Al
2o
3turn θ-Al
2o
3for ~ 980 DEG C; All crystal form aluminum oxide all transfer α-Al to more than 1200 DEG C
2o
3.Contriver also finds the aluminum oxide containing other crystalline phases in the Alpha-alumina that method conventionally prepares by experiment, and purity cannot satisfy the demands.
Summary of the invention
The object of the invention is to propose a kind of energy-conservation, high-level efficiency, maintenance purity and phase transformation transformation efficiency is the method for 100% novel sintered alpha-aluminium oxide powder.
Method of the present invention comprises:
1) aluminum oxide is warming up to 1220-1260 DEG C in 1-6h;
2) adjusting temperature is 1220-1260 DEG C, and maintains this temperature calcination 2-5h;
3) in 2-4h, 100-200 DEG C is cooled to.
Preferably, described step 1) comprise following heating step: described step 1) comprise following heating step: in 1-3h, be warming up to 800-950 DEG C, after heat up in 1-3h and reach 1200-1220 DEG C.
Preferably, described step 1) in the speed of aluminum oxide one 245-255 DEG C/h be elevated to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 135-145 DEG C, the aluminum oxide of finished product grain size at 6.0-6.5um can be obtained.
Preferably, described step 1) in aluminum oxide with the ramp of 225-235 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 145-155 DEG C, the aluminum oxide of finished product grain size at 6.5-7.0um can be obtained.
Preferably, described step 1) in aluminum oxide with the ramp of 255-265 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 125-145 DEG C, the aluminum oxide of finished product grain size at 5.0-5.5um can be obtained.
Preferably, described step 1) in aluminum oxide with the ramp of 235-245 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 115-125 DEG C, the aluminum oxide of finished product grain size at 5.5-6.0um can be obtained.
Preferably, purity >=99.99% of described aluminum oxide, particle diameter at 4.8-6.0um, humidity≤5%.
Concrete, Two-step purifying can be placed in sintering boat in batches, build boat lid, again sintering boat is placed on the first side of the roller kiln getting out temperature curve and reserve rotating speed, sintering boat is sent to tail side from the first side of roller kiln, comes out of the stove, and namely can obtain product of the present invention.
During calcining, along with the rising of temperature, particle starts thermal motion, after arriving certain temperature, particle starts reunion, overall volume starts to shrink, and the gap between coacervate and coacervate increases, the temperature in crucible can be made to reach balanced, particle can be made to keep uniformity.
In addition, during calcining, experienced by chilling process, after first preparing γ-crystalline phase, be converted into Alpha-alumina, experience twice crystal transition and can prepare the higher product of purity.
The Alpha-alumina obtained according to method of the present invention has the high feature of purity, and its particle diameter is 5.0-7.0 micron, and can control the particle diameter of product by controlling sintering temperature, and purity is 100%, and not containing the aluminum oxide of other crystalline phases.
Embodiment
The following is the preferred embodiments of the present invention, it is only used as the explanation of the application and unrestricted.
By Two-step purifying (4.8-6.0um, purity >99.99%) be placed in sintering boat in batches, build boat lid, again sintering boat is placed on the first side of the roller kiln getting out temperature curve and reserve rotating speed, intensification (heating-up time 2h) removes the moisture in product and sloughs the part water of the combination in product, when 1200-1260 DEG C to product Isothermal sinter, sintering boat temperature starts to decline afterwards, the temperature being sent to sintering boat during tail side reaches controlled range, comes out of the stove and all can be converted into alpha-aluminium oxide powder.The product cut size obtained is 6.4 microns, and its crystalline phase is Alpha-alumina.
Actual conditions and the product parameters of the embodiment 1-10 carried out according to aforesaid operations step are as follows:
The heating condition of table 1, embodiment 1-10 and product parameters
Claims (6)
1. prepare a method for Alpha-alumina, comprising:
1) aluminum oxide is warming up to 1220-1260 DEG C in 1-6h;
2) adjusting temperature is 1220-1260 DEG C, and maintains this temperature calcination 2-5h;
3) in 2-4h, 100-200 DEG C is cooled to.
2. method according to claim 1, is characterized in that, described step 1) comprise following heating step: in 1-3h, be warming up to 800-950 DEG C, after in 1-3h heat up reach 1200-1220 DEG C.
3. method according to claim 1, is characterized in that, described step 1) in aluminum oxide with the ramp of 245-255 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 135-145 DEG C.
4. method according to claim 1, is characterized in that, described step 1) in aluminum oxide with the ramp of 225-235 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 145-155 DEG C.
5. method according to claim 1, is characterized in that, described step 1) in aluminum oxide with the ramp of 255-265 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 125-145 DEG C.
6. method according to claim 1, is characterized in that, described step 1) in aluminum oxide with the ramp of 235-245 DEG C/h to 800-950 DEG C, after reach 1200-1220 DEG C with the ramp of 115-125 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510084063.4A CN104787786A (en) | 2015-02-16 | 2015-02-16 | Alpha-alumina preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510084063.4A CN104787786A (en) | 2015-02-16 | 2015-02-16 | Alpha-alumina preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN104787786A true CN104787786A (en) | 2015-07-22 |
Family
ID=53553039
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510084063.4A Pending CN104787786A (en) | 2015-02-16 | 2015-02-16 | Alpha-alumina preparation method |
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| Country | Link |
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| CN (1) | CN104787786A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439283A (en) * | 2018-11-02 | 2019-03-08 | 长沙县新光特种陶瓷有限公司 | A kind of polishing preparation method of alumina powder |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4818515A (en) * | 1985-01-18 | 1989-04-04 | Montedison S.P.A. | Alpha-alumina in the form of spherical non-aggregated particles having a narrow size distribution and sizes below 2 microns and process for preparing same |
| CN1316382A (en) * | 2000-04-04 | 2001-10-10 | 韩嵬 | Process for preparing high-purity superfine alumina powder by aluminium alkoxide hydrolysis |
| JP2004123445A (en) * | 2002-10-02 | 2004-04-22 | Sumitomo Chem Co Ltd | Alpha-alumina powder and method of manufacturing the same |
| US20050008565A1 (en) * | 2003-05-19 | 2005-01-13 | Sumitomo Chemical Company, Limited | Method for producing alpha-alumina powder |
| CN101575110A (en) * | 2008-05-09 | 2009-11-11 | 大连路明纳米材料有限公司 | Preparation method of alumina powder |
| US20100166642A1 (en) * | 2008-12-25 | 2010-07-01 | Sumitomo Chemical Company, Limited | Method for producing alumina |
| CN101863501A (en) * | 2010-04-27 | 2010-10-20 | 中国神华能源股份有限公司 | Method for producing superfine aluminum hydroxide and aluminum oxide by using solution of aluminum chloride |
-
2015
- 2015-02-16 CN CN201510084063.4A patent/CN104787786A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4818515A (en) * | 1985-01-18 | 1989-04-04 | Montedison S.P.A. | Alpha-alumina in the form of spherical non-aggregated particles having a narrow size distribution and sizes below 2 microns and process for preparing same |
| CN1316382A (en) * | 2000-04-04 | 2001-10-10 | 韩嵬 | Process for preparing high-purity superfine alumina powder by aluminium alkoxide hydrolysis |
| JP2004123445A (en) * | 2002-10-02 | 2004-04-22 | Sumitomo Chem Co Ltd | Alpha-alumina powder and method of manufacturing the same |
| US20050008565A1 (en) * | 2003-05-19 | 2005-01-13 | Sumitomo Chemical Company, Limited | Method for producing alpha-alumina powder |
| CN101575110A (en) * | 2008-05-09 | 2009-11-11 | 大连路明纳米材料有限公司 | Preparation method of alumina powder |
| US20100166642A1 (en) * | 2008-12-25 | 2010-07-01 | Sumitomo Chemical Company, Limited | Method for producing alumina |
| CN101863501A (en) * | 2010-04-27 | 2010-10-20 | 中国神华能源股份有限公司 | Method for producing superfine aluminum hydroxide and aluminum oxide by using solution of aluminum chloride |
Non-Patent Citations (3)
| Title |
|---|
| 刘宗昌等编: "《材料组织结构转变原料》", 30 September 2006, article "10.1.2氧化铝的晶型转变", pages: 270-271 * |
| 刘志强: "高纯超细氧化铝粉的制备(Ⅱ)—煅烧过程对氧化铝粉性能的影响", 《广东有色金属学报》, vol. 12, no. 2, 30 November 2002 (2002-11-30), pages 99 - 101 * |
| 杨重愚主编: "《氧化铝生产工艺学》", 31 October 1993, article "氢氧化铝的煅烧", pages: 141-142 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439283A (en) * | 2018-11-02 | 2019-03-08 | 长沙县新光特种陶瓷有限公司 | A kind of polishing preparation method of alumina powder |
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Owner name: LIU GUANHUA Free format text: FORMER OWNER: QINGDAO SHENGNUO OPTOELECTRONIC TECHNOLOGY CO., LTD. Effective date: 20150702 |
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Effective date of registration: 20150702 Address after: 810000 Qinghai Province, Xining City District Nanchuan Industrial Park Industrial Road No. 8 Applicant after: Liu Guanhua Address before: 810000 Qinghai Province, Xining City District Nanchuan Industrial Park Industrial Road No. 8 Applicant before: SHENGNUO OPTOELECTRONIC TECHNOLOGY (QH) Co.,Ltd. |
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Application publication date: 20150722 |