CN104140118A - A producing method of high-purity aluminium oxide - Google Patents
A producing method of high-purity aluminium oxide Download PDFInfo
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- CN104140118A CN104140118A CN201310162168.8A CN201310162168A CN104140118A CN 104140118 A CN104140118 A CN 104140118A CN 201310162168 A CN201310162168 A CN 201310162168A CN 104140118 A CN104140118 A CN 104140118A
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- Prior art keywords
- aluminium oxide
- sodium aluminate
- aluminate solution
- production method
- high purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A producing method of high-purity aluminium oxide is disclosed. The method includes following steps of: 1) reacting aluminium hydroxide and caustic soda flakes into a sodium metaaluminate solution; 2) purifying the sodium metaaluminate solution to remove impurity ions in the sodium metaaluminate solution; 3) diluting; 4) adding a polymer dispersing agent; 5) feeding CO2 gas, heating and stirring; 6) washing the aluminium hydroxide to remove sodium ion in the powder; 7) performing a hydrothermal reaction; and 8) drying and calcinating. Compared with the prior art, the aluminium oxide produced by the method has characteristics of good dispersibility, small granularity and narrow distribution. The crystal structure of the high-purity aluminium oxide is spherical.
Description
Technical field
The present invention relates to a kind of production method of high purity aluminium oxide.The aluminum oxide that the method is produced is mainly used in the fields such as LED fluorescent material, PDP fluorescent material, three primary colors fluorescent powder and electronic material.
Background technology
Be applied at present the high purity aluminium oxide in the fields such as LED fluorescent material, PDP fluorescent material, three primary colors fluorescent powder and electronic material mainly with choline hydrolysis method, metallic aluminium hydrolysis method, exsiccated ammonium alum method, the pattern of the aluminum oxide of producing with aforesaid method is mainly sheet, needle-like, cotton-shaped,, low lightness poor with the fluorescent material pattern of above-mentioned power production, dispersed bad easy reunion, make that optical throughput is little after light fixture, light decay is fast, and aforesaid method cost is high, big for environment pollution.
Summary of the invention
Object of the present invention is just to provide a kind of production method of high purity aluminium oxide, aluminum oxide small grain size, high dispersive, narrowly distributing that the production method of this high purity aluminium oxide is produced, and crystalline structure is spherical.
Technical scheme of the present invention is: a kind of production method of high purity aluminium oxide, comprises the following steps: 1) aluminium hydroxide and sheet alkali reaction generate sodium aluminate solution; 2) purification sodium aluminate solution, removes the foreign ion in sodium aluminate solution; 3) dilution; 4) add macromolecule dispersing agent; 5) heated and stirred, passes into CO
2gas; 6) washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide; 7) hydro-thermal reaction; 8) dry, calcining.
As preferably, the reaction conditions that described aluminium hydroxide and sheet alkali reaction generate sodium aluminate solution is: aluminium hydroxide, sheet base molecule ratio=1.4-1.6, temperature is 140-150 ℃, reaction times 2h.
As preferably, described method of purification is: adopt desiliconization agent to carry out two sections of deep desilications, adopt tiny aluminium hydroxide for kind of a minute crystal seed, corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
As preferably, described dilution is for to be diluted to 50-80g/L by sodium aluminate solution.
As preferably, described macromolecule dispersing agent is acrylate and/or maleic acid ester.
As preferably, described macromolecule dispersing agent add-on be in sodium aluminate solution alumina content be 1-5%.
As preferably, CO in described step 5)
2flow is 0.8-1.2t/h, temperature 60-80 ℃, and mixing speed 400-600r/min, the reaction times is 200-300min, decomposing terminal is controlled at 80%-95%.
As preferably, Na2O≤0.2% after described step 6) washing.
As preferably, described hydro-thermal reaction is carried out in autoclave, adds sodium removing agent during reaction, and reaction conditions is that temperature is 120-130 degree, and pressure is 0.2-0.5Mpa, and the reaction times is 6-8 hour.
As preferably, Na before described step 8) is dry
2o≤0.002%; Moisture≤3% before calcining, calcining is calcined in high temperature electrical kiln, calcining temperature 1000-1200 degree.
Compared with prior art, beneficial effect of the present invention is: it is spherical adopting the high purity aluminium oxide pattern that the production method of the present invention's protection is produced, and size-grade distribution is good, good dispersity, produce fluorescent material pattern and be spherical, brightness is high, light decay is little, coating property is good.
explanation of nouns
Two sections of deep desilication methods-refer to are pressurizeed after desiliconization and are added calcium hydroxide to carry out normal pressure deep desilication with calcium aluminate.
In the present invention, if no special instructions, % refers to mass percent.
Embodiment
A production method for high purity aluminium oxide, comprises the steps:
1, by aluminium hydroxide, sheet alkali, carry out proportioning according to molecular ratio=1.5 ± 0.1, add pure water, temperature is 145 ± 5 ℃, and reaction times 2h carries out chemical reaction, generates sodium aluminate solution, and concrete reaction equation is:
Al(OH)
3 + Na OH=Na AlO
2+H
2O。
2, adopt desiliconization agent calcium aluminate and calcium hydroxide to carry out two sections of deep desilications, adopt tiny aluminium hydroxide for kind of a minute crystal seed, corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
3, dilution sodium aluminate solution is to 50-80g/L.
4, in the sodium aluminate solution after dilution, add one or both mixtures in macromolecule dispersing agent acrylate, maleic acid ester, add-on be in sodium aluminate solution alumina content for 1-5%.
5, pass into fast CO
2gas, CO
2flow is 0.8-1.2t/h, temperature 60-80 ℃, and mixing speed 400-600r/min, the time is 200-300min, obtains aluminium hydroxide, reaction equation is:
NaAlO
2 + CO
2 + H
20 = Al（OH）
3↓ + Na
2CO
3
Rate of decomposition is controlled at 80%-95%.
6, washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide, washs to Na
2o≤0.2%;
7, by washing after aluminium hydroxide according to the ratio furnishing slip of material-water ratio=1:5, with pump, be pumped in reactor, add sodium removing agent, then in high-pressure reactor, carry out hydro-thermal reaction, controlling temperature is 120-130 degree, and pressure is 0.2-0.5Mpa, and the reaction times is to be 6-8 hour in the reaction times.And then wash Na 2-3 time
2o≤0.002%.
8, dry, remove the moisture in powder, make moisture≤3%.
9, calcining: calcine in high temperature electrical kiln, calcining temperature is 1100-1200 ℃.
Experiment 1
Aluminium hydroxide, sheet alkali are prepared burden according to molecular ratio=1.5 ± 0.1, add pure water, and then in 145 ± 5 ℃ of reactions of temperature, reaction times 2h, generates sodium aluminate solution and dissolve rear Al
2o
3concentration is 150g/L.
Detect the silicon-dioxide in sodium aluminate solution, after detection, according to detected silica concentration, add the calcium aluminate desiliconization of pressurizeing in sodium aluminate solution, add-on is Ca (AlO
2)
2(mol): SiO
2(mol)=50:1, adds calcium hydroxide to carry out normal pressure deep desilication, and add-on is Ca(OH)
2(mol): SiO
2(mol)=100:1, then adds tiny aluminium hydroxide (particle diameter is at 5-10um) to carry out as planting a minute crystal seed, and add-on is 100Kg, and corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
By the Al in sodium aluminate solution
2o
3concentration dilution is to 50g/L, to what add alumina content in sodium aluminate solution in this solution, is 3% acrylate, is heated with stirring to 60 ℃, and stir speed (S.S.) 400r/min, passes into CO
2gas, air flow is 0.8t/h, and the time is 200-300min, and decomposing terminal is controlled at 90%, with pure water, according to material-water ratio, be that 1:5 carries out 5 washings, then carry out hydro-thermal reaction, temperature of reaction is 120 ℃, and pressure is 0.2-0.5Mpa, time is 6h, then dry, 1100 ℃ of calcinings.
Experiment 2
Aluminium hydroxide, sheet alkali are prepared burden according to molecular ratio=1.5 ± 0.1, add pure water, and then in 145 ± 5 ℃ of reactions of temperature, reaction times 2h, generates sodium aluminate solution and dissolve rear AL
2o
3concentration is 150g/L.
Detect the silicon-dioxide in sodium aluminate solution, after detection, according to detected silica concentration, add the calcium aluminate desiliconization of pressurizeing in sodium aluminate solution, add-on is Ca (AlO
2)
2(mol): SiO
2(mol)=50:1, adds calcium hydroxide to carry out normal pressure deep desilication, and add-on is Ca(OH)
2(mol): SiO
2(mol)=100:1, then adds tiny aluminium hydroxide (particle diameter is at 5-10um) to carry out as planting a minute crystal seed, and add-on is 100Kg, and corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
By the AL in sodium aluminate solution
2o
3concentration dilution is to 50g/L, to what add alumina content in sodium aluminate solution in this solution, is 3% maleic acid ester, is heated with stirring to 60 ℃, and stir speed (S.S.) 400r/min, passes into CO
2gas, air flow is 1.0t/h, and the time is 200-300min, and decomposing terminal is controlled at 90%, with pure water, according to material-water ratio, be that 1:5 carries out 5 washings, then carry out hydro-thermal reaction, temperature of reaction is 120 ℃, and pressure is 0.2-0.5Mpa, time is 6 hours, then dry, in 1100 calcinings.
Experiment 3
Aluminium hydroxide, sheet alkali are prepared burden according to molecular ratio=1.5 ± 0.1, add pure water, then in 145 ± 5 ℃ of reactions of temperature, and reaction times 2h, generating the rear AL2O3 concentration of sodium aluminate solution dissolving is 150g/L.
Detect the silicon-dioxide in sodium aluminate solution, after detection, according to detected silica concentration, add the calcium aluminate desiliconization of pressurizeing in sodium aluminate solution, add-on is Ca (AlO
2)
2(mol): SiO
2(mol)=50:1, adds calcium hydroxide to carry out normal pressure deep desilication, and add-on is Ca(OH)
2(mol): SiO
2(mol)=100:1, then adds tiny aluminium hydroxide (particle diameter is at 5-10um) to carry out as planting a minute crystal seed, and add-on is 100Kg, and corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
By the Al in sodium aluminate solution
2o
3concentration dilution is to 60g/L, to what add alumina content in sodium aluminate solution in this solution, is 3% maleic acid ester and acrylate mixture, is heated with stirring to 60 ℃, and stir speed (S.S.) 400r/min, passes into CO
2gas, air flow is 1.2t/h, and the time is 200-300min, and decomposing terminal is controlled at 90%, with pure water, according to material-water ratio, be that 1:5 carries out 5 washings, then carry out hydro-thermal reaction, temperature of reaction is 120 degree, and pressure is 0.2-0.5Mpa, time is 6h, then dry, 1100 ℃ of calcinings.
Experiment 4
Aluminium hydroxide, sheet alkali are prepared burden according to molecular ratio=1.5 ± 0.1, add pure water, then in 145 ± 5 ℃ of reactions of temperature, and reaction times 2h, generating the rear AL2O3 concentration of sodium aluminate solution dissolving is 150g/L.
Detect the silicon-dioxide in sodium aluminate solution, after detection, according to detected silica concentration, add the calcium aluminate desiliconization of pressurizeing in sodium aluminate solution, add-on is Ca (AlO
2)
2(mol): SiO
2(mol)=50:1, adds calcium hydroxide to carry out normal pressure deep desilication, and add-on is Ca(OH)
2(mol): SiO
2(mol)=100:1, then adds tiny aluminium hydroxide (particle diameter is at 5-10um) to carry out as planting a minute crystal seed, and add-on is 100Kg, and corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
By the AL in sodium aluminate solution
2o
3concentration dilution is to 90g/L, to what add alumina content in sodium aluminate solution in this solution, is 3% maleic acid ester and acrylate mixture, is heated with stirring to 80 ℃, and stir speed (S.S.) 500r/min, passes into CO
2gas, air flow is 0.8t/h, and the time is 200-300min, and decomposing terminal is controlled at 90%, with pure water, according to material-water ratio, be that 1:5 carries out 5 washings, then carry out hydro-thermal reaction, temperature of reaction is 120 degree, and pressure is 0.2-0.5Mpa, time is 6 hours, then dry, 1100 ℃ of calcinings.
Experiment 5
Aluminium hydroxide, sheet alkali are prepared burden according to molecular ratio=1.5 ± 0.1, add pure water, and then in 145 ± 5 ℃ of reactions of temperature, reaction times 2h, generates sodium aluminate solution and dissolve rear AL
2o
3concentration is 150g/L.
Detect the silicon-dioxide in sodium aluminate solution, after detection, according to detected silica concentration, add the calcium aluminate desiliconization of pressurizeing in sodium aluminate solution, add-on is Ca (AlO
2)
2(mol): SiO
2(mol)=50:1, adds calcium hydroxide to carry out normal pressure deep desilication, and add-on is Ca(OH)
2(mol): SiO
2(mol)=100:1, then adds tiny aluminium hydroxide (particle diameter is at 5-10um) to carry out as planting a minute crystal seed, and add-on is 100Kg, and corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
By the AL in sodium aluminate solution
2o
3concentration dilution is to 90g/L, to what add alumina content in sodium aluminate solution in this solution, is 3% maleic acid ester and acrylate mixture, is heated with stirring to 80 ℃, and stir speed (S.S.) 500r/min, passes into CO
2gas, air flow is 1.2t/h, and the time is 200-300min, and decomposing terminal is controlled at 90%, with pure water, according to material-water ratio, be that 1:5 carries out 5 washings, then carry out hydro-thermal reaction, temperature of reaction is 120 ℃, and pressure is 0.2-0.5Mpa, time is 6 hours, then dry, 1100 ℃ of calcinings.
Claims (10)
1. a production method for high purity aluminium oxide, comprises the following steps:
1) aluminium hydroxide and sheet alkali reaction generate sodium aluminate solution;
2) purification sodium aluminate solution, removes the foreign ion in sodium aluminate solution;
3) dilution;
4) add macromolecule dispersing agent;
5) heated and stirred, passes into CO
2gas;
6) washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide;
7) hydro-thermal reaction;
8) dry, calcining.
2. the production method of high purity aluminium oxide according to claim 1, it is characterized in that: the reaction conditions that described aluminium hydroxide and sheet alkali reaction generate sodium aluminate solution is: aluminium hydroxide, sheet base molecule ratio=1.4-1.6, temperature is 140-150 ℃, reaction times 2h.
3. the production method of high purity aluminium oxide according to claim 1, it is characterized in that: described method of purification is: adopt desiliconization agent to carry out two sections of deep desilications, adopt tiny aluminium hydroxide for kind of a minute crystal seed, corrosion is controlled at 4-6%, then filters to remove the metal ions such as iron in sodium aluminate solution, calcium, copper.
4. the production method of high purity aluminium oxide according to claim 1, is characterized in that: described dilution is for to be diluted to 50-80g/L by sodium aluminate solution.
5. the production method of high purity aluminium oxide according to claim 1, is characterized in that: described macromolecule dispersing agent is acrylate and/or maleic acid ester.
6. the production method of high purity aluminium oxide according to claim 1, is characterized in that: described macromolecule dispersing agent add-on be in sodium aluminate solution alumina content be 1-5%.
7. the production method of high purity aluminium oxide according to claim 1, is characterized in that: CO in described step 5)
2flow is 0.8-1.2t/h, temperature 60-80 ℃, and mixing speed 400-600r/min, the reaction times is 200-300min, decomposing terminal is controlled at 80%-95%.
8. the production method of high purity aluminium oxide according to claim 1, is characterized in that: Na after described step 6) washing
2o≤0.2%.
9. the production method of high purity aluminium oxide according to claim 1, it is characterized in that: described hydro-thermal reaction is carried out in autoclave, add sodium removing agent during reaction, reaction conditions is that temperature is 120-130 degree, pressure is 0.2-0.5Mpa, and the reaction times is 6-8 hour.
10. the production method of high purity aluminium oxide according to claim 1, is characterized in that: Na before described step 8) is dry
2o≤0.002%; Moisture≤3% before calcining, calcining is calcined in high temperature electrical kiln, calcining temperature 1000-1200 degree.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724740A (en) * | 2015-03-20 | 2015-06-24 | 河南能源化工集团研究院有限公司 | Preparation method of high-purity ultra-fine aluminum hydroxide powder |
| CN108423699A (en) * | 2018-04-20 | 2018-08-21 | 淄博鹏丰铝业有限公司 | A kind of preparation method of lithium battery diaphragm coated by special aluminium oxide |
| CN109553121A (en) * | 2018-12-24 | 2019-04-02 | 中铝山东有限公司 | A kind of preparation method of high-purity low-sodium aluminum hydroxide |
| CN112777620A (en) * | 2021-01-29 | 2021-05-11 | 哈尔滨工业大学（威海） | Method for recycling aluminum ash or aluminum slag by using alkaline leaching method |
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| CN1485274A (en) * | 2003-09-02 | 2004-03-31 | 中国铝业股份有限公司 | Sintering process for preparing sand-shape alumina |
| CN1559905A (en) * | 2004-03-04 | 2005-01-05 | 重庆同泰粉体科技有限公司 | Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide |
| CN102491386A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Method for improving silica modulus of purified liquid obtained by Bayer process |
| CN102583473A (en) * | 2012-02-16 | 2012-07-18 | 山东晶鑫晶体科技有限公司 | Production method of high-purity aluminum oxide |
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2013
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| JPH06171929A (en) * | 1992-12-02 | 1994-06-21 | Sumitomo Chem Co Ltd | Production of white aluminum hydroxide |
| CN1485274A (en) * | 2003-09-02 | 2004-03-31 | 中国铝业股份有限公司 | Sintering process for preparing sand-shape alumina |
| CN1559905A (en) * | 2004-03-04 | 2005-01-05 | 重庆同泰粉体科技有限公司 | Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide |
| CN102491386A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Method for improving silica modulus of purified liquid obtained by Bayer process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724740A (en) * | 2015-03-20 | 2015-06-24 | 河南能源化工集团研究院有限公司 | Preparation method of high-purity ultra-fine aluminum hydroxide powder |
| CN108423699A (en) * | 2018-04-20 | 2018-08-21 | 淄博鹏丰铝业有限公司 | A kind of preparation method of lithium battery diaphragm coated by special aluminium oxide |
| CN108423699B (en) * | 2018-04-20 | 2020-01-07 | 淄博鹏丰铝业有限公司 | Preparation method of lithium battery diaphragm coated with special alumina |
| CN109553121A (en) * | 2018-12-24 | 2019-04-02 | 中铝山东有限公司 | A kind of preparation method of high-purity low-sodium aluminum hydroxide |
| CN109553121B (en) * | 2018-12-24 | 2021-06-08 | 中铝山东有限公司 | Preparation method of high-purity low-sodium aluminum hydroxide |
| CN112777620A (en) * | 2021-01-29 | 2021-05-11 | 哈尔滨工业大学（威海） | Method for recycling aluminum ash or aluminum slag by using alkaline leaching method |
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