CN106915755A - A kind of preparation method of high-purity alpha-alumina - Google Patents
A kind of preparation method of high-purity alpha-alumina Download PDFInfo
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- CN106915755A CN106915755A CN201510987036.8A CN201510987036A CN106915755A CN 106915755 A CN106915755 A CN 106915755A CN 201510987036 A CN201510987036 A CN 201510987036A CN 106915755 A CN106915755 A CN 106915755A
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- preparation
- aluminate solution
- reaction
- sodium aluminate
- purity alpha
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of preparation method of high-purity alpha-alumina, it is comprised the following steps：A. aluminium hydroxide generates sodium aluminate solution with the reaction of piece alkali；B. sodium aluminate solution is purified, the foreign ion in sodium aluminate solution is removed；C. dilute；D. macromolecule dispersing agent is added；E. heating stirring, is passed through CO2 gases；F. washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide；G. hydro-thermal reaction；H. dry, calcine.Use the high-purity alpha-alumina aluminium pattern of present invention production for spherical, size distribution is good, good dispersion, not only make that luminous flux after light fixture is big, light decay slowly, and this method low cost, environmental pollution is small.
Description
Technical field
Technical field is prepared the present invention relates to alumina powder, a kind of preparation method of high-purity alpha-alumina is particularly related to.
Background technology
The high purity aluminium oxide for being applied to the field such as electronic material and LED fluorescent powder, PDP fluorescent material, three primary colors fluorescent powder at present is main with choline Hydrolyze method, metallic aluminium Hydrolyze method, alum method, the pattern of the aluminum oxide for producing in aforementioned manners mainly sheet, needle-like, cotton-shaped, using the fluorescent material pattern of above-mentioned power production it is poor, brightness is low, poor dispersion is easily reunited, not only make that luminous flux after light fixture is small, light decay is fast, and above method high cost, it is big for environment pollution.
The content of the invention
The purpose of the present invention is that and provides a kind of preparation method of high-purity alpha-alumina, effectively to overcome above-mentioned the deficiencies in the prior art.
To achieve these goals, the technical solution adopted by the present invention is：A kind of preparation method of high-purity alpha-alumina, it is comprised the following steps：A. aluminium hydroxide generates sodium aluminate solution with the reaction of piece alkali；B. sodium aluminate solution is purified, the foreign ion in sodium aluminate solution is removed；C. dilute；D. macromolecule dispersing agent is added；E. heating stirring, is passed through CO2 gases；F. washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide；G. hydro-thermal reaction；H. dry, calcine.
Preferably, the aluminium hydroxide and the reaction condition of piece alkali reaction generation sodium aluminate solution are aluminium hydroxide：Piece base molecule is 1.4：1.6, its reaction temperature is 140~150 DEG C, reaction time 2h.
Preferably, the method for purification is to carry out two sections of deep desilications using desiliconization agent, and it is kind of a point crystal seed to use tiny aluminium hydroxide, and corrosion controls 4~6%, filters to remove the metal ions such as the iron in sodium aluminate solution, calcium, copper afterwards.
Preferably, it is described to be diluted to for sodium aluminate solution to be diluted to 50~80g/L.
Preferably, the macromolecule dispersing agent is acrylate or maleate, and its macromolecule dispersing agent addition is 1~5% of alumina content in sodium aluminate solution.
In the step e CO2 flows be 0.8~1.2t/h, 60~80 DEG C of temperature, 400~600r/min of speed of agitator, the reaction time be 200~300min, decomposing terminal control 80~95%.
Preferably, Na2O is less than or equal to 0.2% after the step f washings.
Preferably, the hydro-thermal reaction is carried out in autoclave, and sodium removing agent is added during reaction, and reaction condition is that temperature is 120~130 degree, and pressure is 0.2~0.5Mpa, and the reaction time is 6~8h.
Preferably, Na2O is less than or equal to 0.002% before the step h is dried；Moisture is less than or equal to 3% before calcining, and calcining is calcined in high temperature electrical kiln, 1000~1200 degree of calcining heat.
Compared with prior art, the beneficial effects of the invention are as follows：Use the high-purity alpha-alumina aluminium pattern of present invention production for spherical, size distribution is good, good dispersion, not only make that luminous flux after light fixture is big, light decay slowly, and this method low cost, environmental pollution is small.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
A kind of preparation method of high-purity alpha-alumina, it is comprised the following steps：A. aluminium hydroxide generates sodium aluminate solution with the reaction of piece alkali；B. sodium aluminate solution is purified, the foreign ion in sodium aluminate solution is removed；C. dilute；D. macromolecule dispersing agent is added；E. heating stirring, is passed through CO2 gases；F. washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide；G. hydro-thermal reaction；H. dry, calcine.
The aluminium hydroxide is aluminium hydroxide with the reaction condition of piece alkali reaction generation sodium aluminate solution：Piece base molecule is 1.4：1.6, its reaction temperature is 145 DEG C, reaction time 2h.
The method of purification is to carry out two sections of deep desilications using desiliconization agent, and it is kind of a point crystal seed to use tiny aluminium hydroxide, and corrosion controls 5%, filters to remove the metal ions such as the iron in sodium aluminate solution, calcium, copper afterwards.
It is described to be diluted to for sodium aluminate solution to be diluted to 70g/L.
The macromolecule dispersing agent is acrylate or maleate, and its macromolecule dispersing agent addition is 3% of alumina content in sodium aluminate solution.
CO2 flows are 1.0t/h in the step e, temperature 70 C, speed of agitator 500r/min, and the reaction time is 260min, and decomposing terminal is controlled 90%.
Na2O is less than or equal to 0.2% after the step f washings.
The hydro-thermal reaction is carried out in autoclave, and sodium removing agent is added during reaction, and reaction condition is that temperature is 125 degree, and pressure is 0.4Mpa, and the reaction time is 7h.
Na2O is less than or equal to 0.002% before the step h is dried；Moisture is less than or equal to 3% before calcining, and calcining is calcined in high temperature electrical kiln, 1100 degree of calcining heat.
Above are only a kind of embodiment of the invention; it is not intended to limit the invention; those skilled in the art can make various changes and improve to said structure, all any modification equivalents made within the spirit and principles in the present invention and improvement, should be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of high-purity alpha-alumina, it is characterised in that：It is comprised the following steps：
A. aluminium hydroxide generates sodium aluminate solution with the reaction of piece alkali；
B. sodium aluminate solution is purified, the foreign ion in sodium aluminate solution is removed；
C. dilute；
D. macromolecule dispersing agent is added；
E. heating stirring, is passed through CO2 gases；
F. washing aluminum hydroxide, removes the free sodium ion in aluminium hydroxide；
G. hydro-thermal reaction；
H. dry, calcine.
2. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：The aluminium hydroxide is aluminium hydroxide with the reaction condition of piece alkali reaction generation sodium aluminate solution：Piece base molecule is 1.4：1.6, its reaction temperature is 140~150 DEG C, reaction time 2h.
3. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：The method of purification is to carry out two sections of deep desilications using desiliconization agent, and it is kind of a point crystal seed to use tiny aluminium hydroxide, and corrosion controls 4~6%, filters to remove the metal ions such as the iron in sodium aluminate solution, calcium, copper afterwards.
4. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：It is described to be diluted to for sodium aluminate solution to be diluted to 50~80g/L.
5. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：The macromolecule dispersing agent is acrylate or maleate, and its macromolecule dispersing agent addition is 1~5% of alumina content in sodium aluminate solution.
6. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：In the step e CO2 flows be 0.8~1.2t/h, 60~80 DEG C of temperature, 400~600r/min of speed of agitator, the reaction time be 200~300min, decomposing terminal control 80~95%.
7. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：Na2O is less than or equal to 0.2% after the step f washings.
8. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：The hydro-thermal reaction is carried out in autoclave, and sodium removing agent is added during reaction, and reaction condition is that temperature is 120~130 degree, and pressure is 0.2~0.5Mpa, and the reaction time is 6~8h.
9. the preparation method of a kind of high-purity alpha-alumina according to claim 1, it is characterised in that：Na2O is less than or equal to 0.002% before the step h is dried；Moisture is less than or equal to 3% before calcining, and calcining is calcined in high temperature electrical kiln, 1000~1200 degree of calcining heat.
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| CN201510987036.8A CN106915755A (en) | 2015-12-27 | 2015-12-27 | A kind of preparation method of high-purity alpha-alumina |
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| CN201510987036.8A CN106915755A (en) | 2015-12-27 | 2015-12-27 | A kind of preparation method of high-purity alpha-alumina |
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| CN106915755A true CN106915755A (en) | 2017-07-04 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109052442A (en) * | 2018-10-18 | 2018-12-21 | 中铝山东有限公司 | A kind of production method of electron level high heat resistance aluminium hydroxide |
| CN109368675A (en) * | 2018-12-10 | 2019-02-22 | 贵州博汇联润铝业有限公司 | A kind of ultra-fine ultrawhite aluminum hydroxide micro mist removes sodium purification method |
| 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 |
| CN109761254A (en) * | 2019-02-02 | 2019-05-17 | 中国铝业股份有限公司 | A method of reducing aluminium hydroxide or sodium oxide in aluminum oxide impurity content |
| CN110407240A (en) * | 2019-08-29 | 2019-11-05 | 昆明冶金研究院 | A kind of preparation method of modified aluminas |
| CN110697747A (en) * | 2019-12-03 | 2020-01-17 | 山东齐鲁华信实业股份有限公司 | High-efficiency production method of low-caustic-ratio sodium metaaluminate solution |
-
2015
- 2015-12-27 CN CN201510987036.8A patent/CN106915755A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109052442A (en) * | 2018-10-18 | 2018-12-21 | 中铝山东有限公司 | A kind of production method of electron level high heat resistance aluminium hydroxide |
| CN109052442B (en) * | 2018-10-18 | 2021-04-13 | 中铝山东有限公司 | Production method of electronic grade high heat-resistant aluminum hydroxide |
| CN109368675A (en) * | 2018-12-10 | 2019-02-22 | 贵州博汇联润铝业有限公司 | A kind of ultra-fine ultrawhite aluminum hydroxide micro mist removes sodium purification method |
| 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 |
| CN109761254A (en) * | 2019-02-02 | 2019-05-17 | 中国铝业股份有限公司 | A method of reducing aluminium hydroxide or sodium oxide in aluminum oxide impurity content |
| CN110407240A (en) * | 2019-08-29 | 2019-11-05 | 昆明冶金研究院 | A kind of preparation method of modified aluminas |
| CN110697747A (en) * | 2019-12-03 | 2020-01-17 | 山东齐鲁华信实业股份有限公司 | High-efficiency production method of low-caustic-ratio sodium metaaluminate solution |
| CN110697747B (en) * | 2019-12-03 | 2022-05-13 | 山东齐鲁华信实业股份有限公司 | High-efficiency production method of low-caustic-ratio sodium metaaluminate solution |
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Application publication date: 20170704 |