CN103232049A - Preparation method of alpha-Al2O3 cage-structure hollow microspheres - Google Patents
Preparation method of alpha-Al2O3 cage-structure hollow microspheres Download PDFInfo
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- CN103232049A CN103232049A CN2013100847846A CN201310084784A CN103232049A CN 103232049 A CN103232049 A CN 103232049A CN 2013100847846 A CN2013100847846 A CN 2013100847846A CN 201310084784 A CN201310084784 A CN 201310084784A CN 103232049 A CN103232049 A CN 103232049A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000004005 microsphere Substances 0.000 title abstract 7
- 229910052594 sapphire Inorganic materials 0.000 title abstract 5
- 229910002706 AlOOH Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012429 reaction media Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000000877 morphologic effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 description 1
- 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 1
- 238000010923 batch production Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 206010016256 fatigue Diseases 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- -1 pottery Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
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Abstract
The invention provides a preparation method of alpha-Al2O3 cage-structure hollow microspheres. The preparation method comprises the following steps that KAl(SO4)2.12H2O as an aluminum source and urea as a precipitator undergo a reaction under the hydrothermal conditions; the products are subjected to centrifugal washing and drying to form precursor AlOOH microspheres having structured and controllable morphology; and the dried precursor AlOOH microspheres having hierarchical structures are put into a muffle furnace, are heated to a temperature of 1300 to 1400 DEG C at a certain heating rate and then are subjected to heat preservation for 1 to 4h so that AlOOH is decomposed and the alpha-Al2O3 cage-structure hollow microspheres are obtained by phase transition. The alpha-Al2O3 cage-structure hollow microspheres have novel structures. Sizes, morphology, structures and an assembling mode of the AlOOH microspheres having hierarchical structures and the alpha-Al2O3 cage structure are controllable. The reaction system adopted by the preparation method utilizes water as a reaction medium. The preparation method adopts the cheap raw materials and has simple processes.
Description
Technical field
The invention belongs to the inorganic functional material field, relate to a kind of α-Al
2O
3The preparation method of powder specifically, relates to a kind of α-Al
2O
3The preparation method of cage structure tiny balloon.
Background technology
α-Al
2O
3Thermotolerance is strong, good moldability, crystalline phase is stable, the hardness height, the strengthening and toughening that can be widely used in products such as various plastics, rubber, pottery, refractory materials, the particularly wear resisting property of compactness, smooth finish, cold and hot fatigability, fracture toughness property, creep-resistant property and the macromolecular material product of raising pottery.In addition, alpha-phase aluminum oxide resistivity height has the good insulation performance performance, nanometer Al
2O
3Be added to and prepare nano composite material in the polymkeric substance and at electric field important use is arranged, can improve polymer materials to a certain extent in the performance of aspects such as disruptive strength, volume specific resistance, dielectric properties and the aging resistance of anti-the corona.The performance of aluminum oxide/polymer composites not only depends on Al to a great extent
2O
3The size of particulate also depends on Al
2O
3The shape of particle with and assembling morphology and microstructure.Therefore, various morphological structures and different size, jljl Al mutually not
2O
3The preparation of powder becomes the research focus.Lot of documents has been reported Al
2O
3The nanometer Al of nanoparticle and one dimension, two-dimentional yardstick
2O
3Preparation.
The hollow ball structure aluminum oxide has the character of better uniqueness than other microstructures.Synthetic report about alumina hollow ball all adopts template at present, is template with charcoal particle, PS emulsion particle, metallic aluminium powder etc., by Al (OH)
3Coat and form the nucleocapsid structure microballoon, remove the template kernel under the high temperature, form alumina hollow ball.Patent of invention CN201010217412.2 has announced a kind of aluminum oxide tiny balloon preparation method, and 1000 ℃ are incubated 1 hour in vacuum sintering furnace, and the levigate exsiccated ammonium alum powder that sieves acutely decomposes, and burns till the aluminum oxide tiny balloon.Be raw material with glucose and aluminum nitrate, the method that adopts first hydrothermal method to react calcination more also can prepare alumina hollow ball (Liao Hua etc. Chinese powder technology, 2010,16 (6): 14-17; Zhang Guangming etc. Beijing University of Chemical Technology's journal nature version, 2010,37 (4): 83-87).Prepared hollow ball is enclosed construction, and shell is thick.Patent of invention CN201010573994.8 discloses the method that a kind of spray burning prepares the porous nano alumina hollow ball.The method that the present invention then adopts hydro-thermal reaction to combine with roasting prepares by α-Al
2O
3The cage structure microballoon that nanoparticle and nanometer rod are built into.
Summary of the invention
The purpose of this invention is to provide a kind of α-Al
2O
3The preparation method of cage structure tiny balloon.This cage structure is by α-Al
2O
3Nanoparticle and nanometer rod are built into.Above-mentioned purpose of the present invention is to realize by following technological line and measure, at first prepares AlOOH hierarchy microballoon presoma, obtains α-Al by thermolysis with changing mutually again
2O
3Cage structure.Specifically:
1. the potassium aluminium sulfate crystal is dissolved in the solution that obtains 0.01～0.2 mol/L in the deionized water, adding urea then under stirring at room, to make its concentration be 0.05～1 mol/L, continues to stir 10 min it is dissolved fully, mixes to guarantee reactant;
2. above-mentioned mixed solution is transferred to and had in the teflon-lined stainless steel cauldron, sealing at 200 ℃ of 120-reaction 3～48 h down, obtains containing the mixed solution of AlOOH presoma;
3. after the above-mentioned mixed solution that contains the AlOOH presoma being cooled off, centrifugal 5-10 min outwells supernatant liquid under 2000-4000 r/min rotating speed, with throw out water and the ethanol repeated washing that obtains, it is dry to put into 60-80 ℃ of loft drier again, obtains precursor A lOOH hierarchy microballoon;
4. dry precursor AlOOH hierarchy microballoon is put into retort furnace, rise to 1300-1400 ℃ with the heat-up rate of 1～2 ℃/min, be incubated 1-4 h again, obtain α-Al
2O
3The tiny balloon of cage structure.
This operational path has following characteristics: the AlOOH hierarchy microballoon and the α-Al that obtain
2O
3Tiny balloon has cage structure, and the morphological structure novelty not only helps its novel dielectric properties of development research, to exploitation α-Al
2O
3The base novel functional materials is also significant.Simultaneously, this method technology is simple, and reaction conditions is gentle, prepared AlOOH hierarchy microballoon and α-Al
2O
3The size of cage structure, pattern, structure and assembling mode are controlled, and have the batch process feasibility; This reaction system is reaction medium with water, has avoided the use of organic solvent, is raw material with potassium aluminium sulfate and urea, saves cost in the actual production.
Description of drawings
Fig. 1 is the α-Al that utilizes the method for the invention preparation
2O
3Cage structure tiny balloon X-ray diffraction (XRD) collection of illustrative plates.
Fig. 2 is the α-Al that utilizes the method for the invention preparation
2O
3The scanning electronic microscope of cage structure tiny balloon (SEM) photo.
Embodiment
Below by specific embodiment the present invention is described in further detail, but content of the present invention has more than and is limited to described embodiment.
Embodiment one:
1. the potassium aluminium sulfate crystal is dissolved in the solution that obtains 0.05 mol/L in the deionized water, adding urea then under stirring at room, to make its concentration be 0.25 mol/L, continues to stir 10 min it is dissolved fully, mixes to guarantee reactant;
2. above-mentioned mixed solution is transferred to and had in the teflon-lined stainless steel cauldron, sealing at 180 ℃ of reaction 5 h down, obtains containing the mixed solution of AlOOH;
3. after the above-mentioned mixed solution that contains AlOOH being cooled off, centrifugal 5 min outwell supernatant liquid under 3000 r/min rotating speeds, and with throw out water and the ethanol repeated washing that obtains, it is dry to put into 60 ℃ of loft drier again, obtains AlOOH hierarchy microballoon;
4. the AlOOH hierarchy microballoon of drying is put into retort furnace, rise to 1350 ℃ with the heat-up rate of 1 ℃/min, be incubated 1 h, obtain α-Al
2O
3The hierarchy tiny balloon.
Embodiment two:
1. the potassium aluminium sulfate crystal is dissolved in the solution that obtains 0.05 mol/L in the deionized water, adding urea then under stirring at room, to make its concentration be 0.2 mol/L, continues to stir 10 min it is dissolved fully, mixes to guarantee reactant;
2. above-mentioned mixed solution is transferred to and had in the teflon-lined stainless steel cauldron, sealing at 150 ℃ of reaction 12 h down, obtains containing the mixed solution of AlOOH;
3. with after the above-mentioned mixed solution cooling, centrifugal 5 min outwell supernatant liquid under 4000 r/min rotating speeds, and with throw out water and the ethanol repeated washing that obtains, it is dry to put into 60 ℃ of loft drier again, obtains AlOOH hierarchy microballoon;
4. the AlOOH hierarchy microballoon of drying is put into retort furnace, rise to 1300 ℃ with the heat-up rate of 1 ℃/min, be incubated 1 h, obtain α-Al
2O
3The hierarchy tiny balloon.
Embodiment three:
1. the potassium aluminium sulfate crystal is dissolved in the solution that obtains 0.1 mol/L in the deionized water, adding urea then under stirring at room, to make its concentration be 0.5 mol/L, continues to stir 10 min it is dissolved fully, mixes to guarantee reactant;
2. above-mentioned mixed solution is transferred to and had in the teflon-lined stainless steel cauldron, sealing at 180 ℃ of reaction 5 h down, obtains containing the mixed solution of AlOOH;
3. with after the above-mentioned mixed solution cooling, centrifugal 5 min outwell supernatant liquid under 3000 r/min rotating speeds, and with throw out water and the ethanol repeated washing that obtains, it is dry to put into 60 ℃ of loft drier again, obtains AlOOH hierarchy microballoon;
4. the AlOOH hierarchy microballoon of drying is put into retort furnace, rise to 1350 ℃ with the heat-up rate of 1 ℃/min, be incubated 1 h, obtain α-Al
2O
3The hierarchy tiny balloon.
Fig. 1 is the Al that utilizes the embodiment of the invention one described method preparation
2O
3The X-ray diffraction of sample (XRD) collection of illustrative plates, all diffraction peaks among the figure can turn to α-Al according to standard card (card 83-2080) index
2O
3Diffraction peak, among the crystal indices of each diffraction peak correspondence mark and the figure, illustrate that the aluminum oxide that present method prepares is the α-Al of corundum structure
2O
3Sharp-pointed diffraction peak explanation α-Al
2O
3The sample well-crystallized.
Fig. 2 is the α-Al that utilizes the embodiment of the invention one described method preparation
2O
3Scanning electronic microscope under the sample different multiples (SEM) photo.From left figure as can be seen sample mainly be that microballoon by a large amount of 3-4 μ m sizes constitutes, size distribution is even.From right figure enlarged photograph α-Al as can be seen
2O
3Microballoon has cage structure, is by Al
2O
3Nanoparticle and nanometer rod are built into.
The above embodiment is preferred implementation of the present invention; but the specific embodiment of the present invention is not restricted to the described embodiments; do not deviate from other any change of doing under principle of the present invention and the technological process, substitute, simplification etc.; be the displacement of equivalence, all should be included within protection scope of the present invention.
Claims (5)
1. α-Al
2O
3The preparation method of cage structure tiny balloon is characterized in that, described method comprises the steps:
(1) potassium aluminium sulfate crystal and urea are added in the deionized water successively, stirring at room 10 min dissolve it fully, mix to guarantee reactant;
(2) above-mentioned mixed solution is transferred to had in the teflon-lined stainless steel cauldron, hydro-thermal reaction is carried out in sealing, obtains containing the mixed solution of AlOOH presoma;
(3) with after the above-mentioned mixed solution cooling that contains the AlOOH presoma, supernatant liquid is outwelled in centrifugation, and with throw out water and the ethanol repeated washing that obtains, it is dry to put into 60-80 ℃ of loft drier again, obtains precursor A lOOH hierarchy microballoon;
(4) dry precursor AlOOH hierarchy microballoon is put into retort furnace, roasting under the certain condition obtains α-Al
2O
3The tiny balloon of cage structure.
2. preparation method according to claim 1 is characterized in that, in the mixed solution of step (1), the concentration of potassium aluminium sulfate is 0.01～0.2 mol/L, and the concentration of urea is 0.05～1.0 mol/L.
3. preparation method according to claim 1 is characterized in that, in step (2), temperature of reaction is 120-200 ℃, and the reaction times is 3～48 h.
4. preparation method according to claim 1 is characterized in that, in step (3), centrifugation is centrifugal 5-10 min under 2000-4000 r/min rotating speed.
5. preparation method according to claim 1 is characterized in that, in step (4), retort furnace rises to 1300-1400 ℃ with the heat-up rate of 1～2 ℃/min, insulation 1-4 h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103432969A (en) * | 2013-09-09 | 2013-12-11 | 青岛科技大学 | Preparation method of alpha-Fe2O3/FeOOH core-shell structure composite microspheres |
| CN103446965A (en) * | 2013-09-09 | 2013-12-18 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| CN105797727A (en) * | 2016-05-09 | 2016-07-27 | 安徽建筑大学 | Preparation method of CuO@gamma-Al2O3 composite particles with core-shell structure |
| CN106830024A (en) * | 2017-02-16 | 2017-06-13 | 曲阜师范大学 | A kind of red mud is the hydro-thermal thermal conversion process that raw material prepares active boehmite and aluminum oxide porous microballoon |
| CN110373076A (en) * | 2019-07-12 | 2019-10-25 | 成都新柯力化工科技有限公司 | A kind of environment protecting building paint and preparation method of photocatalytic degradation haze precursor |
| CN110386613A (en) * | 2019-08-23 | 2019-10-29 | 广州大学 | A kind of preparation method for the mesoporous alumina hydrate microspherical of graduation that crystal form is controllable |
| RU2740748C1 (en) * | 2020-04-03 | 2021-01-20 | Федеральное государственное бюджетное учреждение науки Физико-технологический институт им. А.Ф. Иоффе Российской академии наук | Method of producing hollow microspheres of aluminium oxide |
| CN112604696A (en) * | 2020-11-20 | 2021-04-06 | 沪东重机有限公司 | Denitration catalyst for purifying tail gas of marine diesel engine and preparation method thereof |
-
2013
- 2013-03-17 CN CN2013100847846A patent/CN103232049A/en active Pending
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103432969A (en) * | 2013-09-09 | 2013-12-11 | 青岛科技大学 | Preparation method of alpha-Fe2O3/FeOOH core-shell structure composite microspheres |
| CN103446965A (en) * | 2013-09-09 | 2013-12-18 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| CN103446965B (en) * | 2013-09-09 | 2015-04-08 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| CN103432969B (en) * | 2013-09-09 | 2015-09-09 | 青岛科技大学 | A kind of α-Fe 2o 3the preparation method of/FeOOH nucleocapsid structure complex microsphere |
| CN105797727A (en) * | 2016-05-09 | 2016-07-27 | 安徽建筑大学 | Preparation method of CuO@gamma-Al2O3 composite particles with core-shell structure |
| CN105797727B (en) * | 2016-05-09 | 2018-07-06 | 安徽建筑大学 | A kind of nucleocapsid CuO@γ-Al2O3The preparation method of compound particle |
| CN106830024A (en) * | 2017-02-16 | 2017-06-13 | 曲阜师范大学 | A kind of red mud is the hydro-thermal thermal conversion process that raw material prepares active boehmite and aluminum oxide porous microballoon |
| CN110373076A (en) * | 2019-07-12 | 2019-10-25 | 成都新柯力化工科技有限公司 | A kind of environment protecting building paint and preparation method of photocatalytic degradation haze precursor |
| CN110386613A (en) * | 2019-08-23 | 2019-10-29 | 广州大学 | A kind of preparation method for the mesoporous alumina hydrate microspherical of graduation that crystal form is controllable |
| CN110386613B (en) * | 2019-08-23 | 2022-04-29 | 广州大学 | Preparation method of hierarchical mesoporous hydrated alumina microspheres with controllable crystal forms |
| RU2740748C1 (en) * | 2020-04-03 | 2021-01-20 | Федеральное государственное бюджетное учреждение науки Физико-технологический институт им. А.Ф. Иоффе Российской академии наук | Method of producing hollow microspheres of aluminium oxide |
| CN112604696A (en) * | 2020-11-20 | 2021-04-06 | 沪东重机有限公司 | Denitration catalyst for purifying tail gas of marine diesel engine and preparation method thereof |
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Application publication date: 20130807 |