CN104556160A - Gamma-Al2O3 nano crystal grain and preparation method thereof - Google Patents
Gamma-Al2O3 nano crystal grain and preparation method thereof Download PDFInfo
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- CN104556160A CN104556160A CN201310495683.8A CN201310495683A CN104556160A CN 104556160 A CN104556160 A CN 104556160A CN 201310495683 A CN201310495683 A CN 201310495683A CN 104556160 A CN104556160 A CN 104556160A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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Abstract
The invention discloses gamma-Al2O3 nano crystal grains and a preparation method thereof. The gamma-Al2O3 nano crystal grains are prepared by mixing an inorganic aluminum salt solution with an alkali solution with certain concentration, and by implementing hydrothermal crystallization. After a hydrothermal product is roasted, the crystal form is gamma-Al2O3, the specific surface area is 120-180 m<2>/g, the grain size is 15-40 nm, and the thickness is 3-6 nm. Compared with flaky Al2O3 grains prepared in the prior art, the gamma-Al2O3 nano crystal grains are low in raw material price, the preparation process is simple and feasible, and the product grains are of nano grade size and relatively high in specific surface area and can be used in the petrochemical engineering process such as catalyst and adsorbent separation.
Description
Technical field
The present invention relates to a kind of γ-Al
2o
3nanocrystal and preparation method thereof, belongs to field of inorganic material preparing technology.
Background technology
Aluminum oxide, as a kind of important inorganic functional material, is widely used in petrochemical complex, catalysis, absorption and ceramic toughening material etc.Nano material has excellent Wuli-Shili-Renli system approach because of the singularity of its shape.The preparation method of the nano alumina material of various form comprises chemical Vapor deposition process, pyrolysis method, water (solvent) Re Fa and hard template method etc.As the one in the form of nano material, the preparation of laminar aluminium oxide nano material has caused the very large concern of investigator at present.
Document " vapor-phase synthesis of alumina nano-sheet and mechanical property thereof " (" Materials Science and Engineering of Powder Metallurgy ", 16(6 in 2011)) in, adopt Al sheet and SiO
2powder is raw material, with H
2for protective atmosphere, synthesize α-Al by CVD (Chemical Vapor Deposition) method
2o
3nanometer sheet.In the synthesis of this vapor phase process, need comparatively complicated equipment and harsh experiment condition, majority is unsuitable for mass-producing preparation.Therefore, exploit condition is gentle, equipment is simple, the technology of preparing of the nano material of suitability for scale production is still the huge challenge that material science faces.
CN101941728A discloses a kind of preparation method of tabular alumina, relates to a kind of sheet Al for pearly pigment
2o
3preparation.The method adopts aluminium hydroxide to be raw material in preparation process, adds sodium sulfate and does synthetic medium, ethanol activates, dispersion agent, obtains flaky alumina through high-temperature calcination.The method needs to add organic medium activation, and synthesis step is comparatively loaded down with trivial details simultaneously, and gained crystal formation is α-Al
2o
3, and can find out that its grain-size reaches 10-20 μm from the data of embodiment, particle is larger.
CN 101691302A has then prepared sheet α-Al by molten-salt growth method
2o
3particle.This invention principal feature is with technical grade sodium aluminate for Alpha-alumina presoma prepared by raw material, prepares particle diameter at 2-18 μm of sheet α-Al by molten-salt growth method
2o
3.The method gained particle diameter is comparatively large, and fused salt mechanical milling process energy consumption is comparatively large, and target product also has problems with being separated of fused salt.
CN 1911809A provides a kind of preparation method of hydroxide flake aluminium of the filler for papermaking, product of rubber and plastic, and its preparation process adds polyalcohols in sodium aluminate solution.Sodium aluminate solution containing polyvalent alcohol is added ultra-fine aluminum hydroxide gel decomposition of crystal seed or the sodium aluminate solution self-decomposition containing polyvalent alcohol; Control seed load, decomposition reaction temperature, resolving time and the parameter such as sodium aluminate solution concentration, solution Crater corrosion, after solid-liquor separation, washing, drying, prepare the fine aluminum hydroxide powder of the sheet of different-grain diameter after the reaction.The method needs to add organic substance, and step is comparatively loaded down with trivial details, and from embodiment, product grain is larger.
By above-mentioned preparation sheet Al
2o
3patented method can find out, the sheet Al obtained
2o
3purposes is generally the fields such as pigment, pottery, filler, and grain-size is comparatively large, and crystal formation is generally α-Al
2o
3.The specific surface area of the aluminum oxide of this form is little, reactive behavior is low, with sheet γ-Al
2o
3compare, less in field application such as petrochemical complex, catalysis, absorption, filtrations.
Summary of the invention
For existing preparation sheet Al
2o
3problem in technology, the invention provides a kind of γ-Al
2o
3nanocrystal and preparation method thereof.
γ-Al of the present invention
2o
3the character of nanocrystal is as follows: specific surface area is 120-180m
2/ g, grain size is 15-40 nm, and thickness is 3-6 nm.
γ-Al of the present invention
2o
3the preparation method of nanocrystal, comprises following content:
(1) under ultrasonic disperse and mechanical stirring, join in inorganic aluminum salting liquid by certain density basic solution, Keep agitation makes both mix;
(2) under ultrasonic disperse and mechanical stirring, the mixture to step (1) adds metal nitrate, afterwards 180-220 DEG C of hydro-thermal reaction 2-10 hour under airtight condition;
(3), after reaction terminates, by reactant washing, drying, at 500-750 DEG C of high-temperature roasting 2-8 hour, γ-Al is obtained
2o
3nanocrystal.
Ultrasonic disperse described in step (1), its operational factors is: the energy density of ultrasonic disperse is 0.2-4kW/L, and action time is with step (1) whole process.The stirring of this process should be violent as far as possible to make mixture fully mix, to disperse.
Inorganic aluminate described in step (1) is aluminum nitrate, one or more in aluminum chloride and Tai-Ace S 150, is preferably aluminum nitrate.Alkaline matter in described basic solution is sodium hydroxide, one or more in potassium hydroxide and lithium hydroxide, is preferably a kind of in sodium hydroxide or potassium hydroxide or both mixtures.
In step (1), described inorganic aluminum salting liquid and basic solution refer to the aqueous solution of respective substance or the low-carbon alcohol solution of below C5, or the mixed solution of both arbitrary proportions, are preferably the aqueous solution.The concentration of inorganic aluminum salting liquid is 0.1 ~ 2.0 mol/L, is preferably 0.2 ~ 1.5 mol/L; The concentration of basic solution is 0.1 ~ 2.0 mol/L, is preferably 0.2 ~ 1.5 mol/L; The proportionlity of the amount of substance in both mixing solutionss meets OH
-/ Al
3+=3.0 ~ 3.5.
In step (2), described metal nitrate is one or more in SODIUMNITRATE, saltpetre or lithium nitrate, preferably corresponding with the positively charged ion of alkali metal hydroxide nitrate, such as: step (1) if in use be sodium hydroxide, then just add corresponding SODIUMNITRATE in step (2).After adding nitrate, in amount of substance, M in mixture
+/ Al
3+be 3.5 ~ 5.5, M
+represent alkali metal cation.
In step (2), hydrothermal reaction condition is: under airtight condition, 180-220 DEG C of reaction 2-10 hour.Roasting condition is: 500-750 DEG C of roasting 2-8 hour.
Compared with prior art, the cheaper starting materials that the present invention adopts, hydro-thermal preparation process is simple, does not need specific installation and technique.Tabular alumina nanocrystal specific surface area of the present invention is 120-180 m
2/ g, grain-size can reach Nano grade, and thickness is only 3 ~ 6nm, has higher specific surface area, can be used for the petrochemical process such as catalyzer, sorbent material separation.
Accompanying drawing explanation
γ-the Al of Fig. 1 prepared by the embodiment of the present invention 1
2o
3the XRD curve of nanocrystal.
γ-the Al of Fig. 2 prepared by the embodiment of the present invention 1
2o
3the images of transmissive electron microscope of nanocrystal.
Embodiment
Below by embodiment to the inventive method detailed description in addition.γ-Al
2o
3nanocrystalline grain size is measured according to images of transmissive electron microscope.Measure length and the width of the projection image of 20 particle side direction at random, get its mean value as granular size and one-tenth-value thickness 1/10.Crystal formation adopts X-ray diffraction to characterize, and specific surface area adopts low temperature nitrogen physical adsorption test (BET method).
Embodiment 1
The preparation aluminum nitrate solution of 0.2mol/L of 10ml and the sodium hydroxide solution of the 0.2mol/L of 35ml, then under the ultrasonication of 0.5KW/L, mix sodium hydroxide solution with aluminum nitrate solution and stir.Then add 0.152 gram of SODIUMNITRATE and fully dissolve.Mixture is transferred in the Pressure vessel of inner liner polytetrafluoroethylene, airtight and be warming up to 180 DEG C reaction 10 hours.Reaction terminate after, by product repeatedly separating, washing to washings be neutrality, after drying, at 550 DEG C, roasting 5 hours, obtains γ-Al
2o
3nanoparticle, grain size is 37 nm, and thickness is 5 nm.Described alumina nanoparticles is characterized by γ-Al through powder x-ray diffraction
2o
3, specific surface area is 169 m
2/ g.
Embodiment 2
The preparation aluminum nitrate solution of 0.2mol/L of 10ml and the sodium hydroxide solution of the 0.2mol/L of 30ml, then under the ultrasonication of 0.5 KW/L, mix sodium hydroxide solution with aluminum nitrate solution and stir.Then add 0.085 gram of SODIUMNITRATE and fully dissolve.Mixture is transferred in the Pressure vessel of inner liner polytetrafluoroethylene, airtight and be warming up to 220 DEG C reaction 3 hours.Reaction terminate after, by product repeatedly separating, washing to washings be neutrality, after drying, at 600 DEG C, roasting 5 hours, obtains γ-Al
2o
3nanoparticle, grain size is 23nm, and thickness is 4nm.Described alumina nanoparticles is characterized by γ-Al through powder x-ray diffraction
2o
3, show that specific surface area is 146m
2/ g.
Embodiment 3
The potassium hydroxide solution of the preparation aluminum nitrate solution of 1.5mol/L of 10ml and the 1.5mol/L of 35ml (aluminum nitrate and potassium hydroxide solution solvent used are the aqueous ethanolic solution of 15wt%).Then, under the ultrasonication of 4KW/L, lithium hydroxide solution is mixed with aluminum nitrate solution and stirs.Then add 2.27 grams of saltpetre and fully dissolve.Mixture is transferred in the Pressure vessel of inner liner polytetrafluoroethylene, more airtight and be warming up to 200 DEG C reaction 5 hours.Reaction terminate after, by product repeatedly separating, washing to washings be neutrality, after drying, at 650 DEG C, roasting 3 hours, obtains γ-Al
2o
3nanoparticle, grain size is 18 nm, and thickness is 3 nm.Crystal formation is γ-Al
2o
3, specific surface area is 117 m
2/ g.
Claims (12)
1. a γ-Al
2o
3nanocrystal, is characterized in that: γ-Al
2o
3specific surface area be 120-180m
2/ g, grain size is 15-40 nm, and thickness is 3-6 nm.
2. γ-Al according to claim 1
2o
3the preparation method of nanocrystal, is characterized in that comprising following content: basic solution, under ultrasonic disperse and mechanical stirring, joins in inorganic aluminum salting liquid by (1), and Keep agitation makes both mix; (2) under ultrasonic disperse and mechanical stirring, the mixture to step (1) adds metal nitrate, afterwards in airtight Water Under thermal response; (3), after reaction terminates, by reactant washing, dry, roasting, γ-Al is obtained
2o
3nanocrystal.
3. in accordance with the method for claim 2, it is characterized in that: the operational factors of the ultrasonic disperse described in step (1) is: the energy density of ultrasonic disperse is 0.2-4kW/L, action time is with step (1) whole process.
4. in accordance with the method for claim 2, it is characterized in that: the inorganic aluminate described in step (1) is aluminum nitrate, one or more in aluminum chloride and Tai-Ace S 150.
5. in accordance with the method for claim 2, it is characterized in that: the alkaline matter in the basic solution described in step (1) is sodium hydroxide, one or more in potassium hydroxide and lithium hydroxide.
6. in accordance with the method for claim 2, it is characterized in that: the inorganic aluminum salting liquid described in step (1) and basic solution refer to the aqueous solution of respective substance or the low-carbon alcohol solution of below C5, or the mixed solution of both arbitrary proportions.
7. according to the method described in claim 2 or 6, it is characterized in that: the concentration of inorganic aluminum salting liquid is 0.1 ~ 2.0 mol/L, the concentration of basic solution is 0.1 ~ 2.0 mol/L, and the proportionlity of the amount of substance in both mixing solutionss meets OH
-/ Al
3+=3.0 ~ 3.5.
8. in accordance with the method for claim 2, it is characterized in that: the metal nitrate described in step (2) is one or more in SODIUMNITRATE, saltpetre or lithium nitrate.
9. in accordance with the method for claim 2, it is characterized in that: the metal nitrate described in step (2) is the nitrate corresponding with the positively charged ion of alkali metal hydroxide.
10. in accordance with the method for claim 2, it is characterized in that: after step (2) adds nitrate, in amount of substance, M in mixture
+/ Al
3+be 3.5 ~ 5.5, wherein M
+represent alkali metal cation.
11. in accordance with the method for claim 2, it is characterized in that: in step (2), hydrothermal reaction condition is: 180-220 DEG C of reaction 2-10 hour.
12. in accordance with the method for claim 2, it is characterized in that: in step (3), roasting condition is: 500-750 DEG C of roasting 2-8 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107304061A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of sheet γ-Al2O3Nanocrystal and preparation method thereof |
| CN107304059A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of γ-Al2O3Nanometer chip and preparation method thereof |
| CN107304060A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of flake nano γ-Al2O3Crystal grain and preparation method thereof |
| CN107597029A (en) * | 2017-10-30 | 2018-01-19 | 苏州瑞晶纳米材料制备与应用研究有限公司 | A kind of preparation method of high-purity Alumina gel |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107304061A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of sheet γ-Al2O3Nanocrystal and preparation method thereof |
| CN107304059A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of γ-Al2O3Nanometer chip and preparation method thereof |
| CN107304060A (en) * | 2016-04-21 | 2017-10-31 | 中国石油化工股份有限公司 | A kind of flake nano γ-Al2O3Crystal grain and preparation method thereof |
| CN107304059B (en) * | 2016-04-21 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of γ-Al2O3Nanometer chip and preparation method thereof |
| CN107304060B (en) * | 2016-04-21 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of flake nano γ-Al2O3Crystal grain and preparation method thereof |
| CN107304061B (en) * | 2016-04-21 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of sheet γ-Al2O3Nanocrystal and preparation method thereof |
| CN107597029A (en) * | 2017-10-30 | 2018-01-19 | 苏州瑞晶纳米材料制备与应用研究有限公司 | A kind of preparation method of high-purity Alumina gel |
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| CN104556160B (en) | 2016-10-26 |
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