CN104556160B - A kind of γ-Al2o3nanocrystal and preparation method thereof - Google Patents
A kind of γ-Al2o3nanocrystal and preparation method thereof Download PDFInfo
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- CN104556160B CN104556160B CN201310495683.8A CN201310495683A CN104556160B CN 104556160 B CN104556160 B CN 104556160B CN 201310495683 A CN201310495683 A CN 201310495683A CN 104556160 B CN104556160 B CN 104556160B
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- 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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- 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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Abstract
The invention discloses a kind of γ Al2O3Nanocrystal and preparation method thereof.The nanometer γ Al of the present invention2O3Crystal grain be by certain density inorganic aluminum salting liquid is mixed with alkaline solution after, obtain through hydrothermal crystallizing.After hydrothermal product is fired, crystal formation is γ Al2O3, specific surface area is 120 180 m2/ g, particle size is 15 40nm, and thickness is 3 6nm.With lamellar Al of preparation in prior art2O3Granule is compared, low in raw material price, and preparation is simple, and product grain is nano-grade size, and specific surface area is higher, can be used for the petrochemical process such as catalyst, adsorbent separation.
Description
Technical field
The present invention relates to a kind of γ-Al2O3Nanocrystal and preparation method thereof, belongs to field of inorganic material preparing technology.
Background technology
Aluminium oxide as a kind of important inorganic functional material, in petrochemical industry, is catalyzed, adsorbs and the aspect such as ceramic toughening material is widely used.Nano material has the Wuli-Shili-Renli system approach of excellence because of the particularity of its shape.The preparation method of the nano alumina material of various forms includes chemical vapour deposition technique, pyrolysismethod, water (solvent) full-boiled process 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 concern that researcher is the biggest at present.
Document " vapor-phase synthesis of alumina nano-sheet and mechanical property thereof " (" Materials Science and Engineering of Powder Metallurgy ", 2011,16(6)) in, use Al sheet and SiO2Powder is raw material, with H2For protective atmosphere, synthesize α-Al by CVD method2O3Nanometer sheet.In the synthesis of this vapor phase method, needing complex equipment and harsh experiment condition, majority is unsuitable for scale to be prepared.Therefore, the technology of preparing of the nano material that exploit condition is gentle, equipment is simple, suitable for scale production is still the huge challenge that material science faces.
CN101941728A discloses the preparation method of a kind of tabular alumina, relates to a kind of lamellar Al for pearlescent pigment2O3Preparation.The method uses aluminium hydroxide to be raw material in preparation process, adds sodium sulfate and does synthetic medium, and ethanol activates, dispersant, obtains flaky alumina through high-temperature calcination.The method needs to add organic agent activating, and simultaneously synthesizing step is relatively complicated, and gained crystal formation is α-Al2O3, and can be seen that its crystallite dimension reaches 10-20 μm from the data of embodiment, granule is bigger.
CN 101691302A is then prepared for lamellar α-Al by molten-salt growth method2O3Granule.This invention is mainly characterized by prepares Alpha-alumina presoma with technical grade sodium aluminate for raw material, prepares particle diameter at 2-18 μm lamellar α-Al by molten-salt growth method2O3.The method gained particle diameter is relatively big, and fused salt mechanical milling process energy consumption is relatively big, and target product separates, with fused salt, the problem of there is also.
CN 1911809A provides a kind of for papermaking, the preparation method of the hydroxide flake aluminum of the filler of product of rubber and plastic, and its preparation process is interpolation polyalcohols in sodium aluminate solution.Sodium aluminate solution containing polyhydric alcohol is added ultra-fine gel aluminum hydroxide decomposition of crystal seed or the sodium aluminate solution selfdecomposition containing polyhydric alcohol；Control seed load, decomposition reaction temperature, resolving time and the parameter such as sodium aluminate solution concentration, solution Crater corrosion, after the reaction through solid-liquor separation, washing, prepare the aluminium hydroxide micro powder of the lamellar of different-grain diameter after drying.The method needs to add organic substance, and step is relatively complicated, and in terms of embodiment, product grain is bigger.
By above-mentioned preparation lamellar Al2O3Patented method it can be seen that lamellar Al that obtains2O3Purposes is generally the fields such as pigment, pottery, filler, and crystallite dimension is relatively big, and crystal formation is generally α-Al2O3.The specific surface area of the aluminium oxide of this form is little, reactivity is low, with lamellar γ-Al2O3Compare, petrochemical industry, be catalyzed, adsorb, the field application such as filtration less.
Summary of the invention
For existing preparation lamellar Al2O3Problem in technology, the invention provides a kind of γ-Al2O3Nanocrystal and preparation method thereof.
γ-the Al of the present invention2O3The character of nanocrystal is as follows: specific surface area is 120-180m2/ g, grain size is 15-40 nm, and thickness is 3-6 nm.
γ-the Al of the present invention2O3The preparation method of nanocrystal, including following content:
(1) under ultrasonic disperse and mechanical agitation, certain density alkaline solution is joined in inorganic aluminum salting liquid, continuously stirred make both mix homogeneously；
(2) under ultrasonic disperse and mechanical agitation, metal nitrate, afterwards 180-220 DEG C of hydro-thermal reaction 2-10 hour under conditions of airtight are added to the mixture of step (1)；
(3) after reaction terminates, reactant washed, be dried, 500-750 DEG C of high-temperature roasting 2-8 hour, obtain γ-Al2O3Nanocrystal.
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 as far as possible acutely so that mixture be sufficiently mixed, disperses.
Inorganic aluminate described in step (1) is one or more in aluminum nitrate, aluminum chloride and aluminum sulfate, preferably aluminum nitrate.The described alkaline matter in alkaline solution is a kind of in one or more in sodium hydroxide, potassium hydroxide and Lithium hydrate, preferably sodium hydroxide or potassium hydroxide or both mixture.
In step (1), described inorganic aluminum salting liquid and alkaline solution refer to the aqueous solution of respective substance or the low-carbon alcohol solution of below C5, or the mixed liquor of both arbitrary proportions, preferably aqueous solution.The concentration of inorganic aluminum salting liquid is 0.1 ~ 2.0 mol/L, preferably 0.2 ~ 1.5 mol/L；The concentration of alkaline solution is 0.1 ~ 2.0 mol/L, preferably 0.2 ~ 1.5 mol/L；The proportionate relationship of the amount of the material in both mixed solutions meets OH-/Al3+ =3.0~3.5。
In step (2), described metal nitrate is one or more in sodium nitrate, potassium nitrate or lithium nitrate, preferably corresponding with the cation of alkali metal hydroxide nitrate, such as: step (1) if in use for sodium hydroxide, then step (2) just adds corresponding sodium nitrate.After adding nitrate, with the gauge of material, M in mixture+/Al3+It is 3.5 ~ 5.5, M+Represent alkali metal cation.
In step (2), hydrothermal reaction condition is: under conditions of airtight, and 180-220 DEG C is reacted 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 uses, hydro-thermal preparation process is simple, it is not necessary to special installation and technique.Tabular alumina nanocrystal specific surface area of the present invention is 120-180 m2/ g, crystallite dimension can reach Nano grade, and thickness is only 3 ~ 6nm, has higher specific surface area, can be used for the petrochemical process such as catalyst, adsorbent separation.
Accompanying drawing explanation
Fig. 1 is the γ-Al prepared by the embodiment of the present invention 12O3The XRD curve of nanocrystal.
Fig. 2 is the γ-Al prepared by the embodiment of the present invention 12O3The images of transmissive electron microscope of nanocrystal.
Detailed description of the invention
Below by embodiment, the inventive method is described in detail.γ-Al2O3Nanocrystalline grain size is measured according to images of transmissive electron microscope.Measure length and the width of 20 lateral projection images of granule at random, take its meansigma methods as granular size and one-tenth-value thickness 1/10.Crystal formation uses X-ray diffraction to characterize, and specific surface area uses low temperature nitrogen physical absorption test (BET method).
Embodiment 1
The aluminum nitrate solution of the 0.2mol/L of preparation 10ml and the sodium hydroxide solution of the 0.2mol/L of 35ml, then under the ultrasonication of 0.5KW/L, be mixed and stirred for sodium hydroxide solution and aluminum nitrate solution uniformly.It is subsequently adding 0.152 gram of sodium nitrate and fully dissolves.Mixture is transferred in the Pressure vessel of inner liner polytetrafluoroethylene, airtight and be warming up to 180 DEG C react 10 hours.After reaction terminates, it is neutral by product separating, washing repeatedly to cleaning mixture, after drying, roasting 5 hours at 550 DEG C, obtain γ-Al2O3Nanoparticle, grain size is 37 nm, and thickness is 5 nm.Described alumina nanoparticles is characterized as γ-Al through powder X-ray diffraction2O3, specific surface area is 169 m2/g。
Embodiment 2
The aluminum nitrate solution of the 0.2mol/L of preparation 10ml and the sodium hydroxide solution of the 0.2mol/L of 30ml, then under the ultrasonication of 0.5 KW/L, be mixed and stirred for sodium hydroxide solution and aluminum nitrate solution uniformly.It is subsequently adding 0.085 gram of sodium nitrate and fully dissolves.Mixture is transferred in the Pressure vessel of inner liner polytetrafluoroethylene, airtight and be warming up to 220 DEG C react 3 hours.After reaction terminates, it is neutral by product separating, washing repeatedly to cleaning mixture, after drying, roasting 5 hours at 600 DEG C, obtain γ-Al2O3Nanoparticle, grain size is 23nm, and thickness is 4nm.Described alumina nanoparticles is characterized as γ-Al through powder X-ray diffraction2O3, show that specific surface area is 146m2/g。
Embodiment 3
The aluminum nitrate solution of the 1.5mol/L of preparation 10ml and the potassium hydroxide solution (solvent used by aluminum nitrate and potassium hydroxide solution is the ethanol water of 15wt%) of the 1.5mol/L of 35ml.Then, under the ultrasonication of 4KW/L, lithium hydroxide solution and aluminum nitrate solution are mixed and stirred for uniformly.It is subsequently adding 2.27 grams of potassium nitrate and fully dissolves.Mixture is transferred in the Pressure vessel of inner liner polytetrafluoroethylene, more airtight and be warming up to 200 DEG C react 5 hours.After reaction terminates, it is neutral by product separating, washing repeatedly to cleaning mixture, after drying, roasting 3 hours at 650 DEG C, obtain γ-Al2O3Nanoparticle, grain size is 18 nm, and thickness is 3 nm.Crystal formation is γ-Al2O3, specific surface area is 117 m2/g。
Claims (5)
1. a γ-Al2O3The preparation method of nanocrystal, described γ-Al2O3Specific surface area be 120-180 m2/ g, grain size is 15-40 nm, and thickness is 3-6 nm, it is characterised in that include following content: alkaline solution, under ultrasonic disperse and mechanical agitation, is joined in inorganic aluminum salting liquid by (1), continuously stirred makes both mix homogeneously；(2) under ultrasonic disperse and mechanical agitation, metal nitrate, afterwards hydro-thermal reaction under conditions of airtight are added to the mixture of step (1)；(3), after reaction terminates, by reactant washing, dry, roasting, γ-Al is obtained2O3Nanocrystal；The operational factors of the ultrasonic disperse described in step (1) is: the energy density of ultrasonic disperse is 0.2-4 kW/L, and action time is with step (1) whole process；
The concentration of inorganic aluminum salting liquid is 0.1 ~ 2.0 mol/L, and the concentration of alkaline solution is 0.1 ~ 2.0 mol/L, and the proportionate relationship of the amount of the material in both mixed solutions meets OH-/Al3+= 3.0~3.5；
After step (2) adds nitrate, with the gauge of material, M in mixture+/Al3+It is 3.5 ~ 5.5, wherein M+Represent alkali metal cation；
Metal nitrate described in step (2) is one or more in sodium nitrate, potassium nitrate or lithium nitrate；
In step (2), hydrothermal reaction condition is: 180-220 DEG C is reacted 2-10 hour；
In step (3), roasting condition is: 500-750 DEG C of roasting 2-8 hour.
The most in accordance with the method for claim 1, it is characterised in that: the inorganic aluminate described in step (1) is one or more in aluminum nitrate, aluminum chloride and aluminum sulfate.
The most in accordance with the method for claim 1, it is characterised in that: the alkaline matter in the alkaline solution described in step (1) is one or more in sodium hydroxide, potassium hydroxide and Lithium hydrate.
The most in accordance with the method for claim 1, it is characterised in that: the inorganic aluminum salting liquid described in step (1) and alkaline solution refer to the aqueous solution of respective substance or the low-carbon alcohol solution of below C5, or the mixed liquor of both arbitrary proportions.
The most in accordance with the method for claim 1, it is characterised in that: the metal nitrate described in step (2) is the nitrate corresponding with the cation of alkali metal hydroxide.
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| 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 |
| 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 |
| 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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| CN100473610C (en) * | 2006-12-22 | 2009-04-01 | 武汉大学 | Preparing process fibrous nano alumina powder |
| CN101269829B (en) * | 2007-03-23 | 2010-07-28 | 中国石油天然气股份有限公司 | Gamma-Al with large specific surface area2O3Material and method for the production thereof |
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