CN102502840B - Preparation method for zirconium molybdate ultra-thin nanoparticles - Google Patents
Preparation method for zirconium molybdate ultra-thin nanoparticles Download PDFInfo
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- CN102502840B CN102502840B CN201110347462.7A CN201110347462A CN102502840B CN 102502840 B CN102502840 B CN 102502840B CN 201110347462 A CN201110347462 A CN 201110347462A CN 102502840 B CN102502840 B CN 102502840B
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- molybdate
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Abstract
The invention provides a method for synthesising zirconium molybdate ultra-thin nanoparticles by microwave radiation method, wherein during preparation process, a zirconium molybdate ultra-thin and small-size particle-shaped material is prepared in a microwave radiation reaction system by using zirconium nitrate and ammonium molybdate as reaction raw materials and using distilled water as a solvent. The zirconium molybdate ultra-thin nanoparticles are 25 to 50 nanometres in diameter. The method for synthesising zirconium molybdate ultra-thin nanoparticles by microwave radiation method has the following advantages that: the microscopic shape of target product can be controlled well by introducing microwave radiation heating system, thereby obtaining the regular shape of the prepared product and laying the foundation for great improvement for application performance; as a whole, the method has the advantages of being simple in preparation process, suitable for low-cost scale production etc; additionally, the material synthesised by the method can provide necessary practical experience for the application fields of photocatalysis, environmental protection etc.
Description
[technical field]: the preparation method who the present invention relates to the technology of preparing of inorganic nano material, particularly a kind of zirconium molybdate ultra-thin nanoparticles
[background technology]: transition metal molybdate is because of the feature of the crystalline structure of material itself, and shown Chemical Diversity feature, therefore be widely used in energy storage and conversion and photocatalysis field; And along with going deep into of applied research, this material also will have bright market outlook in other field.Nanosecond science and technology are promoting the flourish of this class material too, and object is to give full play to the small-size effect of active substance, surface effects and quantum effect etc.As the important member of this series function material, molybdic acid zirconium nano material not only has the character of transition metal zr element, but also combines the function of nano material, this be promote bismuth molybdate material over-all properties optimization condition is provided.
At present, although the preparation method of molybdate nano material can adopt (C.C.Yu, the C.X.Li such as water (solvent) thermal synthesis method, ultrasonic, microwave irradiation and solid-phase synthesis, et al, Crystal Growth & Design.2009,9,783; L.W.Qian, J.Zhu, et al, Chem.Eur.J.2009,15,1233; J.F.Liu, Y.D.Li, J.Mater.Chem.2007,17,1797; Y.P.Fang, A.W.Xu, et al, Adv.Funct.Mater.2003,13.955; M.Saux, J.Galy, C.R.Acad.Sci.1973,276, C81.), but existing document also exists certain problem to the rapidly and efficiently controlledly synthesis aspect of molybdic acid zirconium nano material.And relate to document that microwave irradiation effectively controls molybdic acid zirconium small-size materials microtexture just still less.According to above-mentioned present Research, the invention provides and under normal pressure experiment condition, utilize microwave irradiation successfully to control the nucleation rate of material, regulate the convenient method of target product size, this is undoubtedly for significantly advancing the application performance of bismuth molybdate small scale functional material to pave road.
[summary of the invention]: the summary of the invention of this patent is to provide a kind of preparation method of zirconium molybdate ultra-thin nanoparticles, the distinguishing feature of this microwave irradiation technology is that workable, the especially applicable serialization scale low cost of Key Experiment parameter is synthetic.
[technical scheme of the present invention]: the present invention relates to a kind of method that adopts the synthetic zirconium molybdate ultra-thin nanoparticles of microwave irradiation, in preparation process taking zirconium nitrate, ammonium molybdate as reaction raw materials, solvent is selected distilled water, in microwave radiation reaction system, prepare the ultra-fine small sized particles shape of molybdic acid zirconium material, below concrete steps:
The one, at room temperature, makes zirconium nitrate dissolution of solid the solution of certain zirconium nitrate volumetric molar concentration in distilled water, and vigorous stirring 15 minutes, is just mixed with solution a;
The 2nd, accurate weighing (NH
4)
6mo
7o
244H
2o ammonium molybdate powder, adds the hot distilled water of 60～75 DEG C, stirs after within 10 minutes, dissolving completely to ammonium molybdate to obtain clear solution, is then dropwise added drop-wise in the solution a that step 1 prepares, and 60 DEG C of constant temperature, continue to stir 10 minutes, make solution b;
The 3rd. the precursors mixture that solution b is obtained is transferred in round-bottomed flask, then being placed in normal pressure microwave radiation reactor and setting the reaction times is 30 minutes, reaction finishes rear cotton-shaped product and after 24 hours, just obtains molybdic acid zirconium white look Zr (MoO through centrifugation, washing, alcohol wash, 60 degree freeze-day with constant temperature
4)
2nm-class.
The diameter of described molybdic acid zirconium white look superfine nano particle is 25-50 nanometer, and the compound with regular structure of nano particle, yardstick are even.
[advantage of the present invention and effect]: the present invention adopts microwave irradiation to synthesize zirconium molybdate ultra-thin nanoparticles, its advantage and beneficial effect are embodied in by introducing carry out microwave radiation heating system and can better control the microscopic appearance of target product, thereby the product pattern making is regular, for application performance significantly promotes and lays a good foundation; All in all, the method has the beneficial effects such as preparation flow is simple, also applicable low-coat scale production; In addition, the synthetic material of the method can be the Application Areas such as photochemical catalysis, environment protection necessary theoretical basis and practical experience is provided.
[brief description of the drawings]:
Fig. 1 is zirconium molybdate ultra-thin nanoparticles low power scanning electronic microscope (SEM) figure
Fig. 2 is zirconium molybdate ultra-thin nanoparticles high power SEM figure
[embodiment]:
Embodiment 1:
At room temperature, accurately configure the zirconium nitrate solution that volumetric molar concentration is 0.00125mol/L, vigorous stirring is extremely dissolved for 15 minutes completely; Weigh (NH
4)
6mo
7o
244H
2o ammonium molybdate solid, adds the hot distilled water of 60～75 DEG C, stirs and dissolves to obtain clear solution completely to ammonium molybdate in 10 minutes, and making its ammonium molybdate volumetric molar concentration is 1.79*10
-4mol/L, is then dropwise added to this solution in prepared zirconium nitrate solution, continues to stir 10 minutes; Above-mentioned precursors mixture is dropwise poured in round-bottomed flask, and be placed in normal pressure microwave radiation reactor, controlling heat-up time is 30 minutes, the cotton-shaped product of white obtaining after reaction finishes after 24 hours, makes ultra-fine Zr (MoO through centrifugation, washing, alcohol wash, 60 degree freeze-day with constant temperature
4)
2molybdic acid zirconium nanometer.Product (Fig. 1) is tested and is shown that product main body pattern is finely disseminated molybdic acid zirconium nano particle through scanning electronic microscope (SEM), and the microscopic appearance of its particle is regular and yardstick is even; The diameter that examines more powerful SEM figure (Fig. 2) known molybdic acid zirconium nano material is 25-50 nanometer.
Claims (1)
1. a preparation method for zirconium molybdate ultra-thin nanoparticles, is characterized in that: at room temperature, accurately configure the zirconium nitrate solution that volumetric molar concentration is 0.00125 mol/L, vigorous stirring is extremely dissolved for 15 minutes completely; Weigh (NH
4)
6mo
7o
244H
2o ammonium molybdate solid, adds the hot distilled water of 60～75 DEG C, stirs and dissolves to obtain clear solution completely to ammonium molybdate in 10 minutes, and making its ammonium molybdate volumetric molar concentration is 1.79*10
-4mol/L, is then dropwise added to this solution in prepared zirconium nitrate solution, continues to stir 10 minutes; Above-mentioned precursors mixture is dropwise poured in round-bottomed flask, and be placed in normal pressure microwave radiation reactor, controlling heat-up time is 30 minutes, the cotton-shaped product of white obtaining after reaction finishes after 24 hours, makes ultra-fine Zr (MoO through centrifugation, washing, alcohol wash, 60 degree freeze-day with constant temperature
4)
2molybdic acid zirconium; Product shows that through scanning electronic microscope SEM test product main body pattern is finely disseminated molybdic acid zirconium nano particle, and the microscopic appearance of its particle is regular and yardstick is even; The diameter of molybdic acid zirconium nano material is 25-50 nanometer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391817A (en) * | 2008-10-31 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing molybdate nanocrystalline |
| CN101717120A (en) * | 2009-12-14 | 2010-06-02 | 上海应用技术学院 | Solvent thermal induction control synthesis method for nano molybdate with scheelite structure |
| CN102060330A (en) * | 2010-11-24 | 2011-05-18 | 江南大学 | Method for synthetizing bismuth molybdate octahedral nanoparticle by microwave radiation heating |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391817A (en) * | 2008-10-31 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing molybdate nanocrystalline |
| CN101717120A (en) * | 2009-12-14 | 2010-06-02 | 上海应用技术学院 | Solvent thermal induction control synthesis method for nano molybdate with scheelite structure |
| CN102060330A (en) * | 2010-11-24 | 2011-05-18 | 江南大学 | Method for synthetizing bismuth molybdate octahedral nanoparticle by microwave radiation heating |
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Inventor after: Sun Yan Inventor after: Rong Tao Inventor after: Li Chunsheng Inventor after: Ma Xuegang Inventor after: Shi Jifu Inventor after: Zhang Shaoyan Inventor after: Song Dawei Inventor after: Wang Lina Inventor after: Hu Yiwen Inventor after: Sun Bowei Inventor before: Sun Yan Inventor before: Li Chunsheng Inventor before: Zhang Zhijia Inventor before: Wang Yaozu Inventor before: Ma Xuegang Inventor before: Wang Lina Inventor before: Ma Peijuan |
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