CN102502840A - Preparation method for zirconium molybdate ultra-thin nanoparticles - Google Patents
Preparation method for zirconium molybdate ultra-thin nanoparticles Download PDFInfo
- Publication number
- CN102502840A CN102502840A CN2011103474627A CN201110347462A CN102502840A CN 102502840 A CN102502840 A CN 102502840A CN 2011103474627 A CN2011103474627 A CN 2011103474627A CN 201110347462 A CN201110347462 A CN 201110347462A CN 102502840 A CN102502840 A CN 102502840A
- Authority
- CN
- China
- Prior art keywords
- zirconium
- ultra
- solution
- microwave radiation
- molybdate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
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 present invention relates to the technology of preparing of inorganic nano material, particularly a kind of molybdic acid zirconium superfine nano particulate preparation method
[background technology]: the transition metal molybdate is because of the characteristic of the crystalline structure of material itself, and shown the Chemical Diversity characteristics, so be widely used in store energy 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 type material too, and purpose 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 has combined the function of nano material, this for promote the bismuth molybdate material over-all properties optimization condition is provided.
At present, though the molybdate preparation of nanomaterials can adopt (C.C.Yu, C.X.Li, et al, Crystal Growth&Design.2009,9,783 such as water (solvent) thermal synthesis method, ultrasonic synthesis method, microwave irradiation and solid-phase synthesis; 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 controlledly synthesis aspect rapidly and efficiently 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 the nucleation rate that under the normal pressure experiment condition, utilizes microwave irradiation success control material; Regulate the convenient method of title product size, this has paved road for the application performance that significantly advances bismuth molybdate small size functional materials undoubtedly.
[summary of the invention]: the summary of the invention of this patent is to provide a kind of molybdic acid zirconium superfine nano particulate preparation method, and the distinguishing feature of this microwave irradiation technology is that workable, the especially suitable serialization scale of Key Experiment parameter is low-cost synthetic.
[technical scheme of the present invention]: the present invention relates to the synthetic molybdic acid zirconium superfine nano particulate method of a kind of employing microwave irradiation; Be reaction raw materials with zirconium nitrate, ammonium molybdate in the preparation process; Solvent is selected zero(ppm) water for use; The ultra-fine small sized particles shape of preparation molybdic acid zirconium material in the microwave radiation reaction system, below the concrete steps:
The one, at room temperature is dissolved in the solution that makes certain zirconium nitrate volumetric molar concentration in the zero(ppm) water with the zirconium nitrate solid, and vigorous stirring 15 minutes just is mixed with solution a;
Accurate weighing (the NH of the 2nd,
4)
6Mo
7O
244H
2The O ammonium molybdate powder adds 60～75 ℃ hot distilled water, stir after dissolving fully to ammonium molybdate in 10 minutes clear solution, dropwise be added drop-wise to then among the solution a that step 1 prepares, 60 ℃ of constant temperature continue to stir 10 minutes, make solution b;
The 3rd. the reaction precursor body mixture that solution b obtains is transferred in the round-bottomed flask; Placing normal pressure microwave radiation reactor drum then and setting the reaction times is 30 minutes; Reaction finish the cotton-shaped product in back through spinning, washing, alcohol wash, 60 degree freeze-day with constant temperature are after 24 hours, just obtain molybdic acid zirconium white look Zr (MoO
4)
2Nm-class.
Said molybdic acid zirconium white look superfine nano particulate diameter is the 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 molybdic acid zirconium superfine nano particle; Its advantage and beneficial effect are embodied in through introducing the carry out microwave radiation heating system and can better control the microscopic appearance of title product; Thereby the product pattern that makes is regular, lays a good foundation for application performance significantly promotes; All in all, this method has beneficial effects such as preparation flow is simple, also suitable low-coat scale production; In addition, this method synthetic material can be Application Areass such as photochemical catalysis, environment protection necessary theoretical basis and practical experience is provided.
[description of drawings]:
Fig. 1 is molybdic acid zirconium superfine nano particle low power sem (SEM) figure
Fig. 2 is molybdic acid zirconium superfine nano particle high power SEM figure
[embodiment]:
Embodiment 1:
At room temperature, accurately dispose the zirconium nitrate solution that volumetric molar concentration is 0.00125mol/L, vigorous stirring dissolving extremely fully in 15 minutes; Weighing (NH
4)
6Mo
7O
244H
2O ammonium molybdate solid adds 60～75 ℃ hot distilled water, stir 10 minutes to ammonium molybdate dissolve fully clear solution, making its ammonium molybdate volumetric molar concentration is 1.79*10
-4Mol dropwise is added to this solution in the zirconium nitrate solution of being prepared then, continues to stir 10 minutes; Dropwise pour into above-mentioned reaction precursor body mixture in the round-bottomed flask; And place normal pressure microwave radiation reactor drum; Control is 30 minutes heat-up time, the white cotton-shaped product that reaction obtains after finishing through spinning, washing, alcohol wash, 60 degree freeze-day with constant temperature are after 24 hours, make ultra-fine Zr (MoO
4)
2Molybdic acid zirconium nanometer.Product through sem (SEM) (Fig. 1) test shows product main body pattern be finely disseminated molybdic acid zirconium nano particle, its microcosmic appearance is regular and yardstick is even; The SEM figure (Fig. 2) that examines than high magnification can know that the diameter of molybdic acid zirconium nano material is the 25-50 nanometer.
Claims (2)
1. the present invention relates to the synthetic molybdic acid zirconium superfine nano particulate method of a kind of employing microwave irradiation; Be reaction raw materials with zirconium nitrate, ammonium molybdate in the preparation process; Solvent is selected zero(ppm) water for use, the ultra-fine small sized particles shape of preparation molybdic acid zirconium material in the microwave radiation reaction system, below the concrete steps:
The one, at room temperature is dissolved in the solution that makes certain zirconium nitrate volumetric molar concentration in the zero(ppm) water with the zirconium nitrate solid, and vigorous stirring 15 minutes just is mixed with solution a;
Accurate weighing (the NH of the 2nd,
4)
6Mo
7O
244H
2The O ammonium molybdate powder adds 60～75 ℃ hot distilled water, stir after dissolving fully to ammonium molybdate in 10 minutes clear solution, dropwise be added drop-wise to then among the solution a that step 1 prepares, 60 ℃ of constant temperature continue to stir 10 minutes, make solution b;
The 3rd. the reaction precursor body mixture that solution b obtains is transferred in the round-bottomed flask; Placing normal pressure microwave radiation reactor drum then and setting the reaction times is 30 minutes; Reaction finish the cotton-shaped product in back through spinning, washing, alcohol wash, 60 degree freeze-day with constant temperature are after 24 hours, just obtain molybdic acid zirconium white look Zr (MoO
4)
2Nm-class.
2. according to the said white Zr (MoO of claim 1
4)
2The diameter of nm-class is the 25-50 nanometer, and compound with regular structure, the yardstick of its nano particle are even.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110347462.7A CN102502840B (en) | 2011-11-07 | 2011-11-07 | Preparation method for zirconium molybdate ultra-thin nanoparticles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110347462.7A CN102502840B (en) | 2011-11-07 | 2011-11-07 | Preparation method for zirconium molybdate ultra-thin nanoparticles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102502840A true CN102502840A (en) | 2012-06-20 |
| CN102502840B CN102502840B (en) | 2014-08-06 |
Family
ID=46214991
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110347462.7A Expired - Fee Related CN102502840B (en) | 2011-11-07 | 2011-11-07 | Preparation method for zirconium molybdate ultra-thin nanoparticles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102502840B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115611312A (en) * | 2022-11-04 | 2023-01-17 | 嘉兴市福思矼新材料有限公司 | Preparation method of zirconium molybdate ultrafine nanoparticles |
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 |
-
2011
- 2011-11-07 CN CN201110347462.7A patent/CN102502840B/en not_active Expired - Fee Related
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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115611312A (en) * | 2022-11-04 | 2023-01-17 | 嘉兴市福思矼新材料有限公司 | Preparation method of zirconium molybdate ultrafine nanoparticles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102502840B (en) | 2014-08-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102225784B (en) | Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation | |
| CN104538145B (en) | Multi-scale uniform and single-dispersion magnetic microsphere and preparation method thereof | |
| CN103539210B (en) | A kind of preparation method of cobalt molybdate crystallite | |
| CN102161509B (en) | Method for synthesizing metal molybdate micron/nano materials by adopting microwave radiation method | |
| CN102140691A (en) | Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method | |
| CN105731535B (en) | A kind of preparation method of Zinc oxide/titanium dioxide composite nano materials | |
| Quan et al. | Polyol-mediated synthesis of PbS crystals: shape evolution and growth mechanism | |
| CN102502839B (en) | Method for preparing flaky bismuth molybdate nano material with uniform thickness | |
| CN104310468B (en) | One prepares the method for monodisperse titanium dioxide (B) nanoparticle | |
| CN102786090B (en) | Method for synthesizing vanadic acid zinc overlength nanowire material by microwave radiation | |
| CN104150537B (en) | A kind of six side phase WO3Nanotube and preparation method thereof | |
| CN102887548B (en) | Sea-urchin-shaped hiberarchy cobaltosic oxide nanosphere and preparing method thereof | |
| CN101920940B (en) | Method for preparing tellurium nanocrystals | |
| CN102502834B (en) | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods | |
| CN103145198A (en) | Method for producing nanometer structure cobalt tetroxide sub-micron hollow balls | |
| CN102502885B (en) | Method for preparing cobalt molybdate material in which micron rod is assembled by nano sheets | |
| Zou et al. | Ultrasound-assisted synthesis of CuO nanostructures templated by cotton fibers | |
| CN102502837B (en) | Method for preparing ultrathin lanthanum molybdate nano sheet material | |
| CN102557141A (en) | Structure-oriented synthetic method of zinc tungstate nanometer sheet | |
| CN102502843B (en) | Method for preparing lanthanum molybdate nanotube material by microwave radiation method | |
| CN105290419A (en) | Fishbone-shaped core-shell structure nanometer nickel-copper alloy powder and preparation method thereof | |
| CN102502842A (en) | Preparation method for radial copper molybdate microspheres assembled by nanowires | |
| CN102502840B (en) | Preparation method for zirconium molybdate ultra-thin nanoparticles | |
| CN102502860A (en) | Preparation method for iron molybdate nanosheets | |
| CN102502835A (en) | Method for preparing silver molybdate nano square crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
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 |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: SUN YAN LI CHUNSHENG ZHANG ZHIJIA WANG YAOZU MA XUEGANG WANG LINA MA PEIJUAN TO: SUN YAN LI CHUNSHENG MA XUEGANG SHI JIFU ZHANG SHAOYAN SONG DAWEI WANG LINA HU YIWEN SUN BOWEI RONG TAO |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140806 Termination date: 20191107 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |