CN101691206A - Method for synthesizing various strontium molybdate micro-nano structures at room temperature - Google Patents
Method for synthesizing various strontium molybdate micro-nano structures at room temperature Download PDFInfo
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- CN101691206A CN101691206A CN200910114355A CN200910114355A CN101691206A CN 101691206 A CN101691206 A CN 101691206A CN 200910114355 A CN200910114355 A CN 200910114355A CN 200910114355 A CN200910114355 A CN 200910114355A CN 101691206 A CN101691206 A CN 101691206A
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Abstract
The invention provides a method for synthesizing various strontium molybdate micro-nano structures at room temperature, and the method comprises the steps of selecting quaternary microemulsion consisting of a non-ionic surfactant of alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octanol and a water phase, taking sodium molybdate and strontium chloride as reactants, mixing various components for composing inverse microemulsion and strong stirring on a magnetic stirrer at the room temperature for preparing the uniform and transparent inverse microemulsion with stable nature, then dripping the microemulsion of the strontium chloride in the microemulsion of the sodium molybdate, leading the two to react in finite domain space of the microemulsion, carrying out reaction, aging and centrifugal separation, and washing with acetone, anhydrous ethanol and secondary water repeatedly, thereby preparing the various strontium molybdate micro-nano structures with uniform appearance and size. The technical scheme designs a new microemulsion system and utilizes a template and the finite domain role of the inverse micell microemulsion for preparing the novel various strontium molybdate micro-nano structures. The method is characterized by simple production technology, safe production process and difficult clustering of products and can be widely used in the preparation of inorganic functional materials with three-dimensional structures.
Description
Technical field
The present invention relates to a kind of preparation of inorganic functional material, particularly a kind of method that adopts the uniform multiple strontium molybdate micro-nano structures of the big low height of room temperature prepared by reverse microemulsion method pattern.
Background technology
Tungsten, molybdate are two important members in the inorganic functional material family.Because the special photoelectric properties that itself had, scintillator performance, humidity sensor performance etc. receive much concern it in the inorganic functional material field.In these tungstens, molybdate, cubic phase alkaline-earth metal molybdate---the strontium molybdate of scheelite-type structure based on its unique fluorescence property etc., has caused people's extensive studies interest in recent years.The strontium molybdate micro-nano structures that has prepared multiple different-shape structure by various methods.
Chen etc. [L.P.Chen, Y.H.Gao, Chem.Eng.J.2007,131,181] adopt the micro cell technology to prepare the strontium molybdate fluorescence membrane; [J.C.Sczancoski, L.S.Cavalcante, M.R.Joya such as Sczancoski, J.A.Varela, P.S.Pizani, E.Longo, Chem.Eng.J.2008,140,632] prepared strontium molybdate powder by the microwave assisting alcohol-hydrothermal method with good optical property; Bi etc. [J.Bi, C.-H.Cui, X.Lai, F.Shi, D.-J.Gao, Mater.Res.Bull.2008,43,743] have prepared the strontium molybdate fluorescence membrane by irreversible galvanic cell method.Zhang etc. [Y.M.Zhang, F.D.Yang, J.Yang, Y.Tang, P.Yuan, Solid.State.Comm.2005,133,759] have prepared mono-crystalline structures strontium molybdate nano line under 180 ℃ of hydrothermal conditions; [J.Liu such as Liu, J.F.Ma, B.T.Lin, Y.Ren, X.H.Jiang, J.T.Tao, X.Y.Zhu, Ceram.Inter.2008,34,1557] obtained the ball-type of pattern granularity height unanimity, the strontium molybdate micro-nano structures of corynebacterium structure in the reverse microemulsion liquid medium, fluorometric investigation is the result show, the fluorescence property of product and the appearance structure of product and granular relevant.
Summary of the invention
The objective of the invention is under the temperate condition of normal temperature and pressure, by a kind of simple, safe production technology, by a kind of design of new microemulsion system, at the synthetic even-grained multiple strontium molybdate micro-nano structures of confinement space inner control.
Purpose of the present invention can be achieved through the following technical solutions: the method for the synthetic multiple strontium molybdate micro-nano structures of a kind of room temperature control is characterized in that this preparation method selects raw material non-ionic surface active agent alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octyl alcohol and water [SrCl for use
2The aqueous solution or Na
2MoO
4The aqueous solution] form microemulsion, after each component of forming microemulsion is mixed, be prepared into the reverse micro emulsion of homogeneous transparent, with SrCl
2Microemulsion dropwise add Na
2MoO
4Microemulsion in, SrCl
2And Na
2MoO
4At the confinement space of microemulsion internal reaction, after the reaction, make multiple strontium molybdate micro-nano structures through ageing, centrifugation, washing, concrete preparation process is as follows:
1), with raw material alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octyl alcohol and water [SrCl
2The aqueous solution] insert in the beaker of 50ml the quality percentage composition that selected alkyl polyoxyethylene (10) ether (OP-10) surfactant mixes with alcohol, water [SrCl
2The aqueous solution] amount of substance and the ratio ω of the amount of substance of alkyl polyoxyethylene (10) ether (OP-10), SrCl
2The concentration of the aqueous solution after above-mentioned each component mixing, stirred 30 minutes on constant temperature blender with magnetic force under the room temperature, was mixed with uniform SrCl
2Microemulsion;
2), with raw material alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octyl alcohol and water [Na
2MoO
4The aqueous solution] insert in the beaker of 50ml the quality percentage composition that selected alkyl polyoxyethylene (10) ether (OP-10) surfactant mixes with alcohol, water [Na
2MoO
4The aqueous solution] amount of substance and the ratio ω of the amount of substance of alkyl polyoxyethylene (10) ether (OP-10), Na
2MoO
4The concentration of solution after each component of said mixture fully mixed, stirred 30 minutes on constant temperature blender with magnetic force under the room temperature, was mixed with uniform Na
2MoO
4Microemulsion;
3), with Na
2MoO
4Microemulsion places on the constant temperature blender with magnetic force, at room temperature dropwise drips microemulsion SrCl
2Microemulsion is along with SrCl
2The adding of microemulsion, microemulsion become white gradually, dropwise the back and continue to stir 30 minutes;
4), with preservative film sealing beaker mouth, ageing at room temperature 72 hours;
5), reactant liquor centrifugation that step 4) is obtained, obtain novel multiple strontium molybdate micro-nano structures with acetone, secondary water and absolute ethyl alcohol flush away unnecessary surfactant and water respectively.Compared with prior art, the present invention has following characteristics:
1, the multiple strontium molybdate micro-nano structures of the novelty among the present invention is formed in the microemulsion water nuclear, by the parameter that forms microemulsion is adjusted, and then the particle diameter and the structure of control microemulsion water nuclear, obtains the strontium molybdate micro-nano structures of desired pattern.
2, the present invention at room temperature carries out, mild condition and easily control, and noenergy consumption, cost is low.
3, the present invention can be widely used in the preparation of the flower-shaped inorganic functional material of other 3D.
Description of drawings
Fig. 1 is the SEM figure of the flower-shaped strontium molybdate of 3D of the embodiment of the invention 1 preparation;
Fig. 2 is the SEM figure of the spindle shape strontium molybdate of the embodiment of the invention 2 preparations;
Fig. 3 has the SEM figure of hole 3D strontium molybdate for the petal top of the embodiment of the invention 3 preparations;
Fig. 4 is the SEM figure of the surperficial pertusate spindle shape strontium molybdate of the embodiment of the invention 4 preparations;
Fig. 5 is the X-ray diffractogram (XRD) of the flower-shaped strontium molybdate of 3D of the inventive method embodiment 1 preparation.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment, and the description of embodiment is only for ease of understanding the present invention, but not to the restriction of the present invention's protection.
Embodiment 1
Preparation comprises 0.1mol/LSr
2+SrCl
2Microemulsion, wherein the amount of substance concentration of surfactant is 0.25mol/L, and the mol ratio ω of water and surfactant is 10, and all the other are oil phase content; Make corresponding each constituent content and SrCl
2The MoO of microemulsion unanimity
4 2-Na
2MoO
4Microemulsion.Under the stirring at room condition, with SrCl
2Microemulsion dropwise adds Na
2MoO
4In the microemulsion, dropwise the back and continue to stir 30 minutes, stop to stir the back with preservative film with the sealing of beaker mouth, under room temperature still aging 48 hours again.Centrifugation, washing obtain the flower-shaped strontium molybdate of 3D, as shown in Figure 1.In the confinement space, be self-assembled into the novel flower-shaped strontium molybdate micro-nano structures of 3D in formed spindle shape strontium molybdate structure under this condition, and the particle size of this structure is even.
Embodiment 2
Preparation comprises 0.1mol/LSr
2+SrCl
2Microemulsion, wherein the amount of substance concentration of surfactant (alkyl polyoxyethylene (10) ether (OP-10)) surfactant is 0.25mol/L, and the mol ratio ω of water and surfactant is 20, and all the other are oil phase content; Make corresponding each constituent content and SrCl
2The MoO of microemulsion unanimity
4 2-Na
2MoO
4Microemulsion.Under the stirring at room condition, with SrCl
2Microemulsion dropwise joins Na
2MoO
4In the microemulsion, dropwise the back and continue to stir 30 minutes, stop to stir the back with preservative film sealing beaker mouth, under room temperature still aging 48 hours again.Centrifugation, washing obtain spindle shape strontium molybdate micro-nano structures, as shown in Figure 2.The change of water content has also changed the structure of microemulsion, and then influences the product pattern.
Embodiment 3
Preparation comprises 0.025mol/LSr
2+SrCl
2Microemulsion, wherein the amount of substance concentration of surfactant (alkyl polyoxyethylene (10) ether (OP-10)) surfactant is 0.25mol/L, and the mol ratio ω of water and surfactant is 10, and all the other are oil phase content; Make corresponding each constituent content and SrCl
2The MoO of microemulsion unanimity
4 2-Na
2MoO
4Microemulsion.Under the stirring at room condition, with SrCl
2Microemulsion dropwise adds Na
2MoO
4In the microemulsion, dropwise the back and continue to stir 30 minutes, stop to stir the back with preservative film sealing beaker mouth, under room temperature still aging 48 hours again.Centrifugation, washing obtain the flower-shaped strontium molybdate micro-nano structures of novel 3D that there is the cavity on the petal top, as shown in Figure 3.As seen SrCl
2The change of concentration of aqueous solution is influential to the surface micro-structure of product.
Embodiment 4
Preparation comprises 0.025mol/LSr
2+SrCl
2Microemulsion, wherein the amount of substance concentration of surfactant (alkyl polyoxyethylene (10) ether (OP-10)) surfactant is 0.25mol/L, and the mol ratio ω of water and surfactant is 20, and all the other are oil phase content; Make corresponding each constituent content and SrCl
2The MoO of microemulsion unanimity
4 2-Na
2MoO
4In the microemulsion.Under the stirring at room condition, with SrCl
2Microemulsion dropwise joins Na
2MoO
4In the microemulsion, dropwise the back and continue to stir 30 minutes, stop to stir the back with preservative film sealing beaker mouth, under room temperature still aging 48 hours again.Centrifugation, washing obtain surperficial pertusate spindle shape strontium molybdate micro-nano structures, as shown in Figure 4.
Claims (5)
1. the method for a synthesizing various strontium molybdate micro-nano structures at room temperature is characterized in that this preparation method selects raw material non-ionic surface active agent alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octyl alcohol and water [SrCl for use
2Or Na
2MoO
4The aqueous solution] form microemulsion, after each component of forming microemulsion is mixed, be prepared into the reverse micro emulsion of homogeneous transparent, will contain SrCl again
2Microemulsion dropwise add and contain Na
2MoO
4Microemulsion in, SrCl
2And Na
2MoO
4At confinement space internal reaction, after ageing, centrifugation, washing make multiple strontium molybdate micro-nano structures, concrete preparation process is as follows:
1), with raw material alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octyl alcohol and water [SrCl
2The aqueous solution] insert in the beaker of 50ml the quality percentage composition that selected alkyl polyoxyethylene (10) ether (OP-10) surfactant mixes with alcohol, water [SrCl
2The aqueous solution] amount of substance and the ratio ω of the amount of substance of alkyl polyoxyethylene (10) ether (OP-10), SrCl
2The concentration of the aqueous solution after above-mentioned each component mixing, stirred 30 minutes on constant temperature blender with magnetic force under the room temperature, was mixed with uniform SrCl
2Microemulsion;
2), with raw material alkyl polyoxyethylene (10) ether (OP-10), cyclohexane, n-octyl alcohol and water [Na
2MoO
4The aqueous solution] insert in the beaker of 50ml the quality percentage composition that selected alkyl polyoxyethylene (10) ether (OP-10) surfactant mixes with alcohol, water [Na
2MoO
4The aqueous solution] amount of substance and the ratio ω of the amount of substance of alkyl polyoxyethylene (10) ether (OP-10), Na
2MoO
4The concentration of solution after each component of said mixture fully mixed, stirred 30 minutes on constant temperature blender with magnetic force under the room temperature, was mixed with uniform Na
2MoO
4Microemulsion;
3), with Na
2MoO
4Microemulsion places on the constant temperature blender with magnetic force, at room temperature dropwise drips microemulsion SrCl
2Microemulsion is along with SrCl
2The adding of microemulsion, microemulsion become white gradually, dropwise the back and continue to stir 30 minutes;
4), with preservative film sealing beaker mouth, ageing at room temperature 72 hours;
5), reactant liquor centrifugation that step 4) is obtained, obtain novel multiple strontium molybdate micro-nano structures product with acetone, secondary water and absolute ethyl alcohol flush away unnecessary surfactant and water respectively.
2. the preparation method of the synthetic multiple strontium molybdate micro-nano structures of control is characterized in that the ratio P of the amount of substance of the amount of substance of described n-octyl alcohol and alkyl polyoxyethylene (10) ether (OP-10) is 0.5～2 under the room temperature according to claim 1.
3. the preparation method of the synthetic multiple strontium molybdate micro-nano structures of control is characterized in that described step 1), 2 under the room temperature according to claim 1) in the mol ratio ω of water and surfactant be 10～20.
4. the preparation method of the synthetic multiple flower-shaped strontium molybdate micro-nano structures of control is characterized in that Sr in the described step 3) under the room temperature according to claim 1
2+With MoO
4 2-Mol ratio be 1: 1.
5. the preparation method of the synthetic multiple strontium molybdate micro-nano structures of control is characterized in that the reaction time in the described step 4) is 36～48 hours under the room temperature according to claim 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984902A (en) * | 2016-02-19 | 2016-10-05 | 安徽大学 | Preparation method of strontium-molybdate-dopable nano material |
| CN106915773A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
| CN111592026A (en) * | 2020-05-11 | 2020-08-28 | 贺州学院 | Preparation method of discus-shaped micron calcium carbonate |
| CN114873642A (en) * | 2022-04-06 | 2022-08-09 | 同济大学 | Donut-shaped strontium molybdate nano material and preparation method thereof |
-
2009
- 2009-08-31 CN CN200910114355A patent/CN101691206A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984902A (en) * | 2016-02-19 | 2016-10-05 | 安徽大学 | Preparation method of strontium-molybdate-dopable nano material |
| CN105984902B (en) * | 2016-02-19 | 2018-06-29 | 安徽大学 | A kind of strontium molybdate nano material preparation method adulterated |
| CN106915773A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
| CN106915773B (en) * | 2017-05-04 | 2018-03-06 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
| CN111592026A (en) * | 2020-05-11 | 2020-08-28 | 贺州学院 | Preparation method of discus-shaped micron calcium carbonate |
| CN111592026B (en) * | 2020-05-11 | 2023-05-09 | 贺州学院 | Preparation method of discus-shaped micron calcium carbonate |
| CN114873642A (en) * | 2022-04-06 | 2022-08-09 | 同济大学 | Donut-shaped strontium molybdate nano material and preparation method thereof |
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Open date: 20100407 |