CN104860353A - Preparation method of cadmium molybdate hollow spheres assembled with nano-particles - Google Patents
Preparation method of cadmium molybdate hollow spheres assembled with nano-particles Download PDFInfo
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- CN104860353A CN104860353A CN201510180985.5A CN201510180985A CN104860353A CN 104860353 A CN104860353 A CN 104860353A CN 201510180985 A CN201510180985 A CN 201510180985A CN 104860353 A CN104860353 A CN 104860353A
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Abstract
The invention relates to the technical field of materials, and specifically relates to a preparation method of cadmium molybdate hollow spheres assembled with nano-particles. The method mainly comprises the following steps: a sodium molybdate solution, a cadmium sulfate solution and a sodium carbonate solution are respectively prepared; the obtained sodium molybdate solution is added into the cadmium sulfate solution; shaking is carried out, such that a mixture system with white precipitate is obtained; the mixture system is added into the obtained sodium carbonate solution, and shaking is carried out; the mixture is allowed to stand, such that a crude product is obtained; the crude product is separated, washed and dried, such that a target product is obtained. The process provided by the invention is simple. The prepared cadmium molybdate hollow spheres assembled with nano-particles have photocatalysis and adsorption dual functions, and can be used in the field of environment protection.
Description
Technical field
The invention belongs to field of material technology, be specifically related to a kind of preparation method of the molybdic acid cadmium hollow ball assembled by nano particle.
Background technology
Since the second half in 20th century, people strengthen gradually for the consciousness of environment protection.Organic dye also becomes the very important main source of water pollution while the world bringing people's riot of color, great on health of people impact.For eliminating its negative impact as far as possible, scientists study goes out photocatalytic method and absorption method two kinds of typical treatment processs.
Photocatalytic method mainly utilizes nano level semiconductor material to photoabsorption, and produce electron-hole pair, mineralizing and degrading dyestuff carries out water pollution process.But in a lot of situation, people will apply photocatalytic method and carry out water pollution process and need to face a comparatively severe problem, that is: nano-scale photocatalyst too disperses, and particle is little, not easily separated.
And absorption method be generally utilize the vesicular structure of sorbing material to have high-specific surface area to carry out water pollution process.But absorption method, can not thorough decomposing organic matter compared to photocatalytic method.
As everyone knows, molybdic acid cadmium is a based semiconductor material, and Absorbable rod utilizes ultra violet applications in photocatalysis field.If nano level molybdic acid cadmium groups of grains is dressed up hollow structure, the photocatalysis property of cadmium molybdate nano ball can not only be kept, and the hollow structure be assembled into has comparatively bigger serface, adsorbable more organic dye, contribute to strengthening photo-catalysis function.
Under the guiding of this thinking, research and develop a kind of material with absorption and photochemical catalysis dual-use function and have important practical significance.
Summary of the invention
An object of the present invention is for the deficiencies in the prior art, research and develop and a kind of there is absorption and the material of photochemical catalysis dual-use function, described in there is absorption and photochemical catalysis dual-use function material adopt solution at room temperature method and prepare by Oswald that moral slaking (Ostwald Ripening) mechanism and obtain.
The invention provides a kind of preparation method of the molybdic acid cadmium hollow ball assembled by nano particle, comprise the steps:
Step 1: take deionized water as solvent, compound concentration is the sodium molybdate solution of 0.1mol/L.
Step 2: take deionized water as solvent, compound concentration is the cadmium sulfate solution of 0.1 ~ 0.4mol/L.
Step 3: take deionized water as solvent, compound concentration is the sodium carbonate solution of 0.3mol/L.
Step 4: measure the sodium molybdate solution obtained in step 1 and join in the cadmium sulfate solution obtained in step 2, obtains the mixture system that has white precipitate after rocking certain hour.
Step 5: joined by the mixture system obtained in step 4 in the diluent of the sodium carbonate solution obtained in step 3, leaves standstill after rocking certain hour, obtains thick product.
Step 6: namely obtain target product by after centrifugal for the thick product obtained in step 5, washing, drying.
Say further, the purity of the Sodium orthomolybdate of medicine described in step 1 ~ 3, Cadmium Sulphate and sodium carbonate is not less than chemical pure.
Say further, in the mixture system obtained in described step 4, molybdenum acid ion is 1.5:1 with the ratio of the amount of substance of cadmium ion.
Say further, the time of rocking in described step 4 is no more than 15s.
Say further, in the thick product obtained in described step 5, carbanion is 1:1 with the ratio of the amount of substance of molybdenum acid ion.
Say further, the time of rocking in described step 5 is 5 ~ 20s, and time of repose is 1 ~ 20h.
Say further, the concrete operations of described step 6 be the thick product that obtains in step 5 is centrifugal after, adopt the alternately washing of deionized water, dehydrated alcohol, acetone, after drying, namely obtain target product.
Furthermore, the consumption of described deionized water, dehydrated alcohol, acetone is take washing leaching cake as mark, and the mass ratio of deionized water, dehydrated alcohol, acetone and washing leaching cake is 20:20:20:1.
Furthermore, described alternately washing times is 3 ~ 6 times.
Furthermore, described drying temperature is 60 ~ 80 DEG C, and time of drying is 4 ~ 8h.
Beneficial effect of the present invention is:
1, present invention achieves under normal temperature and obtain in solution blending mode the molybdic acid cadmium hollow ball that is assembled into by nano particle, the Inorganic synthese for nano material provides a kind of new route of synthesis.
2, the present invention adopts simply common pharmaceutical chemicals to be precursors, and in preparation process, do not produce by product, environmental pollution is little, is a kind of environment-friendly type synthesis technique.
3, the present invention controls hollow ball size by the concentration of regulator solution, and solvent materials is easy to get, and strength of solution is easily adjusted, and products therefrom is easily separated, good dispersity.
4, the present invention does not use any organic additive or tensio-active agent, does not need other heating or hydro-thermal, simplifies the operation steps of hydro-thermal reaction etc., makes technique more simple, is convenient to industrial operation.
In brief, present invention process is simple, and whole preparation system easily builds, and easy and simple to handle, condition is easily controlled, with low cost, and target product pattern is homogeneous, and size is easily controlled, and purity is high, better crystallinity degree, and process is convenient succinct, is suitable for industrial mass production.And target product has the excellent properties of nano material, responsive to UV-irradiation, can photocatalytically degradating organic dye.Meanwhile, molybdic acid cadmium groups of grains is dressed up hollow ball, there is larger specific surface area, there is good adsorption function, especially very good to the adsorption effect of organic dye, be conducive to the realization of photo-catalysis function.The hollow ball that the present invention obtains has photochemical catalysis and adsorption dual function, can be used for field of environment protection.
Accompanying drawing explanation
Figure 1 shows that the structural characterization figure of the molybdic acid cadmium hollow ball assembled by nano particle that the method for the invention obtains.
Wherein, (a) is XRD figure, and (b) is FE-SEM figure.
Figure 2 shows that the FE-SEM figure of the embodiment of the present invention 1 ~ 4 products therefrom.
Wherein (a) schemes for embodiment 1 products obtained therefrom FE-SEM, and (b) schemes for embodiment 2 products obtained therefrom FE-SEM, and (c) schemes for embodiment 3 products obtained therefrom FE-SEM, and (d) schemes for embodiment 4 products obtained therefrom FE-SEM.
Embodiment
The invention provides a kind of preparation method of the molybdic acid cadmium hollow ball assembled by nano particle, comprise the steps:
Step 1: take deionized water as solvent, compound concentration is the sodium molybdate solution of 0.1mol/L.
Step 2: take deionized water as solvent, compound concentration is the cadmium sulfate solution of 0.1 ~ 0.4mol/L.
Step 3: take deionized water as solvent, compound concentration is the sodium carbonate solution of 0.3mol/L.
Step 4: measure the sodium molybdate solution obtained in step 1 and join in the cadmium sulfate solution obtained in step 2, obtains the mixture system that has white precipitate after rocking certain hour.
Step 5: joined by the mixture system obtained in step 4 in the diluent of the sodium carbonate solution obtained in step 3, leaves standstill after rocking certain hour, obtains thick product.
Step 6: namely obtain target product by after centrifugal for the thick product obtained in step 5, washing, drying.
Say further, the purity of the Sodium orthomolybdate of medicine described in step 1 ~ 3, Cadmium Sulphate and sodium carbonate is not less than chemical pure.
Say further, in the mixture system obtained in described step 4, molybdenum acid ion is 1.5:1 with the ratio of the amount of substance of cadmium ion.
Say further, the time of rocking in described step 4 is no more than 15s.
Say further, in the thick product obtained in described step 5, carbanion is 1:1 with the ratio of the amount of substance of molybdenum acid ion.
Say further, the time of rocking in described step 5 is 5 ~ 20s, and time of repose is 1 ~ 20h.
Say further, the concrete operations of described step 6 be the thick product that obtains in step 5 is centrifugal after, adopt the alternately washing of deionized water, dehydrated alcohol, acetone, after drying, namely obtain target product.
Furthermore, the consumption of described deionized water, dehydrated alcohol, acetone is take washing leaching cake as mark, and the mass ratio of deionized water, dehydrated alcohol, acetone and washing leaching cake is 20:20:20:1.
Furthermore, described alternately washing times is 3 ~ 6 times.
Furthermore, described drying temperature is 60 ~ 80 DEG C, and time of drying is 4 ~ 8h.
Hereafter will in conjunction with specific embodiments and accompanying drawing describe the present invention.It should be noted that the combination of technical characteristic or the technical characteristic described in following embodiment should not be considered to isolated, they can mutually be combined thus be reached better technique effect.
Embodiment 1
Preparing sodium molybdate solution concentration is 0.1mol/L, and cadmium sulfate solution concentration is 0.4mol/L, gained molybdic acid cadmium hollow ball when sodium carbonate solution volume is 13mL after dilution.
Preparation method:
(1) to scale be 10mL centrifuge tube in add the cadmium sulfate solution of 1mL 0.4mol/L, then the sodium molybdate solution of 6mL 0.1mol/L is poured in described cadmium sulfate solution, after rocking a little, obtains white suspension.
(2) white suspension in centrifuge tube is distributed to (wherein, the amount of substance of sodium carbonate is 0.0006mol) in the 13mL sodium carbonate solution be loaded in 50mL beaker, rocks latter standing 1 hour a little.Precipitated product after leaving standstill is transferred to centrifugation in centrifuge tube, alternately use deionized water, dehydrated alcohol and acetone (wherein, the consumption of deionized water, dehydrated alcohol, acetone is: take washing leaching cake as mark, deionized water, dehydrated alcohol, acetone consumption are its 20 times respectively) wash 3 times respectively, after each washing completes, centrifugation.Namely final gained centrifugal sediment dry 4h at 80 DEG C obtains target product.
Figure 1 shows that the structural characterization figure of the molybdic acid cadmium hollow ball assembled by nano particle that the method for the invention obtains, wherein, (a) is XRD figure, and (b) is FE-SEM figure.The X-ray powder diffraction pattern of the present embodiment products therefrom and the substantially identical of Fig. 1 (a), therefore do not repeat to list, gained peak is the diffraction peak of molybdic acid cadmium crystal.Fig. 2 (a) is depicted as field emission scanning electron microscope (FE-SEM) photo of the present embodiment product, and products therefrom is the hollow ball that tiny nano particle is assembled into as seen from the figure, and its size is at 400 ~ 600nm.
Embodiment 2
Preparing sodium molybdate solution concentration is 0.1mol/L, and cadmium sulfate solution concentration is 0.2mol/L, gained molybdic acid cadmium hollow ball when sodium carbonate solution volume is 12mL after dilution.
Preparation method:
(1) to scale be 10mL centrifuge tube in add the cadmium sulfate solution of 2mL 0.2mol/L, then pour the sodium molybdate solution of 6mL 0.1mol/L into described cadmium sulfate solution, after rocking a little, obtain white suspension.
(2) white suspension in centrifuge tube is distributed to (wherein, the amount of substance of sodium carbonate is 0.0006mol) in the 12mL sodium carbonate solution be loaded in 50mL beaker, rocks latter standing 1 hour a little.Precipitated product after leaving standstill is transferred to centrifugation in centrifuge tube, alternately use deionized water, dehydrated alcohol and acetone (wherein, the consumption of deionized water, dehydrated alcohol, acetone is: take washing leaching cake as mark, deionized water, dehydrated alcohol, acetone consumption are its 20 times respectively) wash 3 times respectively, after each washing completes, centrifugation, namely final gained centrifugal sediment dry 8h at 60 DEG C obtains target product.
The X-ray powder diffraction pattern of the present embodiment products therefrom and the substantially identical of Fig. 1 (a), therefore do not repeat to list, gained peak is the diffraction peak of molybdic acid cadmium crystal.Fig. 2 (b) is depicted as field emission scanning electron microscope (FE-SEM) photo of the present embodiment product, and product is the hollow ball that tiny nano particle is assembled into as seen from the figure, and its size is in 500 ~ 1000 nanometers.
Embodiment 3
Preparing sodium molybdate solution concentration is 0.1mol/L, and cadmium sulfate solution concentration is 0.133mol/L, gained molybdic acid cadmium hollow ball when sodium carbonate solution volume is 11mL after dilution.
Preparation method:
(1) to scale be 10mL centrifuge tube in add the cadmium sulfate solution of 3mL 0.133mol/L, then pour the sodium molybdate solution of 6mL0.1mol/L into described cadmium sulfate solution, after rocking a little, obtain white suspension.
(2) white suspension in centrifuge tube is distributed to (wherein, the amount of substance of sodium carbonate is 0.0006mol) in the 11mL sodium carbonate solution be loaded in 50mL beaker, rocks latter standing 1 hour a little.Precipitated product after leaving standstill is transferred to centrifugation in centrifuge tube, alternately use deionized water, dehydrated alcohol and acetone (wherein, the consumption of deionized water, dehydrated alcohol, acetone is: take washing leaching cake as mark, deionized water, dehydrated alcohol, acetone consumption are its 20 times respectively) wash 3 times respectively, after each washing completes, centrifugation, namely final gained centrifugal sediment dry 6h at 60 DEG C obtains target product
The X-ray powder diffraction pattern of the present embodiment products therefrom and the substantially identical of Fig. 1 (a), therefore do not repeat to list, gained peak is the diffraction peak of molybdic acid cadmium crystal.Fig. 2 (c) is depicted as field emission scanning electron microscope (FE-SEM) photo of the present embodiment product, and product is the hollow ball that tiny nano particle is assembled into as seen from the figure, and its size is in 1000 ~ 1500 nanometers.
Embodiment 4
Preparing sodium molybdate solution concentration is 0.1mol/L, and cadmium sulfate solution concentration is 0.1mol/L, gained molybdic acid cadmium hollow ball when sodium carbonate solution volume is 10mL after dilution.
Preparation method:
(1) to scale be 10mL centrifuge tube in add the cadmium sulfate solution of 4mL 0.1mol/L, then pour the sodium molybdate solution of 6mL 0.1mol/L into described cadmium sulfate solution, after rocking a little, obtain white suspension.
(2) white suspension in centrifuge tube is distributed to (wherein, the amount of substance of sodium carbonate is 0.0006mol) in the 10mL sodium carbonate solution be loaded in 50mL beaker, rocks latter standing 1 hour a little.Precipitated product after leaving standstill is transferred to centrifugation in centrifuge tube, alternately use deionized water, dehydrated alcohol and acetone (wherein, the consumption of deionized water, dehydrated alcohol, acetone is: take washing leaching cake as mark, deionized water, dehydrated alcohol, acetone consumption are its 20 times respectively) wash 3 times respectively, after each washing completes, centrifugation, namely final gained centrifugal sediment dry 6h at 70 DEG C obtains target product.
The X-ray powder diffraction pattern of the present embodiment products therefrom and the substantially identical of Fig. 1 (a), therefore do not repeat to list, gained peak is the diffraction peak of molybdic acid cadmium crystal.Fig. 2 (d) is depicted as field emission scanning electron microscope (FE-SEM) photo of the present embodiment product, and product is the hollow ball that tiny nano particle is assembled into as seen from the figure, and its size is at 1500 ran.
Present invention process is simple, and obtained target product has the excellent properties of nano material, responsive to UV-irradiation, can photocatalytically degradating organic dye.Meanwhile, molybdic acid cadmium groups of grains is dressed up hollow ball, there is larger specific surface area, there is good adsorption function, especially very good to the adsorption effect of organic dye, be conducive to the realization of photo-catalysis function.The hollow ball that the present invention obtains has photochemical catalysis and adsorption dual function, can be used for field of environment protection.
Although give some embodiments of the present invention, it will be understood by those of skill in the art that without departing from the spirit of the invention herein, can change embodiment herein.Above-described embodiment is exemplary, should using embodiment herein as the restriction of interest field of the present invention.
Claims (10)
1. a preparation method for the molybdic acid cadmium hollow ball assembled by nano particle, is characterized in that, comprise the steps:
Step 1: take deionized water as solvent, compound concentration is the sodium molybdate solution of 0.1mol/L;
Step 2: take deionized water as solvent, compound concentration is the cadmium sulfate solution of 0.1 ~ 0.4mol/L;
Step 3: take deionized water as solvent, compound concentration is the sodium carbonate solution of 0.3mol/L;
Step 4: measure the sodium molybdate solution obtained in step 1 and join in the cadmium sulfate solution obtained in step 2, obtains the mixture system that has white precipitate after rocking certain hour;
Step 5: joined by the mixture system obtained in step 4 in the diluent of the sodium carbonate solution obtained in step 3, leaves standstill after rocking certain hour, obtains thick product;
Step 6: namely obtain target product by after centrifugal for the thick product obtained in step 5, washing, drying.
2. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 1, it is characterized in that, the purity of the Sodium orthomolybdate of medicine described in step 1 ~ 3, Cadmium Sulphate and sodium carbonate is not less than chemical pure.
3. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 1, it is characterized in that, in the mixture system obtained in described step 4, molybdenum acid ion is 1.5:1 with the ratio of the amount of substance of cadmium ion.
4. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 1, it is characterized in that, the time of rocking in described step 4 is no more than 15s.
5. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 1, it is characterized in that, in the thick product obtained in described step 5, carbanion is 1:1 with the ratio of the amount of substance of molybdenum acid ion.
6. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 1, it is characterized in that, the time of rocking in described step 5 is 5 ~ 20s, and time of repose is 1 ~ 20h.
7. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 1, it is characterized in that, the concrete operations of described step 6 be the thick product that obtains in step 5 is centrifugal after, adopt the alternately washing of deionized water, dehydrated alcohol, acetone, after drying, namely obtain target product.
8. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 7, it is characterized in that, the consumption of described deionized water, dehydrated alcohol, acetone is take washing leaching cake as mark, and the mass ratio of deionized water, dehydrated alcohol, acetone and washing leaching cake is 20:20:20:1.
9. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 7, is characterized in that, described alternately washing times is 3 ~ 6 times.
10. the preparation method of a kind of molybdic acid cadmium hollow ball assembled by nano particle as claimed in claim 7, it is characterized in that, described drying temperature is 60 ~ 80 DEG C, and time of drying is 4 ~ 8h.
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Cited By (2)
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| CN109012683A (en) * | 2018-08-09 | 2018-12-18 | 扬州大学 | A kind of preparation method of cobalt molybdate tiny balloon elctro-catalyst |
| CN109336178A (en) * | 2018-12-06 | 2019-02-15 | 洛阳理工学院 | A kind of preparation method of molybdic acid cadmium skeleton |
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| CN101665269A (en) * | 2009-08-31 | 2010-03-10 | 广西民族大学 | Preparation method of cadmium molybdate octahedron with controllable grain size |
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| CN101665269A (en) * | 2009-08-31 | 2010-03-10 | 广西民族大学 | Preparation method of cadmium molybdate octahedron with controllable grain size |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012683A (en) * | 2018-08-09 | 2018-12-18 | 扬州大学 | A kind of preparation method of cobalt molybdate tiny balloon elctro-catalyst |
| CN109012683B (en) * | 2018-08-09 | 2021-05-14 | 扬州大学 | Preparation method of cobalt molybdate hollow microsphere electrocatalyst |
| CN109336178A (en) * | 2018-12-06 | 2019-02-15 | 洛阳理工学院 | A kind of preparation method of molybdic acid cadmium skeleton |
| CN109336178B (en) * | 2018-12-06 | 2020-12-08 | 洛阳理工学院 | Preparation method of cadmium molybdate dendritic crystal |
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