CN104671285B - A kind of preparation method of cadmium molybdate nano rod - Google Patents
A kind of preparation method of cadmium molybdate nano rod Download PDFInfo
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- CN104671285B CN104671285B CN201510042640.3A CN201510042640A CN104671285B CN 104671285 B CN104671285 B CN 104671285B CN 201510042640 A CN201510042640 A CN 201510042640A CN 104671285 B CN104671285 B CN 104671285B
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
Abstract
A kind of preparation method of cadmium molybdate nano rod, cadmium chloride solution and solution of potassium carbonate hybrid reaction are obtained cadmium carbonate precipitation, then it is mixed to join reactor at 110 150 DEG C, to be incubated 26 hours carry out hydrothermal treatment consists with sodium tungstate solution, sodium molybdate powder is added after naturally cooling to room temperature, at 180 220 DEG C, insulation carries out hydrothermal treatment consists in 8 12 hours, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain molybdic acid Cd monocrystal nanometer rods after drying.Achieve the preparation of the cadmium molybdate nano rod of one-dimentional structure first, there is technical process and simply, do not use any organic surface active agent, the advantage such as pollution-free, it is easily achieved industrialized production, is with a wide range of applications in fields such as luminescence generated by light, optical fiber, sensors.
Description
Technical field
The present invention relates to the preparation method of a kind of molybdic acid cadmium material, the preparation method of a kind of cadmium molybdate nano rod.
Background technology
Molybdic acid cadmium (CdMoO4) there is scheelite-type structure, it is a kind of important inorganic material.Owing to molybdic acid cadmium has superior luminescent properties and good colour developing, discoloration effect, have broad application prospects in a lot of field such as catalysis material, scintillator detector, magnetic material, luminescence generated by light, optical fiber, laser material, sensor, thus become the study hotspot of Material Field in recent years.
It is known that, the performance of nano material depends on the factors such as pattern and the size of nanocrystal, novel, the special nano material of pattern can show the performance of uniqueness, particularly monodimension nanometer material and have process based prediction model excellent especially because having higher draw ratio and specific surface area.
At present, the molybdic acid cadmium material using hydro-thermal method to prepare is typically only capable to obtain spherical morphology powder granule, and uses the octahedra molybdic acid cadmium crystallite that microemulsion method synthesizes because adding large amount of organic, brings inconvenience for subsequent treatment.
Summary of the invention
The technical problem to be solved is to provide a kind of method preparing bar-shaped cadmium molybdate nano material.
The present invention solves that above-mentioned technical problem be the technical scheme is that the preparation method of a kind of cadmium molybdate nano rod, comprise the steps:
Step one, Caddy (Cleary) being dissolved in deionized water, form Caddy (Cleary) aqueous solution, the concentration of the Caddy (Cleary) in regulation solution is 0.1-3.0mol/L；Potassium carbonate being dissolved in deionized water, forms wet chemical, the concentration of the potassium carbonate in regulation solution is 0.1-3.0mol/L；Sodium tungstate being dissolved in deionized water, forms sodium tungstate aqueous solution, the concentration of the sodium tungstate in regulation solution is 0.1-3.0mol/L；
Step 2, cadmium chloride solution step one prepared and solution of potassium carbonate hybrid reaction, obtain cadmium carbonate precipitation；
After the cadmium carbonate precipitation that step 3, sodium tungstate solution step one prepared prepare with step 2 mixes, add mixture in reactor inner bag, reach the 70%-90% of reactor inner bag volume with the volume of reaction mass in distilled water regulation reactor inner bag；
Step 4, being placed in reactor by reactor inner bag equipped with reaction mass in step 3, seal, at 110-150 DEG C, insulation carries out hydrothermal treatment consists in 2-6 hour, then reactor is naturally cooled to room temperature；
Step 5, the reactor being cooled to room temperature in step 4 is opened after, in reactor inner bag add sodium molybdate powder；
Step 6, reactor inner bag equipped with reaction mass in step 5 is placed in reactor, seal, at 180-220 DEG C, insulation carries out hydrothermal treatment consists in 8-12 hour, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain molybdic acid Cd monocrystal nanometer rods after drying.
In described step 5 the addition of sodium molybdate powder react with step 4 generate cadmium tungstate mole equal.
The invention has the beneficial effects as follows: the present invention uses hydro-thermal method the most successfully to prepare the molybdic acid Cd monocrystal nanometer rods with one-dimentional structure, and the performance of its uniqueness has huge development potentiality and wide application prospect in fields such as catalysis material, luminescence generated by light, laser material, sensors.The preparation method of the cadmium molybdate nano rod that the present invention provides has any organic surface active agent simple to operate, inapplicable, is easily achieved the advantages such as industrialized production.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of cadmium molybdate nano rod prepared by the present invention；
Fig. 2 is transmission electron microscope (TEM) photo of cadmium molybdate nano rod prepared by the present invention.
Detailed description of the invention
The preparation method of a kind of cadmium molybdate nano rod, comprises the steps:
Step one, Caddy (Cleary) being dissolved in deionized water, form Caddy (Cleary) aqueous solution, the concentration of the Caddy (Cleary) in regulation solution is 0.1-3.0mol/L；Potassium carbonate being dissolved in deionized water, forms wet chemical, the concentration of the potassium carbonate in regulation solution is 0.1-3.0mol/L；Sodium tungstate being dissolved in deionized water, forms sodium tungstate aqueous solution, the concentration of the sodium tungstate in regulation solution is 0.1-3.0mol/L；
Step 2, cadmium chloride solution step one prepared and solution of potassium carbonate hybrid reaction, obtain cadmium carbonate precipitation；
After the cadmium carbonate precipitation that step 3, sodium tungstate solution step one prepared prepare with step 2 mixes, add mixture in reactor inner bag, reach the 70%-90% of reactor inner bag volume with the volume of reaction mass in distilled water regulation reactor inner bag；
Step 4, being placed in reactor by reactor inner bag equipped with reaction mass in step 3, seal, at 110-150 DEG C, insulation carries out hydrothermal treatment consists in 2-6 hour, then reactor is naturally cooled to room temperature；
Step 5, the reactor being cooled to room temperature in step 4 is opened after, in reactor inner bag add sodium molybdate powder；
Step 6, reactor inner bag equipped with reaction mass in step 5 is placed in reactor, seal, at 180-220 DEG C, insulation carries out hydrothermal treatment consists in 8-12 hour, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain molybdic acid Cd monocrystal nanometer rods after drying.
In described step 5 the addition of sodium molybdate powder react with step 4 generate cadmium tungstate mole equal.
In preparation process, it is necessary to first with Caddy (Cleary), sodium tungstate and potassium carbonate as raw material, prepare cadmium tungstate as reaction precursor, then mix mutually with sodium molybdate and carry out hydro-thermal reaction, otherwise can not get molybdic acid Cd monocrystal nanometer rods.
Described Caddy (Cleary), potassium carbonate, sodium tungstate, the purity of sodium molybdate are all not less than chemical pure.
With detailed description of the invention, the present invention is further described below in conjunction with the accompanying drawings.
Embodiment 1
Step one, Caddy (Cleary) being dissolved in deionized water, form Caddy (Cleary) aqueous solution, the concentration of the Caddy (Cleary) in regulation solution is 0.16mol/L；
Step 2, potassium carbonate being dissolved in deionized water, form wet chemical, the concentration of the potassium carbonate in regulation solution is 0.16mol/L；
Step 3, sodium tungstate being dissolved in deionized water, form sodium tungstate aqueous solution, the concentration of the sodium tungstate in regulation solution is 0.16mol/L；
The solution of potassium carbonate that step 4, cadmium chloride solution step one prepared and step 2 prepare, according to mol ratio 1:1 hybrid reaction, obtains cadmium carbonate precipitation；
After the cadmium carbonate precipitation that step 5, sodium tungstate solution step 3 prepared prepare with step 4 mixes according to mol ratio 1:1, add mixture in reactor inner bag, reach the 70% of reactor inner bag volume with the volume of reaction mass in distilled water regulation reactor inner bag；
Step 6, being placed in reactor by reactor inner bag equipped with reaction mass in step 5, seal, at 120 DEG C, insulation carries out hydrothermal treatment consists in 6 hours, then reactor is naturally cooled to room temperature, prepares cadmium tungstate as reaction precursor；
Step 7, the reactor being cooled to room temperature in step 6 is opened after, in reactor inner bag add with the equimolar sodium molybdate powder of cadmium tungstate；
Step 8, reactor inner bag equipped with reaction mass in step 7 is placed in reactor, seal, at 180 DEG C, insulation carries out hydrothermal treatment consists in 12 hours, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain molybdic acid Cd monocrystal nanometer rods after drying.
Products therefrom X-ray diffraction (XRD) of the present invention is characterized, as shown in Figure 1, it can be seen that product is typical molybdic acid cadmium diffraction maximum, and does not has any impurity, and diffraction maximum the most sharply shows that the crystallinity of product is fine；Being characterized by products therefrom transmission electron microscope (TEM), as in figure 2 it is shown, molybdic acid cadmium crystal is club shaped structure, length is about 300-400nm, and diameter is about 20-40nm.
Embodiment 2
Step one, Caddy (Cleary) being dissolved in deionized water, form Caddy (Cleary) aqueous solution, the concentration of the Caddy (Cleary) in regulation solution is 1.8mol/L；
Step 2, potassium carbonate being dissolved in deionized water, form wet chemical, the concentration of the potassium carbonate in regulation solution is 1.8mol/L；
Step 3, sodium tungstate being dissolved in deionized water, form sodium tungstate aqueous solution, the concentration of the sodium tungstate in regulation solution is 1.8mol/L；
The solution of potassium carbonate that step 4, cadmium chloride solution step one prepared and step 2 prepare, according to mol ratio 1:1 hybrid reaction, obtains cadmium carbonate precipitation；
After the cadmium carbonate precipitation that step 5, sodium tungstate solution step 3 prepared prepare with step 4 mixes according to mol ratio 1:1, add mixture in reactor inner bag, reach the 80% of reactor inner bag volume with the volume of reaction mass in distilled water regulation reactor inner bag；
Step 6, being placed in reactor by reactor inner bag equipped with reaction mass in step 5, seal, at 130 DEG C, insulation carries out hydrothermal treatment consists in 4 hours, then reactor is naturally cooled to room temperature, prepares cadmium tungstate as reaction precursor；
Step 7, the reactor being cooled to room temperature in step 6 is opened after, in reactor inner bag add with the equimolar sodium molybdate powder of cadmium tungstate；
Step 8, reactor inner bag equipped with reaction mass in step 7 is placed in reactor, seal, at 200 DEG C, insulation carries out hydrothermal treatment consists in 10 hours, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain molybdic acid Cd monocrystal nanometer rods after drying.
Embodiment 3
Step one, Caddy (Cleary) being dissolved in deionized water, form Caddy (Cleary) aqueous solution, the concentration of the Caddy (Cleary) in regulation solution is 2.9mol/L；
Step 2, potassium carbonate being dissolved in deionized water, form wet chemical, the concentration of the potassium carbonate in regulation solution is 2.9mol/L；
Step 3, sodium tungstate being dissolved in deionized water, form sodium tungstate aqueous solution, the concentration of the sodium tungstate in regulation solution is 2.9mol/L；
The solution of potassium carbonate that step 4, cadmium chloride solution step one prepared and step 2 prepare, according to mol ratio 1:1 hybrid reaction, obtains cadmium carbonate precipitation；
After the cadmium carbonate precipitation that step 5, sodium tungstate solution step 3 prepared prepare with step 4 mixes according to mol ratio 1:1, add mixture in reactor inner bag, reach the 90% of reactor inner bag volume with the volume of reaction mass in distilled water regulation reactor inner bag；
Step 6, being placed in reactor by reactor inner bag equipped with reaction mass in step 5, seal, at 150 DEG C, insulation carries out hydrothermal treatment consists in 2 hours, then reactor is naturally cooled to room temperature, prepares cadmium tungstate as reaction precursor；
Step 7, the reactor being cooled to room temperature in step 6 is opened after, in reactor inner bag add with the equimolar sodium molybdate powder of cadmium tungstate；
Step 8, reactor inner bag equipped with reaction mass in step 7 is placed in reactor, seal, at 220 DEG C, insulation carries out hydrothermal treatment consists in 8 hours, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain molybdic acid Cd monocrystal nanometer rods after drying.
Claims (2)
1. the preparation method of a cadmium molybdate nano rod, it is characterised in that: comprise the steps:
Step one, Caddy (Cleary) being dissolved in deionized water, form Caddy (Cleary) aqueous solution, the concentration of the Caddy (Cleary) in regulation solution is 0.16mol/L；Potassium carbonate being dissolved in deionized water, forms wet chemical, the concentration of the potassium carbonate in regulation solution is 0.16mol/L；Sodium tungstate being dissolved in deionized water, forms sodium tungstate aqueous solution, the concentration of the sodium tungstate in regulation solution is 0.16mol/L；
Step 2, cadmium chloride solution step one prepared and solution of potassium carbonate, according to mol ratio 1:1 hybrid reaction, obtain cadmium carbonate precipitation；
After the cadmium carbonate precipitation that step 3, sodium tungstate solution step one prepared prepare with step 2 mixes according to mol ratio 1:1, add mixture in reactor inner bag, reach the 70% of reactor inner bag volume with the volume of reaction mass in distilled water regulation reactor inner bag；
Step 4, being placed in reactor by reactor inner bag equipped with reaction mass in step 3, seal, at 120 DEG C, insulation carries out hydrothermal treatment consists in 6 hours, then reactor is naturally cooled to room temperature；
Step 5, the reactor being cooled to room temperature in step 4 is opened after, in reactor inner bag add sodium molybdate powder；
Step 6, reactor inner bag equipped with reaction mass in step 5 is placed in reactor, seal, at 180 DEG C, insulation carries out hydrothermal treatment consists in 12 hours, then reactor is naturally cooled to room temperature, after unloading still, by distilled water cyclic washing product, and filter, obtain after drying the molybdic acid Cd monocrystal nanometer rods of a length of 300-400nm.
A kind of cadmium molybdate nano the most according to claim 1 rod preparation method, it is characterised in that: in described step 5 the addition of sodium molybdate powder react with step 4 generation cadmium tungstate mole equal.
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| CN107055620B (en) * | 2017-05-11 | 2018-08-31 | 安徽建筑大学 | A kind of method that two one-step hydrothermals prepares CdWO4/MnWO4 composite nano materials |
| 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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| RU2241081C2 (en) * | 2001-07-12 | 2004-11-27 | Фурукава Ко., Лтд. | Method for producing tungstate mono-crystal |
| CN100389072C (en) * | 2006-09-14 | 2008-05-21 | 上海交通大学 | Preparation method of octahedronlike cadmium molybdate crystal |
| CN101665269B (en) * | 2009-08-31 | 2011-04-13 | 广西民族大学 | Preparation method of cadmium molybdate octahedron with controllable grain size |
| CN103833080B (en) * | 2014-03-25 | 2016-01-20 | 洛阳理工学院 | A kind of preparation method of molybdic acid cadmium porous ball |
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