CN104671285A - Method for preparing cadmium molybdate nanorod - Google Patents
Method for preparing cadmium molybdate nanorod Download PDFInfo
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- CN104671285A CN104671285A CN201510042640.3A CN201510042640A CN104671285A CN 104671285 A CN104671285 A CN 104671285A CN 201510042640 A CN201510042640 A CN 201510042640A CN 104671285 A CN104671285 A CN 104671285A
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- C01—INORGANIC CHEMISTRY
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- C01G39/00—Compounds of molybdenum
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/10—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
The invention discloses a method for preparing a cadmium molybdate nanorod. The method comprises the following steps: mixing a cadmium chloride solution and a potassium carbonate solution, and reacting to obtain a cadmium carbonate precipitate; mixing the precipitate with a sodium tungstate solution, adding the mixture into a reaction kettle, preserving the temperature to 110-150 DEG C for 2-6 hours, and performing hydrothermal treatment; naturally cooling to room temperature, adding sodium molybdate powder, preserving the temperature to 180-220 DEG C for 8-12 hours, and performing hydrothermal treatment; and naturally cooling the reaction kettle to room temperature, discharging the kettle, repeatedly washing the reaction product by using distilled water, filtering, and drying, thereby obtaining the cadmium molybdate nanorod. The preparation of the cadmium molybdate nanorod having a one-dimensional structure is realized at the first time, the preparation method has the advantages that the process flow is simple, any organic surfactant is not used and the pollution is avoided, industrial production is easily realized, and the cadmium molybdate nanorod has wide application values in the fields of photoluminescence, optical fibers and sensors.
Description
Technical field
The present invention relates to a kind of preparation method of molybdic acid cadmium material, particularly a kind of preparation method of cadmium molybdate nano rod.
Background technology
Molybdic acid cadmium (CdMoO
4) there is scheelite-type structure, be a kind of important inorganic materials.Because molybdic acid cadmium has superior luminescent properties and good colour developing, discoloration effect, have broad application prospects in photocatalyst material, scintillator detector, magneticsubstance, photoluminescence, optical fiber, laserable material, a lot of field of sensor, thus become the study hotspot of Material Field in recent years.
As everyone knows, the performance of nano material depends on the factor such as pattern and size of nanocrystal, novel, the special nano material of pattern can show unique performance, particularly monodimension nanometer material and have process based prediction model excellent especially because having higher length-to-diameter ratio and specific surface area.
At present, the molybdic acid cadmium material adopting hydrothermal method to prepare can only obtain spherical morphology powder granule usually, and the octahedra molybdic acid cadmium crystallite adopting microemulsion method to synthesize is because adding large amount of organic, for subsequent disposal brings inconvenience.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method preparing bar-shaped cadmium molybdate nano material.
The present invention for solving the problems of the technologies described above adopted technical scheme is: a kind of preparation method of cadmium molybdate nano rod, comprises the steps:
Step one, Cadmium chloride fine powder is dissolved in deionized water, form the Cadmium chloride fine powder aqueous solution, the concentration of the Cadmium chloride fine powder in regulator solution is 0.1-3.0mol/L; Salt of wormwood is dissolved in deionized water, and form wet chemical, the concentration of the salt of wormwood in regulator solution is 0.1-3.0mol/L; Sodium wolframate is dissolved in deionized water, and form the sodium wolframate aqueous solution, the concentration of the sodium wolframate in regulator solution is 0.1-3.0mol/L;
Step 2, cadmium chloride solution step one obtained and solution of potassium carbonate hybrid reaction, obtain cadmium carbonate precipitation;
Mixture joins in reactor inner bag after precipitating and mixing by the cadmium carbonate that step 3, sodium tungstate solution step one obtained and step 2 obtain, and regulates the volume of reaction mass in reactor inner bag to reach the 70%-90% of reactor inner bag volume with distilled water;
Step 4, the reactor inner bag that reaction mass is housed in step 3 is placed in reactor, sealing, is incubated 2-6 hour and carries out hydrothermal treatment consists, then reactor is naturally cooled to room temperature at 110-150 DEG C;
Step 5, the reactor being cooled to room temperature in step 4 is opened after, in reactor inner bag, add Sodium orthomolybdate powder;
Step 6, the reactor inner bag that reaction mass is housed in step 5 is placed in reactor, sealing, at 180-220 DEG C, be incubated 8-12 hour carry out hydrothermal treatment consists, then reactor is naturally cooled to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, and filter, obtain molybdic acid Cd monocrystal nanometer rod after drying.
In described step 5, to react the cadmium tungstate molar weight generated equal for add-on and the step 4 of Sodium orthomolybdate powder.
The invention has the beneficial effects as follows: the present invention adopts hydrothermal method successfully to prepare first to have the molybdic acid Cd monocrystal nanometer rod of one-dimentional structure, and the performance of its uniqueness has huge development potentiality and wide application prospect in photocatalyst material, photoluminescence, laserable material, sensor field.The preparation method of cadmium molybdate nano rod provided by the invention has simple to operate, inapplicable any organic surface active agent, is easy to realize the advantages such as suitability for 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.
Embodiment
A preparation method for cadmium molybdate nano rod, comprises the steps:
Step one, Cadmium chloride fine powder is dissolved in deionized water, form the Cadmium chloride fine powder aqueous solution, the concentration of the Cadmium chloride fine powder in regulator solution is 0.1-3.0mol/L; Salt of wormwood is dissolved in deionized water, and form wet chemical, the concentration of the salt of wormwood in regulator solution is 0.1-3.0mol/L; Sodium wolframate is dissolved in deionized water, and form the sodium wolframate aqueous solution, the concentration of the sodium wolframate in regulator solution is 0.1-3.0mol/L;
Step 2, cadmium chloride solution step one obtained and solution of potassium carbonate hybrid reaction, obtain cadmium carbonate precipitation;
Mixture joins in reactor inner bag after precipitating and mixing by the cadmium carbonate that step 3, sodium tungstate solution step one obtained and step 2 obtain, and regulates the volume of reaction mass in reactor inner bag to reach the 70%-90% of reactor inner bag volume with distilled water;
Step 4, the reactor inner bag that reaction mass is housed in step 3 is placed in reactor, sealing, is incubated 2-6 hour and carries out hydrothermal treatment consists, then reactor is naturally cooled to room temperature at 110-150 DEG C;
Step 5, the reactor being cooled to room temperature in step 4 is opened after, in reactor inner bag, add Sodium orthomolybdate powder;
Step 6, the reactor inner bag that reaction mass is housed in step 5 is placed in reactor, sealing, at 180-220 DEG C, be incubated 8-12 hour carry out hydrothermal treatment consists, then reactor is naturally cooled to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, and filter, obtain molybdic acid Cd monocrystal nanometer rod after drying.
In described step 5, to react the cadmium tungstate molar weight generated equal for add-on and the step 4 of Sodium orthomolybdate powder.
In preparation process, necessary elder generation for raw material with Cadmium chloride fine powder, sodium wolframate and salt of wormwood, prepares cadmium tungstate as reaction precursor, then mixes mutually with Sodium orthomolybdate and carry out hydro-thermal reaction, otherwise can not get molybdic acid Cd monocrystal nanometer rod.
The purity of described Cadmium chloride fine powder, salt of wormwood, sodium wolframate, Sodium orthomolybdate is all not less than chemical pure.
Below in conjunction with the drawings and specific embodiments, the present invention is further described.
Embodiment 1
Step one, Cadmium chloride fine powder is dissolved in deionized water, form the Cadmium chloride fine powder aqueous solution, the concentration of the Cadmium chloride fine powder in regulator solution is 0.16mol/L;
Step 2, salt of wormwood is dissolved in deionized water, form wet chemical, the concentration of the salt of wormwood in regulator solution is 0.16mol/L;
Step 3, sodium wolframate is dissolved in deionized water, form the sodium wolframate aqueous solution, the concentration of the sodium wolframate in regulator solution is 0.16mol/L;
The solution of potassium carbonate that step 4, cadmium chloride solution step one obtained and step 2 obtain, according to mol ratio 1:1 hybrid reaction, obtains cadmium carbonate precipitation;
After the cadmium carbonate that step 5, the sodium tungstate solution and the step 4 that step 3 are obtained obtain precipitates and mixes according to mol ratio 1:1, mixture is joined in reactor inner bag, regulate the volume of reaction mass in reactor inner bag to reach 70% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that reaction mass is housed in step 5 is placed in reactor, sealing, at 120 DEG C, insulation carries out hydrothermal treatment consists in 6 hours, then reactor is naturally cooled to room temperature, and obtained cadmium tungstate is as reaction precursor;
Step 7, the reactor being cooled to room temperature in step 6 is opened after, in reactor inner bag, add the equimolar Sodium orthomolybdate powder with cadmium tungstate;
Step 8, the reactor inner bag that reaction mass is housed in step 7 is placed in reactor, sealing, 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 repetitive scrubbing reaction product, and filter, obtain molybdic acid Cd monocrystal nanometer rod after drying.
Products therefrom X-ray diffraction (XRD) of the present invention is characterized, as shown in Figure 1, can find out that product is typical molybdic acid cadmium diffraction peak, and without any impurity, diffraction peak comparatively sharply shows that the crystallinity of product is fine; Characterized by products therefrom transmission electron microscope (TEM), as shown in Figure 2, molybdic acid cadmium crystal is club shaped structure, and length is about 300-400nm, and diameter is about 20-40nm.
Embodiment 2
Step one, Cadmium chloride fine powder is dissolved in deionized water, form the Cadmium chloride fine powder aqueous solution, the concentration of the Cadmium chloride fine powder in regulator solution is 1.8mol/L;
Step 2, salt of wormwood is dissolved in deionized water, form wet chemical, the concentration of the salt of wormwood in regulator solution is 1.8mol/L;
Step 3, sodium wolframate is dissolved in deionized water, form the sodium wolframate aqueous solution, the concentration of the sodium wolframate in regulator solution is 1.8mol/L;
The solution of potassium carbonate that step 4, cadmium chloride solution step one obtained and step 2 obtain, according to mol ratio 1:1 hybrid reaction, obtains cadmium carbonate precipitation;
After the cadmium carbonate that step 5, the sodium tungstate solution and the step 4 that step 3 are obtained obtain precipitates and mixes according to mol ratio 1:1, mixture is joined in reactor inner bag, regulate the volume of reaction mass in reactor inner bag to reach 80% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that reaction mass is housed in step 5 is placed in reactor, sealing, at 130 DEG C, insulation carries out hydrothermal treatment consists in 4 hours, then reactor is naturally cooled to room temperature, and obtained cadmium tungstate is as reaction precursor;
Step 7, the reactor being cooled to room temperature in step 6 is opened after, in reactor inner bag, add the equimolar Sodium orthomolybdate powder with cadmium tungstate;
Step 8, the reactor inner bag that reaction mass is housed in step 7 is placed in reactor, sealing, 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 repetitive scrubbing reaction product, and filter, obtain molybdic acid Cd monocrystal nanometer rod after drying.
Embodiment 3
Step one, Cadmium chloride fine powder is dissolved in deionized water, form the Cadmium chloride fine powder aqueous solution, the concentration of the Cadmium chloride fine powder in regulator solution is 2.9mol/L;
Step 2, salt of wormwood is dissolved in deionized water, form wet chemical, the concentration of the salt of wormwood in regulator solution is 2.9mol/L;
Step 3, sodium wolframate is dissolved in deionized water, form the sodium wolframate aqueous solution, the concentration of the sodium wolframate in regulator solution is 2.9mol/L;
The solution of potassium carbonate that step 4, cadmium chloride solution step one obtained and step 2 obtain, according to mol ratio 1:1 hybrid reaction, obtains cadmium carbonate precipitation;
After the cadmium carbonate that step 5, the sodium tungstate solution and the step 4 that step 3 are obtained obtain precipitates and mixes according to mol ratio 1:1, mixture is joined in reactor inner bag, regulate the volume of reaction mass in reactor inner bag to reach 90% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that reaction mass is housed in step 5 is placed in reactor, sealing, at 150 DEG C, insulation carries out hydrothermal treatment consists in 2 hours, then reactor is naturally cooled to room temperature, and obtained cadmium tungstate is as reaction precursor;
Step 7, the reactor being cooled to room temperature in step 6 is opened after, in reactor inner bag, add the equimolar Sodium orthomolybdate powder with cadmium tungstate;
Step 8, the reactor inner bag that reaction mass is housed in step 7 is placed in reactor, sealing, 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 repetitive scrubbing reaction product, and filter, obtain molybdic acid Cd monocrystal nanometer rod after drying.
Claims (2)
1. a preparation method for cadmium molybdate nano rod, is characterized in that: comprise the steps:
Step one, Cadmium chloride fine powder is dissolved in deionized water, form the Cadmium chloride fine powder aqueous solution, the concentration of the Cadmium chloride fine powder in regulator solution is 0.1-3.0mol/L; Salt of wormwood is dissolved in deionized water, and form wet chemical, the concentration of the salt of wormwood in regulator solution is 0.1-3.0mol/L; Sodium wolframate is dissolved in deionized water, and form the sodium wolframate aqueous solution, the concentration of the sodium wolframate in regulator solution is 0.1-3.0mol/L;
Step 2, cadmium chloride solution step one obtained and solution of potassium carbonate hybrid reaction, obtain cadmium carbonate precipitation;
Mixture joins in reactor inner bag after precipitating and mixing by the cadmium carbonate that step 3, sodium tungstate solution step one obtained and step 2 obtain, and regulates the volume of reaction mass in reactor inner bag to reach the 70%-90% of reactor inner bag volume with distilled water;
Step 4, the reactor inner bag that reaction mass is housed in step 3 is placed in reactor, sealing, is incubated 2-6 hour and carries out hydrothermal treatment consists, then reactor is naturally cooled to room temperature at 110-150 DEG C;
Step 5, the reactor being cooled to room temperature in step 4 is opened after, in reactor inner bag, add Sodium orthomolybdate powder;
Step 6, the reactor inner bag that reaction mass is housed in step 5 is placed in reactor, sealing, at 180-220 DEG C, be incubated 8-12 hour carry out hydrothermal treatment consists, then reactor is naturally cooled to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, and filter, obtain molybdic acid Cd monocrystal nanometer rod after drying.
2. the preparation method of a kind of cadmium molybdate nano rod according to claim 1, is characterized in that: in described step 5, to react the cadmium tungstate molar weight generated equal for add-on and the step 4 of Sodium orthomolybdate powder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055620A (en) * | 2017-05-11 | 2017-08-18 | 安徽建筑大学 | A kind of method that two one-step hydrothermal prepares CdWO4/MnWO4 composite nano materials |
| 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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| CN1464920A (en) * | 2001-07-12 | 2003-12-31 | 古河机械金属株式会社 | Method for preparing tungstate single crystal |
| CN1923704A (en) * | 2006-09-14 | 2007-03-07 | 上海交通大学 | Preparation method of octahedronlike cadmium molybdate crystal |
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1464920A (en) * | 2001-07-12 | 2003-12-31 | 古河机械金属株式会社 | Method for preparing tungstate single crystal |
| CN1923704A (en) * | 2006-09-14 | 2007-03-07 | 上海交通大学 | Preparation method of octahedronlike cadmium molybdate crystal |
| 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055620A (en) * | 2017-05-11 | 2017-08-18 | 安徽建筑大学 | A kind of method that two one-step hydrothermal prepares CdWO4/MnWO4 composite nano materials |
| 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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