CN109336178B - Preparation method of cadmium molybdate dendritic crystal - Google Patents
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- CN109336178B CN109336178B CN201811487975.6A CN201811487975A CN109336178B CN 109336178 B CN109336178 B CN 109336178B CN 201811487975 A CN201811487975 A CN 201811487975A CN 109336178 B CN109336178 B CN 109336178B
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Abstract
The invention relates to a preparation method of cadmium molybdate dendritic crystals, which comprises the steps of preparing a sodium benzoate aqueous solution and a cadmium chloride aqueous solution respectively, mixing the sodium benzoate aqueous solution and the cadmium chloride aqueous solution to obtain a cadmium benzoate precipitation solution, preparing a sodium molybdate aqueous solution and a polyvinyl alcohol aqueous solution, mixing the sodium molybdate aqueous solution and the polyvinyl alcohol aqueous solution, mixing the cadmium benzoate precipitation solution with the mixed solution of sodium molybdate and polyvinyl alcohol, evaporating water from the obtained mixture, performing microwave treatment, washing, filtering and drying to obtain the cadmium molybdate dendritic crystals. The method has simple process and controllable appearance, and is easy to realize industrial production. The prepared cadmium molybdate dendritic crystal has an ordered tree structure and a large specific surface area, and has a good application prospect in the fields of laser materials, magnetic materials, photoluminescence, photocatalytic materials, optical fibers, scintillator detectors, sensors and the like.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic materials, and particularly relates to a preparation method of cadmium molybdate dendrite.
Background
The molybdate has excellent optical, electrical, magnetic and other properties, so that the molybdate has a wide application prospect in the aspects of catalytic materials, laser donor materials, luminescent materials, magnetic materials, antibacterial materials and the like. Cadmium molybdate is a very important functional material in molybdate, and has very wide application in a plurality of fields such as laser and photoelectricity, photocatalysis, luminescence and display, detection technology and the like. As is well known, the performance of the nano material depends on factors such as the morphology and the size of the nano crystal, and the like, so that the preparation of the cadmium molybdate nano crystal with a special morphology has very important significance in the aspects of theoretical basic research and practical application.
The increasing miniaturization and complication of nanometer devices have made higher demands on the diversification of the shapes of nanometer materials, and the performances of the nanometer materials depend on the shapes and the sizes of the nanometer materials to a great extent, so that the preparation of nanometer particles with controllable shapes and the research and development of new shapes is still the research hotspot and the focus of scientific workers nowadays. The dendrite presents peculiar performance due to very large specific surface area, and the ordered tree structure of the dendrite creates very favorable conditions for the preparation and the application of the nanometer device. At present, no report on the preparation of cadmium molybdate dendrite exists.
Disclosure of Invention
The invention aims to provide a preparation method of cadmium molybdate dendrite, which has simple process, controllable morphology and easy realization of industrialization. The cadmium molybdate dendrite prepared by the invention has an ordered tree structure and a larger specific surface area, so the cadmium molybdate dendrite has a very good application prospect in the fields of laser materials, magnetic materials, photoluminescence materials, photocatalytic materials, optical fibers, scintillator detectors, sensors and the like.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The preparation method of the cadmium molybdate dendrite provided by the invention comprises the following steps:
1) dissolving sodium benzoate in deionized water to form a sodium benzoate aqueous solution, and adjusting the concentration of sodium benzoate in the solution to be 0.3-1.5 mol/L;
2) dissolving cadmium chloride in deionized water to form a cadmium chloride aqueous solution, and adjusting the concentration of the cadmium chloride in the solution to be 0.2-1.0 mol/L;
3) mixing the sodium benzoate aqueous solution prepared in the step 1) with the cadmium chloride aqueous solution prepared in the step 2) to obtain a cadmium benzoate precipitate solution, wherein the molar ratio of the sodium benzoate to the cadmium chloride is 1.5: 1;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 0.3-1.5 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the mass fraction of the polyvinyl alcohol in the solution to be 2%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 30-60 minutes;
7) mixing the cadmium benzoate precipitation solution prepared in the step 3) with the mixed solution of sodium molybdate and polyvinyl alcohol prepared in the step 6), wherein the molar ratio of sodium molybdate to cadmium benzoate is 1.5:1, evaporating water from the obtained mixture at 70-100 ℃ to obtain a precursor, placing the obtained precursor in a corundum crucible, covering a crucible cover, moving the corundum crucible into a microwave oven, reacting for 20-60 minutes under the action of microwaves, repeatedly washing the reaction product with distilled water, filtering, and drying to obtain the cadmium molybdate dendritic crystal.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
In the preparation method of the cadmium molybdate dendrite, the volume ratio of the sodium molybdate aqueous solution to the polyvinyl alcohol aqueous solution is 1:1 during the mixing in the step (6).
The preparation method of the cadmium molybdate dendrite comprises the step (7) of controlling the power of the microwave oven to be 800W-2000W.
In the preparation method of the cadmium molybdate dendrite, the purity of the sodium molybdate, the sodium benzoate, the cadmium chloride and the polyvinyl alcohol is not lower than the chemical purity.
The preparation method of the cadmium molybdate dendrite comprises the step of preparing the cadmium molybdate dendrite, wherein the diameter of the obtained cadmium molybdate dendrite is 50-200 nm, and the length of the obtained cadmium molybdate dendrite is 3-5 um.
In the preparation method of the cadmium molybdate dendrite, the obtained cadmium molybdate dendrite can be used for preparing laser materials, magnetic materials, photoluminescent materials, photocatalytic materials, optical fiber materials, scintillator detector materials, sensor materials and the like.
The key points of the technology of the invention are as follows:
(1) the cadmium benzoate precipitate solution is prepared by mixing the aqueous solution of sodium benzoate and the aqueous solution of cadmium chloride, and is used as a reaction precursor, otherwise, the cadmium molybdate dendrite cannot be obtained.
(2) The sodium molybdate aqueous solution and the polyvinyl alcohol aqueous solution are mixed to prepare a mixed solution of sodium molybdate and polyvinyl alcohol, otherwise, the cadmium molybdate dendrite cannot be obtained.
(3) The precipitate obtained must be subjected to microwave treatment, otherwise cadmium molybdate dendrites are not obtained.
(4) The above three points must be simultaneously possessed, otherwise, cadmium molybdate dendrites cannot be obtained.
The invention has the beneficial effects that:
the cadmium molybdate dendrite prepared by the method has good crystallinity and high purity, has an ordered dendritic structure, and has the purity of over 99 percent, and the diameter of the prepared cadmium molybdate dendrite is about 50-200 nm, and the length of the prepared cadmium molybdate dendrite is about 3-5 um. The preparation method of the cadmium molybdate dendrite provided by the invention has the advantages of controllable morphology, simple operation, low cost and the like, and is easy for industrial production. The prepared cadmium molybdate dendritic crystal has an ordered tree structure and a large specific surface area (the specific surface area can reach 89 m)2And/g), thereby having very good application prospect in the fields of laser materials, magnetic materials, photoluminescence, photocatalytic materials, optical fibers, scintillator detectors, sensors and the like.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following preferred embodiments are described in detail with reference to the accompanying drawings.
Drawings
FIG. 1 is an XRD pattern of a cadmium molybdate dendrite synthesized in example 1 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) photograph of the cadmium molybdate dendrite synthesized in example 1 of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the method for preparing cadmium molybdate dendrite according to the present invention, the specific implementation manner, structure, characteristics and effects thereof will be made with reference to the accompanying drawings and preferred embodiments.
Example 1
1) Dissolving sodium benzoate in deionized water to form a sodium benzoate aqueous solution, and adjusting the concentration of sodium benzoate in the solution to be 0.3 mol/L;
2) dissolving cadmium chloride in deionized water to form a cadmium chloride aqueous solution, and adjusting the concentration of the cadmium chloride in the solution to be 0.2 mol/L;
3) mixing the sodium benzoate aqueous solution prepared in the step 1) with the cadmium chloride aqueous solution prepared in the step 2) to obtain a cadmium benzoate precipitate solution (a mixture of cadmium benzoate precipitate and sodium chloride solution), wherein the molar ratio of sodium benzoate to cadmium chloride is 1.5: 1;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 0.3 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol in the solution to be 2%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 30 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1;
7) mixing the cadmium benzoate precipitation solution prepared in the step 3) with the mixed solution of sodium molybdate and polyvinyl alcohol prepared in the step 6), wherein the molar ratio of sodium molybdate to cadmium benzoate is 1.5:1, then placing the precipitation solution in a container such as a beaker, evaporating water at 70 ℃, placing the obtained precursor in a corundum crucible, covering the corundum crucible with a crucible cover, then moving the corundum crucible into a microwave oven with the power of 800W, and reacting for 60 minutes under the action of microwaves. And then repeatedly washing the reaction product by using distilled water, filtering and drying to obtain the cadmium molybdate dendrite.
The diameter of the obtained cadmium molybdate dendrite is about 100-200 nm, the length is about 3-4 um, and the XRD pattern is shown in figure 1; FIG. 2 shows a transmission electron micrograph.
Example 2
1) Dissolving sodium benzoate in deionized water to form a sodium benzoate aqueous solution, and adjusting the concentration of sodium benzoate in the solution to be 0.9 mol/L;
2) dissolving cadmium chloride in deionized water to form a cadmium chloride aqueous solution, and adjusting the concentration of the cadmium chloride in the solution to be 0.6 mol/L;
3) mixing the sodium benzoate aqueous solution prepared in the step 1) with the cadmium chloride aqueous solution prepared in the step 2) to obtain cadmium benzoate precipitate and a sodium chloride solution, wherein the molar ratio of the sodium benzoate to the cadmium chloride is 1.5: 1;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 0.9 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol in the solution to be 2%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 45 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1;
7) mixing the cadmium benzoate precipitation solution prepared in the step 3) with the mixed solution of sodium molybdate and polyvinyl alcohol prepared in the step 6), wherein the molar ratio of sodium molybdate to cadmium benzoate is 1.5:1, then placing the precipitation solution in a container such as a beaker, evaporating water at 80 ℃, placing the obtained precursor in a corundum crucible, covering the corundum crucible with a crucible cover, then moving the corundum crucible into a microwave oven with the power of 1500W, and reacting for 40 minutes under the action of microwaves. And then repeatedly washing the reaction product by using distilled water, filtering and drying to obtain the cadmium molybdate dendrite.
The diameter of the obtained cadmium molybdate dendrite is about 50-150 nm, and the length is about 3-4 um.
Example 3
1) Dissolving sodium benzoate in deionized water to form a sodium benzoate aqueous solution, and adjusting the concentration of sodium benzoate in the solution to be 1.5 mol/L;
2) dissolving cadmium chloride in deionized water to form a cadmium chloride aqueous solution, and adjusting the concentration of the cadmium chloride in the solution to be 1.0 mol/L;
3) mixing the sodium benzoate aqueous solution prepared in the step 1) with the cadmium chloride aqueous solution prepared in the step 2) to obtain cadmium benzoate precipitate and a sodium chloride solution, wherein the molar ratio of the sodium benzoate to the cadmium chloride is 1.5: 1;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 1.5 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol in the solution to be 2%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 60 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1;
7) mixing the cadmium benzoate precipitation solution prepared in the step 3) with the mixed solution of sodium molybdate and polyvinyl alcohol prepared in the step 6), wherein the molar ratio of sodium molybdate to cadmium benzoate is 1.5:1, then placing the precipitation solution in a container such as a beaker, evaporating water at 90 ℃, placing the obtained precursor in a corundum crucible, covering the corundum crucible with a crucible cover, then moving the corundum crucible into a microwave oven with the power of 2000W, and reacting for 20 minutes under the action of microwaves. And then repeatedly washing the reaction product by using distilled water, filtering and drying to obtain the cadmium molybdate dendrite.
The diameter of the obtained cadmium molybdate dendrite is about 100-200 nm, and the length is about 4-5 um.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The preparation method of the cadmium molybdate dendrite is characterized by comprising the following steps of:
1) dissolving sodium benzoate in deionized water to form a sodium benzoate aqueous solution, and adjusting the concentration of sodium benzoate in the solution to be 0.3-1.5 mol/L;
2) dissolving cadmium chloride in deionized water to form a cadmium chloride aqueous solution, and adjusting the concentration of the cadmium chloride in the solution to be 0.2-1.0 mol/L;
3) mixing the sodium benzoate aqueous solution prepared in the step 1) with the cadmium chloride aqueous solution prepared in the step 2) to obtain a cadmium benzoate precipitate solution, wherein the molar ratio of the sodium benzoate to the cadmium chloride is 1.5: 1;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 0.3-1.5 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the mass fraction of the polyvinyl alcohol in the solution to be 2%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) and the polyvinyl alcohol aqueous solution prepared in the step 5) according to the volume ratio of 1:1 to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 30-60 minutes;
7) mixing the cadmium benzoate precipitation solution prepared in the step 3) with the mixed solution of sodium molybdate and polyvinyl alcohol prepared in the step 6), wherein the molar ratio of sodium molybdate to cadmium benzoate is 1.5:1, evaporating water from the obtained mixture at 70-100 ℃ to obtain a precursor, placing the obtained precursor in a corundum crucible, covering a crucible cover, moving the corundum crucible into a microwave oven, reacting for 20-60 minutes under the action of microwaves, repeatedly washing the reaction product with distilled water, filtering, and drying to obtain the cadmium molybdate dendritic crystal.
2. The method of claim 1, wherein the microwave oven of step (7) has a power of 800W to 2000W.
3. The method for preparing cadmium molybdate dendrites of claim 1, wherein the purity of sodium molybdate, sodium benzoate, cadmium chloride and polyvinyl alcohol is not lower than chemical purity.
4. The method for preparing cadmium molybdate dendrites of claim 1, wherein the diameter of the obtained cadmium molybdate dendrites is 50-200 nm, and the length is 3-5 um.
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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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| CN106430311A (en) * | 2016-09-12 | 2017-02-22 | 洛阳理工学院 | Preparation method of strontium tungstate dendrite |
| CN106915773B (en) * | 2017-05-04 | 2018-03-06 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
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- 2018-12-06 CN CN201811487975.6A patent/CN109336178B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| PL213464B1 (en) * | 2009-09-25 | 2013-03-29 | Univ West Pomeranian Szczecin Tech | Process for the preparation of oxosalts in a two-component system of cadmium molybdate (VI) and metal tungstates (VI) |
| CN103833080A (en) * | 2014-03-25 | 2014-06-04 | 洛阳理工学院 | Preparation method for cadmium molybdate porous spheres |
| CN104671285A (en) * | 2015-01-28 | 2015-06-03 | 洛阳理工学院 | Method for preparing cadmium molybdate nanorod |
| CN104860353A (en) * | 2015-04-16 | 2015-08-26 | 东华理工大学 | Preparation method of cadmium molybdate hollow spheres assembled with nano-particles |
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| CN106915773B (en) * | 2017-05-04 | 2018-03-06 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
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