CN109336178A - A kind of preparation method of molybdic acid cadmium skeleton - Google Patents
A kind of preparation method of molybdic acid cadmium skeleton Download PDFInfo
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- CN109336178A CN109336178A CN201811487975.6A CN201811487975A CN109336178A CN 109336178 A CN109336178 A CN 109336178A CN 201811487975 A CN201811487975 A CN 201811487975A CN 109336178 A CN109336178 A CN 109336178A
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- solution
- acid cadmium
- polyvinyl alcohol
- skeleton
- molybdic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/30—Particle morphology extending in three dimensions
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of preparation methods of molybdic acid cadmium skeleton, aqueous sodium benzoate solution and caddy aqueous solution are first prepared respectively and are mixed to obtain benzoic acid cadmium precipitation solution, then sodium molybdate aqueous solution and polyvinyl alcohol water solution are prepared and is mixed, benzoic acid cadmium precipitation solution and the mixed solution of sodium molybdate and polyvinyl alcohol are mixed, then obtained mixture is first evaporated into moisture, microwave treatment is carried out again obtains molybdic acid cadmium skeleton after washed, filtering, drying.Method and process of the invention is simple, morphology controllable, is easily industrialized production.Prepared molybdic acid cadmium skeleton, has orderly tree, and biggish specific surface area has extraordinary application prospect in fields such as laser material, magnetic material, luminescence generated by light, catalysis material, optical fiber, scintillator detector, sensors.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, and in particular to a kind of preparation side of molybdic acid cadmium skeleton
Method.
Background technique
Molybdate is because having the properties such as excellent optics, electricity, magnetics in catalysis material, laser donor material, hair
Luminescent material, magnetic material, anti-biotic material etc. have biggish application prospect.Molybdic acid cadmium is the function of extremely important one kind in molybdate
Energy material, in laser and photoelectricity, photocatalysis, shining all has very extensive purposes with various fields such as display, Detection Techniques.
It is well known that the performance of nano material depends on the factors such as the morphology and size of nanocrystal, thus prepare with special form
The cadmium molybdate nano crystal of looks, all has very important significance in terms of theoretical basis research and practical application.
Being miniaturized and complicating increasingly for nano-device proposes higher want to the diversification of appearance of nano material
It asks, the performance of nano material is largely dependent upon their morphology and size, therefore prepares morphology controllable, the new pattern of research and development
Nanoparticle be still scientific worker now research hotspot and emphasis.Skeleton is due to comparing table with very big
Area and show peculiar performance, while the orderly tree of skeleton is also the preparation and application wound of nano-device
Highly beneficial condition is made.It there is no the report in terms of the preparation of molybdic acid cadmium skeleton at present.
Summary of the invention
The object of the present invention is to provide a kind of simple process, morphology controllable, the molybdic acid cadmium dendroids being easily industrialized
The preparation method of crystal.Molybdic acid cadmium skeleton prepared by the present invention has larger because having orderly tree
Specific surface area, thus in laser material, magnetic material, luminescence generated by light, catalysis material, optical fiber, scintillator detector, sensing
The fields such as device have extraordinary application prospect.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.
A kind of preparation method of molybdic acid cadmium skeleton proposed according to the present invention comprising following steps:
1) sodium benzoate is dissolved in deionized water, forms aqueous sodium benzoate solution, adjust the concentration of sodium benzoate in solution
For 0.3~1.5mol/L；
2) caddy being dissolved in deionized water, forms caddy aqueous solution, the concentration for adjusting Chlorine in Solution cadmium is 0.2~
1.0mol/L；
3) caddy aqueous solution made from aqueous sodium benzoate solution made from step 1) and step 2) is mixed, obtains benzene
Formic acid cadmium precipitation solution, wherein the molar ratio of sodium benzoate and caddy is 1.5:1；
4) sodium molybdate being dissolved in deionized water, forms sodium molybdate aqueous solution, the concentration for adjusting Molybdenum in Solution acid sodium is 0.3~
1.5mol/L；
5) polyvinyl alcohol is dissolved in deionized water, forms polyvinyl alcohol water solution, adjust the quality of polyvinyl alcohol in solution
Score is 2%；
6) polyvinyl alcohol water solution made from sodium molybdate aqueous solution made from step 4) and step 5) is mixed, obtains molybdenum
The mixed solution of sour sodium and polyvinyl alcohol stirs 30~60 minutes；
7) by the mixing of sodium molybdate and polyvinyl alcohol made from benzoic acid cadmium precipitation solution made from step 3) and step 6)
Solution mixes, and the molar ratio of sodium molybdate and benzoic acid cadmium is 1.5:1 when mixing, then by obtained mixture 70~100
DEG C moisture is evaporated, obtain presoma, obtained presoma is placed in corundum crucible, cover crucible lid, then by corundum earthenware
Crucible moves in micro-wave oven, reacts 20~60 minutes under the action of microwave, then with distilled water washing reaction product repeatedly, mistake
After filter, drying, molybdic acid cadmium skeleton is obtained.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
A kind of preparation method of molybdic acid cadmium skeleton above-mentioned, wherein step (6) mix when sodium molybdate aqueous solution and
The volume ratio of polyvinyl alcohol water solution is 1:1.
A kind of preparation method of molybdic acid cadmium skeleton above-mentioned, wherein the power of step (7) micro-wave oven be 800W~
2000W。
The preparation method of a kind of molybdic acid cadmium skeleton above-mentioned, wherein the sodium molybdate, sodium benzoate, chlorination
Cadmium, polyvinyl alcohol purity be not less than chemistry it is pure.
A kind of preparation method of molybdic acid cadmium skeleton above-mentioned, wherein the diameter of gained molybdic acid cadmium skeleton
For 50~200nm, length is 3~5um.
The preparation method of a kind of molybdic acid cadmium skeleton above-mentioned, wherein gained molybdic acid cadmium skeleton can be used for
Prepare laser material, magnetic material, embedded photoluminescent material, catalysis material, fiber optic materials, scintillator detector material, sensing
Equipment material etc..
Key problem in technology point of the invention is:
(1) first aqueous sodium benzoate solution and caddy aqueous solution must be mixed, benzoic acid cadmium precipitation solution is made and makees
To react precursor, it otherwise cannot get molybdic acid cadmium skeleton.
(2) it has to mix sodium molybdate aqueous solution and polyvinyl alcohol water solution, prepares sodium molybdate and polyvinyl alcohol
Mixed solution, otherwise cannot get molybdic acid cadmium skeleton.
(3) it has to obtained precipitating carrying out microwave treatment, otherwise cannot get molybdic acid cadmium skeleton.
(4) it must be provided simultaneously with for 3 points more than, otherwise cannot get molybdic acid cadmium skeleton.
The beneficial effects of the present invention are:
The present invention has prepared good crystallinity, purity is high, the molybdic acid cadmium skeleton with orderly tree,
Purity is up to 99% or more, and the diameter of obtained molybdic acid cadmium skeleton is about 50~200nm, and length is about 3~5um.
The preparation method of molybdic acid cadmium skeleton provided by the invention has many advantages, such as morphology controllable, easy to operate, low in cost,
It is easy to industrialized production.Prepared molybdic acid cadmium skeleton compares table with biggish because having orderly tree
(specific surface area is up to 89m for area2/ g), thus in laser material, magnetic material, luminescence generated by light, catalysis material, optical fiber, sudden strain of a muscle
The fields such as bright detector, sensor have extraordinary application prospect.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can
It is clearer and more comprehensible, it is special below to lift preferred embodiment, and cooperate attached drawing, detailed description are as follows.
Detailed description of the invention
Fig. 1 is the XRD spectrum for the molybdic acid cadmium skeleton that the embodiment of the present invention 1 synthesizes；
Fig. 2 is transmission electron microscope (TEM) photo for the molybdic acid cadmium skeleton that the embodiment of the present invention 1 synthesizes.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to a kind of preparation method of molybdic acid cadmium skeleton proposed according to the present invention, specific implementation
Mode, structure, feature and its effect, detailed description is as follows.
Embodiment 1
1) sodium benzoate is dissolved in deionized water, forms aqueous sodium benzoate solution, adjust the dense of the sodium benzoate in solution
Degree is 0.3mol/L；
2) caddy is dissolved in deionized water, forms caddy aqueous solution, the concentration for adjusting Chlorine in Solution cadmium is
0.2mol/L；
3) caddy aqueous solution made from aqueous sodium benzoate solution made from step 1) and step 2) is mixed, obtains benzene
Formic acid cadmium precipitation solution (mixture for referring to benzoic acid cadmium precipitating and sodium chloride solution), wherein sodium benzoate and caddy rub
You are than being 1.5:1；
4) sodium molybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the concentration for adjusting Molybdenum in Solution acid sodium is
0.3mol/L；
5) polyvinyl alcohol is dissolved in deionized water, forms polyvinyl alcohol water solution, adjust the concentration of polyvinyl alcohol in solution
It is 2%；
6) polyvinyl alcohol water solution made from sodium molybdate aqueous solution made from step 4) and step 5) is mixed, obtains molybdenum
The mixed solution of sour sodium and polyvinyl alcohol stirs 30 minutes, and wherein the volume ratio of sodium molybdate solution and poly-vinyl alcohol solution is 1:
1；
7) by the mixing of sodium molybdate and polyvinyl alcohol made from benzoic acid cadmium precipitation solution made from step 3) and step 6)
Solution mixes, and the molar ratio of sodium molybdate and benzoic acid cadmium is 1.5:1 when mixing, this precipitation solution is then placed in beaker etc. and is held
Moisture is evaporated at 70 DEG C in device, obtained presoma is placed in corundum crucible, covers crucible lid, then corundum crucible is moved
To micro-wave oven, the power of micro-wave oven is 800W, is reacted 60 minutes under the action of microwave.Then it is washed repeatedly with distilled water anti-
Product is answered to obtain molybdic acid cadmium skeleton after filtering, drying.
The diameter of gained molybdic acid cadmium skeleton is about 100~200nm, and length is about 3~4um, and XRD spectrum is shown in figure
1；Transmission electron microscope picture is shown in Fig. 2.
Embodiment 2
1) sodium benzoate is dissolved in deionized water, forms aqueous sodium benzoate solution, adjust the dense of the sodium benzoate in solution
Degree is 0.9mol/L；
2) caddy is dissolved in deionized water, forms caddy aqueous solution, the concentration for adjusting Chlorine in Solution cadmium is
0.6mol/L；
3) caddy aqueous solution made from aqueous sodium benzoate solution made from step 1) and step 2) is mixed, obtains benzene
Formic acid cadmium precipitating and sodium chloride solution, wherein the molar ratio of sodium benzoate and caddy is 1.5:1；
4) sodium molybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the concentration for adjusting Molybdenum in Solution acid sodium is
0.9mol/L；
5) polyvinyl alcohol is dissolved in deionized water, forms polyvinyl alcohol water solution, adjust the concentration of polyvinyl alcohol in solution
It is 2%；
6) polyvinyl alcohol water solution made from sodium molybdate aqueous solution made from step 4) and step 5) is mixed, obtains molybdenum
The mixed solution of sour sodium and polyvinyl alcohol stirs 45 minutes, and wherein the volume ratio of sodium molybdate solution and poly-vinyl alcohol solution is 1:
1；
7) by the mixing of sodium molybdate and polyvinyl alcohol made from benzoic acid cadmium precipitation solution made from step 3) and step 6)
Solution mixes, and the molar ratio of sodium molybdate and benzoic acid cadmium is 1.5:1 when mixing, this precipitation solution is then placed in beaker etc. and is held
Moisture is evaporated at 80 DEG C in device, obtained presoma is placed in corundum crucible, covers crucible lid, then corundum crucible is moved
To micro-wave oven, the power of micro-wave oven is 1500W, is reacted 40 minutes under the action of microwave.Then it is washed repeatedly with distilled water
Reaction product obtains molybdic acid cadmium skeleton after filtering, drying.
The diameter of gained molybdic acid cadmium skeleton is about 50~150nm, and length is about 3~4um.
Embodiment 3
1) sodium benzoate is dissolved in deionized water, forms aqueous sodium benzoate solution, adjust the dense of the sodium benzoate in solution
Degree is 1.5mol/L；
2) caddy is dissolved in deionized water, forms caddy aqueous solution, the concentration for adjusting Chlorine in Solution cadmium is
1.0mol/L；
3) caddy aqueous solution made from aqueous sodium benzoate solution made from step 1) and step 2) is mixed, obtains benzene
Formic acid cadmium precipitating and sodium chloride solution, wherein the molar ratio of sodium benzoate and caddy is 1.5:1；
4) sodium molybdate is dissolved in deionized water, forms sodium molybdate aqueous solution, the concentration for adjusting Molybdenum in Solution acid sodium is
1.5mol/L；
5) polyvinyl alcohol is dissolved in deionized water, forms polyvinyl alcohol water solution, adjust the concentration of polyvinyl alcohol in solution
It is 2%；
6) sodium molybdate aqueous solution made from step 4) and polyvinyl alcohol water solution made from step 5) are mixed, obtains molybdenum
The mixed solution of sour sodium and polyvinyl alcohol stirs 60 minutes, and wherein the volume ratio of sodium molybdate solution and poly-vinyl alcohol solution is 1:
1；
7) by the mixing of sodium molybdate and polyvinyl alcohol made from benzoic acid cadmium precipitation solution made from step 3) and step 6)
Solution mixes, and the molar ratio of sodium molybdate and benzoic acid cadmium is 1.5:1 when mixing, this precipitation solution is then placed in beaker etc. and is held
Moisture is evaporated at 90 DEG C in device, obtained presoma is placed in corundum crucible, covers crucible lid, then corundum crucible is moved
To micro-wave oven, the power of micro-wave oven is 2000W, is reacted 20 minutes under the action of microwave.Then it is washed repeatedly with distilled water
Reaction product obtains molybdic acid cadmium skeleton after filtering, drying.
The diameter of gained molybdic acid cadmium skeleton is about 100~200nm, and length is about 4~5um.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (5)
1. a kind of preparation method of molybdic acid cadmium skeleton, it is characterised in that the following steps are included:
1) sodium benzoate is dissolved in deionized water, forms aqueous sodium benzoate solution, the concentration for adjusting sodium benzoate in solution is 0.3
~1.5mol/L；
2) caddy being dissolved in deionized water, forms caddy aqueous solution, the concentration for adjusting Chlorine in Solution cadmium is 0.2~
1.0mol/L；
3) caddy aqueous solution made from aqueous sodium benzoate solution made from step 1) and step 2) is mixed, obtains benzoic acid
Cadmium precipitation solution, wherein the molar ratio of sodium benzoate and caddy is 1.5:1；
4) sodium molybdate being dissolved in deionized water, forms sodium molybdate aqueous solution, the concentration for adjusting Molybdenum in Solution acid sodium is 0.3~
1.5mol/L；
5) polyvinyl alcohol is dissolved in deionized water, forms polyvinyl alcohol water solution, adjust the mass fraction of polyvinyl alcohol in solution
It is 2%；
6) polyvinyl alcohol water solution made from sodium molybdate aqueous solution made from step 4) and step 5) is mixed, obtains sodium molybdate
With the mixed solution of polyvinyl alcohol, stir 30~60 minutes；
7) by the mixed solution of sodium molybdate and polyvinyl alcohol made from benzoic acid cadmium precipitation solution made from step 3) and step 6)
It mixes, the molar ratio of sodium molybdate and benzoic acid cadmium is 1.5:1 when mixing, then steams obtained mixture at 70~100 DEG C
Hair falls moisture, obtains presoma, obtained presoma is placed in corundum crucible, cover crucible lid, then corundum crucible is moved
To micro-wave oven, reacted under the action of microwave 20~60 minutes, then with distilled water, washing reaction product, filtering are dried repeatedly
After dry, molybdic acid cadmium skeleton is obtained.
2. the preparation method of molybdic acid cadmium skeleton according to claim 1, it is characterised in that molybdenum when step (6) mixes
The volume ratio of acid sodium aqueous solution and polyvinyl alcohol water solution is 1:1.
3. the preparation method of molybdic acid cadmium skeleton according to claim 1, it is characterised in that step (7) micro-wave oven
Power is 800W~2000W.
4. the preparation method of molybdic acid cadmium skeleton according to claim 1, it is characterised in that the sodium molybdate, benzene
Sodium formate, caddy, polyvinyl alcohol purity be not less than chemistry it is pure.
5. the preparation method of molybdic acid cadmium skeleton according to claim 1, it is characterised in that gained molybdic acid cadmium branch
The diameter of shape crystal is 50~200nm, and length is 3~5um.
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Citations (7)
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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 |
| 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 |
-
2018
- 2018-12-06 CN CN201811487975.6A patent/CN109336178B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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