CN103833080A - Preparation method for cadmium molybdate porous spheres - Google Patents
Preparation method for cadmium molybdate porous spheres Download PDFInfo
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- CN103833080A CN103833080A CN201410111987.4A CN201410111987A CN103833080A CN 103833080 A CN103833080 A CN 103833080A CN 201410111987 A CN201410111987 A CN 201410111987A CN 103833080 A CN103833080 A CN 103833080A
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Abstract
The invention discloses a preparation method for cadmium molybdate porous spheres. The preparation method comprises the following steps of mixing a cadmium chloride solution and a sodium acetate solution to prepare a cadmium acetate precipitate solution, mixing the cadmium acetate precipitate solution and a sodium molybdate solution, loading the mixed solution in a reaction kettle, preserving heat for 2 to 12 hours at 110 to 200 DEG C, performing hydrothermal treatment, repeatedly washing a reaction product by using distilled water after the reaction product is unloaded from the reaction kettle, and filtering and drying the reaction product to obtain the cadmium molybdate porous spheres. The preparation method has the advantages of simple process, no organic surfactants, no pollution, easiness in industrial production, high crystallinity, high purity, capability of effectively controlling the morphology of cadmium molybdate crystals, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of molybdic acid cadmium, relate in particular to a kind of preparation method of molybdic acid cadmium porous ball.
Background technology
Molybdic acid cadmium (CdMoO
4) there is scheelite-type structure, in this structure, molybdenum atom is in tetrahedron center, the luminescent properties of molybdic acid cadmium is mainly due to the transfer of electronics in molybdate and transition, therefore it all has broad application prospects in photoluminescence, photocatalyst material, optical fiber, scintillator detector, laserable material, magneticsubstance, a lot of fields of sensor, thereby becomes one of inorganic materials of primary study in recent years.
As everyone knows, the photoluminescence property of solid is relevant with the size of solid particulate, pattern and microstructure, and the performance of nano material also depends on the factor such as pattern and size of its nanocrystal, thereby cause size, pattern and the microstructure of different reaction conditionss on nanometer molybdic acid cadmium to have important impact, thereby the nano material with special appearance all can show some excellent performances, therefore the cadmium molybdate nano crystal of, preparing pattern novelty is all having very important significance aspect theoretical basis research and practical application.
At present, the preparation method of molybdic acid cadmium is hydrothermal method and micro emulsion assisting alcohol-hydrothermal method.While utilizing micro emulsion assisting alcohol-hydrothermal method, owing to having added a large amount of organism, thereby follow-up processing is brought to trouble; The molybdic acid cadmium pattern that hydrothermal method and micro emulsion assisting alcohol-hydrothermal method are prepared is simultaneously also more regular, does not reach the effect of rationality in performance.
Summary of the invention
The object of the invention is the deficiency in order to solve the problems of the technologies described above existence, provide a kind of technique simply, do not use any organic surface active agent, pollution-free, be easy to suitability for industrialized production, advantages of good crystallization, purity high, and effectively control the preparation method of the molybdic acid cadmium porous ball of crystal morphology.
The preparation method of molybdic acid cadmium porous ball of the present invention, concrete steps are as follows:
Step 1, Cadmium chloride fine powder is dissolved in to deionized water, forms the Cadmium chloride fine powder aqueous solution, the Cd in regulator solution
2+the concentration of ion is 0.1 ~ 3.0mol/L;
Step 2, sodium acetate is dissolved in to deionized water, forms aqueous sodium acetate solution, the CH in regulator solution
3cOO
-the concentration of ion is 0.1 ~ 3.0mol/L;
Step 3, Sodium orthomolybdate is dissolved in to deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 0.1 ~ 3.0mol/L;
The sodium acetate solution that step 4, the cadmium chloride solution that step 1 is made make with step 2 mixes mutually, and blending ratio is 1:1, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution that step 3 is made make with step 4 mixes mutually, blending ratio is 1:1, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 70% ~ 90% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, sealing, at 110 ~ 200 DEG C, be incubated and within 2 ~ 12 hours, carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, after filtering, drying, obtain molybdic acid cadmium porous ball.
In preparation process of the present invention, must be using cadmium acetate precipitation as reaction precursor, otherwise can not get molybdic acid cadmium porous ball, this is because the unique porous ball of molybdic acid cadmium is to form in the process being at high temperature incubated, and reacts the rear formation of precursor reaction by molybdenum acid ion with cadmium acetate.Because process of growth and the chemical reaction process of crystal are closely related, at specific chemical reaction process, can impel crystal generation oriented growth, obtain having the crystal of special appearance and structure.The present invention adopts cadmium acetate as reaction precursor, can make the direction of growth of molybdic acid cadmium crystal change, and impels it to be grown to serve as molybdic acid cadmium porous ball, and cadmium acetate is to form the very crucial factor of molybdic acid cadmium porous ball.
In preparation process of the present invention, the purity of described Sodium orthomolybdate, Cadmium chloride fine powder, sodium acetate and dehydrated alcohol is all not less than chemical pure.
In step 5, regulate the reaction mass volume in reactor inner bag to reach 70% ~ 90% of reactor inner bag volume with distilled water, this is in order to make hydro-thermal reaction system in boiling state, utilize the carrying out of chemical reaction, make sodium molybdate solution and cadmium acetate solution reaction more abundant.
In step 6, washing and filtration are that the impurity such as sodium ion, chlorion, oven dry in order to remove in solution are in order to remove after distilled water, obtain the molybdic acid cadmium porous ball that purity is higher.
Beneficial effect of the present invention is:
The preparation method of this molybdic acid cadmium porous ball provided by the invention, has technological process and simply, does not use any organic surface active agent, pollution-free, good crystallinity, purity advantages of higher, can effectively control the pattern of cadmium molybdate nano crystal.The molybdic acid cadmium porous ball that the present invention prepares, because of its unique vesicular structure having, thereby aspect photoluminescence, photocatalyst material, optical fiber, scintillator detector, laserable material, magneticsubstance, sensor, have more more excellent performance, and there is application prospect more widely.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the synthetic molybdic acid cadmium porous ball of the present invention;
Fig. 2 is transmission electron microscope (TEM) photo of the synthetic molybdic acid cadmium porous ball of the present invention.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
Embodiment 1
Step 1, Cadmium chloride fine powder is dissolved in to deionized water, forms the Cadmium chloride fine powder aqueous solution, the Cd in regulator solution
2+the concentration of ion is 0.15mol/L;
Step 2, sodium acetate is dissolved in to deionized water, forms aqueous sodium acetate solution, the CH in regulator solution
3cOO
-the concentration of ion is 0.15mol/L;
Step 3, Sodium orthomolybdate is dissolved in to deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 0.15mol/L;
The sodium acetate solution that step 4, the cadmium chloride solution that step 1 is made make with step 2 mixes mutually, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution that step 3 is made make with step 4 mixes mutually, then joins in reactor inner bag, regulates the reaction mass volume in reactor inner bag to reach 70% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 110
ounder C, be incubated and within 10 hours, carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, after filtering, drying, obtain molybdic acid cadmium porous ball.The XRD figure spectrum obtaining is shown in Fig. 1; Transmission electron microscope picture is shown in Fig. 2.
Fig. 1 illustrates that molybdic acid cadmium of the present invention does not have dephasign, and purity is very high, and diffraction peak is very sharp-pointed, thereby explanation molybdic acid cadmium crystal structure is good; Fig. 2 illustrates spherical that molybdic acid cadmium crystal of the present invention is porous, and the diameter of molybdic acid cadmium porous ball is about 700-900nm.
Embodiment 2
Step 1, Cadmium chloride fine powder is dissolved in to deionized water, forms the Cadmium chloride fine powder aqueous solution, the Cd in regulator solution
2+the concentration of ion is 1.65mol/L;
Step 2, sodium acetate is dissolved in to deionized water, forms aqueous sodium acetate solution, the CH in regulator solution
3cOO
-the concentration of ion is 1.65mol/L;
Step 3, Sodium orthomolybdate is dissolved in to deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 1.65mol/L;
The sodium acetate solution that step 4, the cadmium chloride solution that step 1 is made make with step 2 mixes mutually, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution that step 3 is made make with step 4 mixes mutually, then joins in reactor inner bag, regulates the reaction mass volume in reactor inner bag to reach 80% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 160
ounder C, be incubated and within 6 hours, carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, after filtering, drying, obtain molybdic acid cadmium porous ball.
Embodiment 3
Step 1, Cadmium chloride fine powder is dissolved in to deionized water, forms the Cadmium chloride fine powder aqueous solution, the Cd in regulator solution
2+the concentration of ion is 3.0mol/L;
Step 2, sodium acetate is dissolved in to deionized water, forms aqueous sodium acetate solution, the CH in regulator solution
3cOO
-the concentration of ion is 3.0mol/L;
Step 3, Sodium orthomolybdate is dissolved in to deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 3.0mol/L;
The sodium acetate solution that step 4, the cadmium chloride solution that step 1 is made make with step 2 mixes mutually, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution that step 3 is made make with step 4 mixes mutually, then joins in reactor inner bag, regulates the reaction mass volume in reactor inner bag to reach 90% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 200
ounder C, be incubated and within 3 hours, carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, after filtering, drying, obtain molybdic acid cadmium porous ball.
Claims (4)
1. a preparation method for molybdic acid cadmium porous ball, is characterized in that: step 1, Cadmium chloride fine powder is dissolved in to deionized water, forms the Cadmium chloride fine powder aqueous solution, the Cd in regulator solution
2+the concentration of ion is 0.1 ~ 3.0mol/L; Step 2, sodium acetate is dissolved in to deionized water, forms aqueous sodium acetate solution, the CH in regulator solution
3cOO
-the concentration of ion is 0.1 ~ 3.0mol/L; Step 3, Sodium orthomolybdate is dissolved in to deionized water, forms sodium molybdate aqueous solution, the MoO in regulator solution
4 2-the concentration of ion is 0.1 ~ 3.0mol/L; The sodium acetate solution that step 4, the cadmium chloride solution that step 1 is made make with step 2 is mixed to get cadmium acetate precipitation mutually as reaction precursor; The cadmium acetate precipitation solution that step 5, the sodium molybdate solution that step 3 is made make with step 4 mixes mutually, then joins in reactor inner bag; Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 110 ~ 200
ounder C, be incubated and within 2 ~ 12 hours, carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, after filtering, drying, obtain molybdic acid cadmium porous ball.
2. the preparation method of a kind of molybdic acid cadmium porous ball according to claim 1, is characterized in that: the ratio that cadmium chloride solution mixes with sodium acetate solution is 1:1.
3. the preparation method of a kind of molybdic acid cadmium porous ball according to claim 1, is characterized in that: the ratio that sodium molybdate solution mixes with cadmium acetate precipitation solution is 1:1.
4. the preparation method of a kind of molybdic acid cadmium porous ball according to claim 1, it is characterized in that: the cadmium acetate precipitation solution that the sodium molybdate solution that step 3 is made makes with step 4 mixes mutually, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 70% ~ 90% of reactor inner bag volume with distilled water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109336178A (en) * | 2018-12-06 | 2019-02-15 | 洛阳理工学院 | A kind of preparation method of molybdic acid cadmium skeleton |
| CN111704169A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of manganese molybdate nanosheet crystal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923704A (en) * | 2006-09-14 | 2007-03-07 | 上海交通大学 | Preparation method of octahedronlike cadmium molybdate crystal |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923704A (en) * | 2006-09-14 | 2007-03-07 | 上海交通大学 | Preparation method of octahedronlike cadmium molybdate crystal |
Non-Patent Citations (2)
| Title |
|---|
| (苏)卡里亚金，(苏)安格洛夫著，任道华译: "《纯化学物质的制备》", 31 July 1986, article "乙酸镉", pages: 94 * |
| 张大凤，等。: "CdMoO4微球的微波辅助法快速合成及其光催化性能", 《材料导报》, vol. 25, no. 1, 31 May 2011 (2011-05-31) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104860353B (en) * | 2015-04-16 | 2016-07-20 | 东华理工大学 | A kind of preparation method of the molybdic acid cadmium hollow ball assembled by nano-particle |
| 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 |
| CN111704169A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of manganese molybdate nanosheet crystal |
| CN111704169B (en) * | 2020-07-01 | 2022-09-30 | 洛阳理工学院 | Preparation method of manganese molybdate nanosheet crystal |
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