CN103833080B - A kind of preparation method of molybdic acid cadmium porous ball - Google Patents
A kind of preparation method of molybdic acid cadmium porous ball Download PDFInfo
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- CN103833080B CN103833080B CN201410111987.4A CN201410111987A CN103833080B CN 103833080 B CN103833080 B CN 103833080B CN 201410111987 A CN201410111987 A CN 201410111987A CN 103833080 B CN103833080 B CN 103833080B
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- cadmium
- solution
- molybdic acid
- inner bag
- porous ball
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- VLAPMBHFAWRUQP-UHFFFAOYSA-L Molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 title claims abstract description 35
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- TVXXNOYZHKPKGW-UHFFFAOYSA-N Sodium molybdate Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 19
- LHQLJMJLROMYRN-UHFFFAOYSA-L Cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 18
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 17
- VMHLLURERBWHNL-UHFFFAOYSA-M sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 17
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 17
- 239000001632 sodium acetate Substances 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 13
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 13
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 6
- 230000003252 repetitive Effects 0.000 claims abstract description 6
- 238000005201 scrubbing Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 45
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 150000002500 ions Chemical class 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- OZAIFHULBGXAKX-UHFFFAOYSA-N precursor Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 8
- 229910015621 MoO Inorganic materials 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 8
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000005712 crystallization Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011068 load Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000004530 micro-emulsion Substances 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 238000005424 photoluminescence Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- KWPZWLVBWFDGMY-UHFFFAOYSA-N cadmium(2+);dioxido(dioxo)molybdenum Chemical compound [Cd+2].[O-][Mo]([O-])(=O)=O KWPZWLVBWFDGMY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 229960000935 Dehydrated Alcohol Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention discloses a kind of preparation method of molybdic acid cadmium porous ball.Cadmium chloride solution and sodium acetate solution are mixed obtained cadmium acetate precipitation solution by the present invention mutually, again this cadmium acetate precipitation solution is mixed mutually with sodium molybdate solution, load in reactor, at 110 ~ 200 DEG C, be incubated and carry out hydrothermal treatment consists in 2 ~ 12 hours, after unloading still, by distilled water repetitive scrubbing reaction product, after filtration, oven dry, obtain molybdic acid cadmium porous ball.The present invention have technique simply, do not use any organic surface active agent, pollution-free, be easy to suitability for industrialized production, advantages of good crystallization, purity are high and effectively control the advantages such as molybdic acid cadmium crystal morphology.
Description
Technical field
The present invention relates to a kind of preparation method of molybdic acid cadmium, particularly relate 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 transfer and the transition of electronics in molybdate, therefore it all has broad application prospects in photoluminescence, photocatalyst material, optical fiber, scintillator detector, laserable material, magneticsubstance, a lot of field of sensor, thus 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, thus cause different reaction conditionss to have important impact to the size of nanometer molybdic acid cadmium, pattern and microstructure, the nano material thus with special appearance all can show the performance of some excellences, therefore, the cadmium molybdate nano crystal preparing novel in shape all has very important significance in 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.When utilizing micro emulsion assisting alcohol-hydrothermal method, owing to adding a large amount of organism, thus trouble is brought to follow-up process; Simultaneously the molybdic acid cadmium pattern prepared of hydrothermal method and micro emulsion assisting alcohol-hydrothermal method is also more regular, and performance does not reach the effect of rationality.
Summary of the invention
The object of the invention is the deficiency in order to solve the problems of the technologies described above existence, providing that a kind of technique simply, does not use any organic surface active agent, pollution-free, to 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 one, Cadmium chloride fine powder is dissolved in 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 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 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, cadmium chloride solution step one obtained and step 2 obtain 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 and the step 4 that step 3 are obtained obtain 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, reactor inner bag step 5 being equipped with reaction mass are placed in reactor, sealing, at 110 ~ 200 DEG C, be incubated and carry out hydrothermal treatment consists in 2 ~ 12 hours, then reactor is allowed to naturally cool to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, after filtration, oven dry, obtain molybdic acid cadmium porous ball.
In preparation process of the present invention, must 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 formed in the process be at high temperature incubated, reacted after precursor is reacted by molybdenum acid ion and cadmium acetate and formed.Due to the process of growth of crystal and chemical reaction process closely related, at specific chemical reaction process, crystal generation oriented growth can be impelled, obtain the crystal with special appearance and structure.The present invention adopts cadmium acetate as reaction precursor, the direction of growth of molybdic acid cadmium crystal can be made to change, impel it to be grown to serve as molybdic acid cadmium porous ball, and cadmium acetate forms 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 to make hydro-thermal reaction system be in boiling state, utilize the carrying out of chemical reaction, make sodium molybdate solution and cadmium acetate solution react more abundant.
Washing and to filter be in order to after removing distilled water to remove the impurity such as sodium ion, chlorion in solution, drying in step 6, obtains 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, effectively can control the pattern of cadmium molybdate nano crystal.The molybdic acid cadmium porous ball that the present invention prepares, because of unique vesicular structure that it has, thus in photoluminescence, photocatalyst material, optical fiber, scintillator detector, laserable material, magneticsubstance, sensor, have more more excellent performance, and have application prospect more widely.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the molybdic acid cadmium porous ball that the present invention synthesizes;
Fig. 2 is transmission electron microscope (TEM) photo of the molybdic acid cadmium porous ball that the present invention synthesizes.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
Step one, Cadmium chloride fine powder is dissolved in 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 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 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, cadmium chloride solution step one obtained and step 2 obtain mixes mutually, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution and the step 4 that step 3 are obtained obtain 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, reactor inner bag step 5 being equipped with reaction mass are placed in reactor, and sealing, 110
ounder C, be incubated and carry out hydrothermal treatment consists in 10 hours, then allow reactor naturally cool to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, after filtration, oven dry, obtain molybdic acid cadmium porous ball.The XRD figure spectrum obtained 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, thus illustrates that molybdic acid cadmium crystal structure is good; Fig. 2 illustrates that molybdic acid cadmium crystal of the present invention is the spherical of porous, and the diameter of molybdic acid cadmium porous ball is about 700-900nm.
Embodiment 2
Step one, Cadmium chloride fine powder is dissolved in 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 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 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, cadmium chloride solution step one obtained and step 2 obtain mixes mutually, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution and the step 4 that step 3 are obtained obtain 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, reactor inner bag step 5 being equipped with reaction mass are placed in reactor, and sealing, 160
ounder C, be incubated and carry out hydrothermal treatment consists in 6 hours, then allow reactor naturally cool to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, after filtration, oven dry, obtain molybdic acid cadmium porous ball.
Embodiment 3
Step one, Cadmium chloride fine powder is dissolved in 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 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 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, cadmium chloride solution step one obtained and step 2 obtain mixes mutually, obtains cadmium acetate precipitation as reaction precursor;
The cadmium acetate precipitation solution that step 5, the sodium molybdate solution and the step 4 that step 3 are obtained obtain 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, reactor inner bag step 5 being equipped with reaction mass are placed in reactor, and sealing, 200
ounder C, be incubated and carry out hydrothermal treatment consists in 3 hours, then allow reactor naturally cool to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, after filtration, oven dry, obtain molybdic acid cadmium porous ball.
Claims (2)
1. a preparation method for molybdic acid cadmium porous ball, is characterized in that: step one, Cadmium chloride fine powder is dissolved in 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 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 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, cadmium chloride solution step one obtained and step 2 obtain mixes mutually, and the ratio of mixing is 1:1, obtains cadmium acetate precipitation as reaction precursor; The cadmium acetate precipitation solution that step 5, the sodium molybdate solution and the step 4 that step 3 are obtained obtain mixes mutually, and the ratio of mixing is 1:1, then joins in reactor inner bag; Step 6, reactor inner bag step 5 being equipped with reaction mass are placed in reactor, and sealing, 110 ~ 200
ounder C, be incubated and carry out hydrothermal treatment consists in 2 ~ 12 hours, then allow reactor naturally cool to room temperature, after unloading still, by distilled water repetitive scrubbing reaction product, after filtration, oven dry, obtain molybdic acid cadmium porous ball.
2. 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 sodium molybdate solution step 3 obtained obtains 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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| CN103833080B true CN103833080B (en) | 2016-01-20 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104671285B (en) * | 2015-01-28 | 2016-08-03 | 洛阳理工学院 | A kind of preparation method of cadmium molybdate nano rod |
| 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 |
| CN109336178B (en) * | 2018-12-06 | 2020-12-08 | 洛阳理工学院 | Preparation method of cadmium molybdate dendritic crystal |
| CN111704169B (en) * | 2020-07-01 | 2022-09-30 | 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 (1)
| Title |
|---|
| CdMoO4微球的微波辅助法快速合成及其光催化性能;张大凤，等。;《材料导报》;20110531;第25卷(第S1期);第82页左联第21-25行 * |
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