CN110451566B - Europium tungstate carbon composite nanospheres and preparation method thereof - Google Patents
Europium tungstate carbon composite nanospheres and preparation method thereof Download PDFInfo
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- CN110451566B CN110451566B CN201910759960.9A CN201910759960A CN110451566B CN 110451566 B CN110451566 B CN 110451566B CN 201910759960 A CN201910759960 A CN 201910759960A CN 110451566 B CN110451566 B CN 110451566B
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses europium tungstate carbon composite nanospheres and a preparation method thereof, belonging to the field of preparation of inorganic nanomaterials. The preparation method of the europium tungstate carbon composite nanospheres prepares the europium tungstate precursor by stirring at normal temperature and normal pressure, adds the aminophenol derivative and obtains the europium tungstate carbon composite nanospheres by simple calcination treatment, and the coordination effect of the added aminophenol derivative and the europium tungstate can effectively control the microstructure of a target product.
Description
Technical Field
The invention belongs to the field of inorganic nano material preparation, and particularly relates to europium tungstate carbon composite nanospheres and a preparation method thereof.
Background
Nanostructured materials have gained attention in recent years, and their unique nanocrystalline properties are influenced not only by composition, but also by size, shape, and size distribution of the material. In recent years, along with the rapid development of industrialization, toxic and harmful organic substances such as rhodamine B, methyl blue, methyl orange and the like cause more and more serious harm to the environment, particularly water resources. The adoption of the nano material has important significance for the catalytic degradation of the harmful substances. Rare earth metal tungstates include: magnetic materials, catalysts, luminescent materials, fluorescent materials, solid state fuel cell electrode materials, and the like.
The Chinese patent 201210057068.4 uses sodium tungstate and cerium nitrate as reaction raw materials, uses a mixed solution of distilled water and acetone as a system liquid phase reaction environment, and applies a microwave radiation method to controllably prepare the cerium tungstate nano sheet material. The obtained cerium tungstate material has an ultra-thin sheet structure, and has a large specific surface area and high chemical activity. Chinese patent 201110023272.X discloses a hydrothermal method for preparing a series of rare earth tungstates, including ytterbium, thulium, holmium, gadolinium and other rare earth metals. The Chinese patent 201811582417.8 discloses a flower-like microsphere-structured potassium yttrium tungstate prepared by using a hydrothermal method to assist a surfactant. The rare earth metal tungstate prepared by the method has the problems of large size and single appearance structure.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides europium tungstate-carbon composite nanospheres and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of europium tungstate carbon composite nanospheres comprises the following steps:
1) preparing a europium salt methanol solution and a tungstate aqueous solution; wherein, the concentration of europium ions in the europium salt methanol solution is 0.1-0.5mol/L, and the concentration of tungstate ions in the tungstate aqueous solution is 0.3-0.5 mol/L;
2) mixing the europium salt methanol solution and the tungstate aqueous solution according to a volume ratio of 1: (0.5-1.5), stirring the obtained mixed solution at room temperature for 3-5h for reaction, and cleaning and drying after the reaction is finished to obtain a precursor;
3) dispersing the precursor in an aminophenol derivative aqueous solution to obtain a reaction solution A, stirring the reaction solution A at room temperature for 3-7 hours for reaction, and filtering, cleaning and drying after the reaction is finished to obtain a product A;
wherein the concentration of the aminophenol derivative aqueous solution is 0.1-0.3 mol/L, and 40mg of the product A is added into each 100mL of the aminophenol derivative aqueous solution;
4) calcining the product A for 2h at the temperature of 500-700 ℃ in the inert gas atmosphere to obtain the europium tungstate-carbon composite nanospheres.
Further, in step 1), the europium salt is europium nitrate or europium acetate.
Further, the tungstate in step 1) is ammonium tungstate or sodium tungstate.
Further, the aminophenol derivative in the step 3) is 2-amino-4-nitrophenol, 4- (2-aminoethyl) -1, 2-benzenediol or 4-acetaminophenol.
The europium tungstate carbon composite nanospheres prepared by the preparation method.
Furthermore, the particle size of the nanospheres is 90-100 nm.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the europium tungstate carbon composite nanospheres prepares the europium tungstate precursor by stirring at normal temperature and normal pressure, adds the aminophenol derivative and obtains the europium tungstate carbon composite nanospheres by simple calcination treatment, and the coordination effect of the added aminophenol derivative and the europium tungstate can effectively control the microstructure of a target product.
The europium tungstate carbon composite nanospheres are uniform in size and regular in shape, and the nano material prepared by the method can be widely applied to the fields of photoluminescence, electromagnetic materials, photocatalysis, energy storage and conversion and the like, and has wide market prospect.
Drawings
Fig. 1 is an SEM image of europium tungstate carbon composite nanospheres prepared in example 1 of the present invention;
fig. 2 is an XRD pattern of the europium tungstate carbon composite nanosphere prepared in example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
1) Respectively preparing a 0.1mol/L europium nitrate methanol solution and a 0.3mol/L ammonium tungstate aqueous solution;
2) according to the volume ratio of 1: 0.5 mixing the europium nitrate methanol solution and the ammonium tungstate aqueous solution, stirring for 4 hours at room temperature, and cleaning and drying to obtain a precursor;
3) dispersing 20mg of precursor in 50mL of 0.1 mol/L2-amino-4-nitrophenol aqueous solution to obtain reaction liquid A, stirring the reaction liquid A at room temperature for 3 hours for reaction, and after the reaction is finished, filtering, cleaning and drying to obtain a product A;
4) and calcining the product A at 500 ℃ for 2h in a nitrogen atmosphere to obtain the europium tungstate carbon composite nanospheres.
Referring to fig. 1, fig. 1 is an SEM image of europium tungstate carbon composite nanospheres prepared in example 1 of the present invention, and it can be seen that the obtained products have spherical morphology and diameters of 90-100 nm.
Referring to fig. 2, fig. 2 is an XRD pattern of the europium tungstate carbon composite nanosphere prepared in example 1 of the present invention, which is tested to have a 2 theta range of 10-80 deg.. The figure shows that the diffraction peak is sharp, the diffraction intensity is high, and other miscellaneous peaks do not appear, which indicates that the product synthesized by the preparation method has high purity and good crystallinity.
Example 2
1) Respectively preparing a 0.2mol/L europium acetate methanol solution and a 0.4mol/L sodium tungstate aqueous solution;
2) according to the volume ratio of 1: 0.7 mixing the europium acetate methanol solution and the sodium tungstate aqueous solution, standing for 10 minutes, stirring for 4 hours at room temperature, and cleaning and drying to obtain a precursor;
3) dispersing 10mg of the precursor in 25mL of 0.3 mol/L4- (2-aminoethyl) -1, 2-benzenediol aqueous solution to obtain a reaction solution A, stirring the reaction solution A at room temperature for 7 hours for reaction, and after the reaction is finished, filtering, cleaning and drying to obtain a product A;
4) and calcining the product A at 700 ℃ for 2h under the argon atmosphere to obtain the europium tungstate carbon composite nanospheres.
Example 3
1) Respectively preparing a 0.3mol/L europium nitrate methanol solution and a 0.5mol/L ammonium tungstate aqueous solution;
2) according to the volume ratio of 1: 1 mixing a europium nitrate methanol solution and an ammonium tungstate aqueous solution, standing for 10 minutes, stirring for 3 hours at room temperature for reaction, and cleaning and drying after the reaction is finished to obtain a precursor;
3) dispersing 10mg of precursor in 25mL of 0.3 mol/L4-acetamidophenol aqueous solution to obtain reaction liquid A, stirring the reaction liquid A at room temperature for 6 hours for reaction, and after the reaction is finished, filtering, cleaning and drying to obtain a product A;
4) and calcining the product A at 600 ℃ for 2h under the argon atmosphere to obtain the europium tungstate carbon composite nanospheres.
Example 4
1) Respectively preparing a 0.4mol/L europium acetate methanol solution and a 0.3mol/L sodium tungstate aqueous solution;
2) according to the volume ratio of 1: 1.5 mixing the europium acetate methanol solution and the sodium tungstate aqueous solution, standing for 10 minutes, stirring for 3 hours at room temperature for reaction, and cleaning and drying after the reaction is finished to obtain a precursor;
3) dispersing 10mg of the precursor in 25mL of 0.2 mol/L4- (2-aminoethyl) -1, 2-benzenediol aqueous solution to obtain a reaction solution A, stirring the reaction solution A at room temperature for 7 hours, and after the reaction is finished, filtering, cleaning and drying to obtain a product A;
4) and calcining the product A at 500 ℃ for 2h under the argon atmosphere to obtain the europium tungstate carbon composite nanospheres.
Example 5
1) Respectively preparing a 0.5mol/L europium nitrate methanol solution and a 0.4mol/L ammonium tungstate aqueous solution;
2) according to the volume ratio of 1: 0.7 mixing the europium nitrate methanol solution and the ammonium tungstate aqueous solution, standing for 10 minutes, stirring for 4 hours at room temperature for reaction, and cleaning and drying to obtain a precursor;
3) dispersing 10mg of precursor in 25mL of 0.2 mol/L2-amino-4-nitrophenol aqueous solution to obtain reaction liquid A, stirring the reaction liquid A at room temperature for 5 hours to react, and after the reaction is finished, filtering, cleaning and drying to obtain a product A;
4) and calcining the product A at 550 ℃ for 2h under the argon atmosphere to obtain the europium tungstate carbon composite nanospheres.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (5)
1. A preparation method of europium tungstate carbon composite nanospheres is characterized by comprising the following steps of:
1) preparing a europium salt methanol solution and a tungstate aqueous solution; wherein, the concentration of europium ions in the europium salt methanol solution is 0.1-0.5mol/L, and the concentration of tungstate ions in the tungstate aqueous solution is 0.3-0.5 mol/L;
2) mixing the europium salt methanol solution and the tungstate aqueous solution according to a volume ratio of 1: (0.5-1.5), stirring the obtained mixed solution at room temperature for 3-5h for reaction, and cleaning and drying after the reaction is finished to obtain a precursor;
3) dispersing the precursor in an aminophenol derivative aqueous solution to obtain a reaction solution A, stirring the reaction solution A at room temperature for 3-7 hours for reaction, and filtering, cleaning and drying after the reaction is finished to obtain a product A;
wherein the concentration of the aminophenol derivative aqueous solution is 0.1-0.3 mol/L, and 40mg of the product A is added into each 100mL of the aminophenol derivative aqueous solution;
in the step 3), the aminophenol derivative is 2-amino-4-nitrophenol, 4- (2-aminoethyl) -1, 2-benzenediol or 4-acetaminophenol;
4) calcining the product A for 2h at the temperature of 500-700 ℃ in the inert gas atmosphere to obtain the europium tungstate-carbon composite nanospheres.
2. The method for preparing europium tungstate carbon composite nanospheres according to claim 1, wherein the europium salt in step 1) is europium nitrate or europium acetate.
3. The method for preparing europium tungstate-carbon composite nanospheres of claim 1, wherein the tungstate in step 1) is ammonium tungstate or sodium tungstate.
4. A europium tungstate carbon composite nanosphere prepared according to the preparation method of any one of claims 1 to 3.
5. The europium tungstate-carbon composite nanospheres of claim 4, wherein the particle size of the nanospheres is 90-100 nm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951686A (en) * | 2012-11-14 | 2013-03-06 | 陕西科技大学 | Preparation method for granular manganese tungstate nanocrystals |
| CN103387265A (en) * | 2013-07-25 | 2013-11-13 | 洛阳理工学院 | Manganese tungsten nano crystal material and preparation method thereof |
| CN107486200A (en) * | 2017-09-21 | 2017-12-19 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of the compound wolframic acid Mn catalyst of carbon |
| CN108365196A (en) * | 2018-02-06 | 2018-08-03 | 湖北大学 | A kind of MnWO4The preparation method and application of/C composite |
| CN109659145A (en) * | 2018-12-17 | 2019-04-19 | 上海应用技术大学 | A method of preparing porous spherical manganese oxide/carbon complex |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951686A (en) * | 2012-11-14 | 2013-03-06 | 陕西科技大学 | Preparation method for granular manganese tungstate nanocrystals |
| CN103387265A (en) * | 2013-07-25 | 2013-11-13 | 洛阳理工学院 | Manganese tungsten nano crystal material and preparation method thereof |
| CN107486200A (en) * | 2017-09-21 | 2017-12-19 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of the compound wolframic acid Mn catalyst of carbon |
| CN108365196A (en) * | 2018-02-06 | 2018-08-03 | 湖北大学 | A kind of MnWO4The preparation method and application of/C composite |
| CN109659145A (en) * | 2018-12-17 | 2019-04-19 | 上海应用技术大学 | A method of preparing porous spherical manganese oxide/carbon complex |
Non-Patent Citations (2)
| Title |
|---|
| Fe-Mo与其碳复合材料的电化学合成及其应用研究;张道明;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20180215;第32-40页 * |
| Mn-Mo-O catalyst for methanol oxidation preparation and characterization of the catalysts;Ivanov,Krasimir et al.;《Collet.Czech.Chem.Commun》;19921231;第2529-2538页 * |
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