MnMoO4Micro-nano material and preparation method thereof
Technical Field
The invention belongs to the field of micro-nano materials, and particularly relates to MnMoO4Micro-nano material and a preparation method thereof.
Background
Manganese molybdate (MnMoO)4) Is an important inorganic functional material, has excellent magnetic property, catalytic property and electrochemical property due to the special crystal structure and the changeable combination state of molybdenum and manganese elements, is often used for preparing catalysts, luminescent materials and humidity detectionThe device and the electrode material are widely applied to the fields of chemical industry, national defense, electronic industry and the like.
MnMoO4The preparation and application of micro-nano materials and composite materials thereof are also reported. For example, chinese patent No. cn201710130453.x prepares a manganese molybdate porous nanotube by using an electrostatic spinning method, and a cross-linked network structure is formed between the porous nanotubes, so that the transfer of ions/electrons and the permeation of an electrolyte can be effectively promoted, the diffusion path of electrolyte ions in a material is shortened, and the manganese molybdate porous nanotube has a higher specific capacity, an excellent rate capability and a better cycling stability as an electrode material. The Chinese patent CN202011505651.8 combines a coprecipitation method with high-temperature calcination to prepare the carbon-coated manganese molybdate single-crystal micron rod, which is used as a cathode material of a sodium ion battery and shows better electrochemical performance compared with the manganese molybdate micron rod without carbon coating. In the Chinese patent CN201110347430.7, ammonium molybdate and manganese nitrate are used as reaction raw materials, Cetyl Trimethyl Ammonium Bromide (CTAB) is used as a surfactant, distilled water is used as a solvent, and a microwave radiation method is utilized to prepare the manganese molybdate material assembled into a micron rod structure by nanosheets. MnMoO disclosed above4Related reports prove that the MnMoO with different micro-nano structures4Has wide application in various aspects. However, the above MnMoO4The preparation of nanomaterials usually requires relatively complex and expensive equipment, such as microwave radiation, electrospinning, etc. Therefore, the MnMoO having a novel structure is prepared using a relatively simple method4The micro-nano material is worthy of further exploration.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide MnMoO4Micro-nano material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
MnMoO4The preparation method of the micro-nano material comprises the following steps:
1) dissolving 1 part of sodium molybdate, 0.5-1 part of polyvinylpyrrolidone and 1-4 parts of manganese acetate tetrahydrate in 50 parts of deionized water according to parts by mass to obtain a mixed solution A;
2) reacting the mixed solution A under an ultrasonic condition for 1-3 h, and filtering, washing and drying an obtained product after the reaction is finished to obtain a product B;
3) dissolving 1 part of the product B and 0.5-1 part of 3- (dibutylamino) phenol in 50 parts of deionized water by mass, stirring at room temperature for 1-3 hours, and then filtering, washing and drying to obtain a product C;
4) calcining the product C at 600-800 ℃ for 1h to obtain MnMoO4And (3) micro-nano materials.
Further, in step 2), the ultrasonic condition is provided by an ultrasonic generator.
Further, the ultrasonic power of the ultrasonic generator is 60-100W.
Further, in the step 2), washing with water is performed for 3-6 times.
Further, in the step 2), the drying temperature is 50-70 ℃, and the drying time is 6-10 hours.
Further, in the step 3), washing with water is performed for 3-6 times.
Furthermore, the drying temperature is 50-70 ℃, and the drying time is 6-10 hours.
The MnMoO prepared by the preparation method of the invention4And (3) micro-nano materials.
Furthermore, the structure is in a cauliflower-shaped multilevel structure.
Compared with the prior art, the invention has the following beneficial effects:
MnMoO of the invention4The preparation method of the micro-nano material uses a molybdenum source and a manganese source which are cheap as raw materials, and MnMoO is prepared by adjusting technological parameters such as ultrasound, calcination and the like4The nanoparticles self-assemble into unique micron-scale multilevel structures. The invention adjusts the ultrasonic condition to form regular MnMoO at room temperature4And (3) precursor. And the addition of polyvinylpyrrolidone and 3- (dibutylamino) phenol solution to MnMoO4The formation of the cauliflower-shaped special appearance has certain auxiliary effect. After the product is properly calcined, the purity and crystallinity of the product are further improved. The preparation methodThe method is simple and easy to operate, has strong repeatability, low cost and no pollution to the environment, and is suitable for industrial mass production.
MnMoO of the invention4The micro-nano material has the characteristics of distinct morphological characteristics, high purity, high crystallinity, large specific surface and the like, and has wide application prospects in the fields of photocatalysis materials, luminescent materials, sensing, new energy and the like.
Drawings
FIG. 1 is an XRD pattern of the product prepared in example 1;
FIG. 2 is a scanning electron micrograph of the product prepared in example 1.
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
According to the mass parts, 1 part of sodium molybdate, 0.5 part of polyvinylpyrrolidone and 1 part of manganese acetate tetrahydrate are dissolved in 50 parts of deionized water to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 1h under the ultrasonic power of 100W, filtering, washing with water, and drying to obtain a product B. And (3) dissolving 1 part of the product B and 0.5 part of 3- (dibutylamino) phenol in 50 parts of deionized water according to parts by mass, stirring for 3 hours at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C in a muffle furnace at 600 ℃ for 1h to obtain MnMoO4And (3) micro-nano materials.
Referring to fig. 1, fig. 1 shows MnMoO prepared according to the present invention4The XRD pattern of the micro-nano material can determine MnMoO from figure 14The micro-nano material has high phase composition and high purity.
Referring to fig. 2, fig. 2 shows MnMoO prepared according to the present invention4The obtained MnMoO can be seen in the scanning electron microscope picture of the micro-nano material4The micro-nano material has distinct morphology and features and is in a cauliflower-shaped multi-level structure.
Example 2
According to the mass parts, 1 part of sodium molybdate, 0.8 part of polyvinylpyrrolidone and 50 parts of deionized water of 2 parts of manganese acetate tetrahydrate are added to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 3 hours under the ultrasonic power of 60W, filtering, washing with water, and drying to obtain a product B. And (3) dissolving 1 part of the product B and 1 part of 3- (dibutylamino) phenol in 50 parts of deionized water according to parts by mass, stirring for 1 hour at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C at 800 ℃ for 1h to obtain MnMoO4And (3) micro-nano materials.
Example 3
According to the mass parts, 1 part of sodium molybdate, 1 part of polyvinylpyrrolidone and 4 parts of manganese acetate tetrahydrate are dissolved in 50 parts of deionized water to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 2 hours under the ultrasonic power of 80W, filtering, washing with water, and drying to obtain a product B. According to the mass portion of the raw materials,and dissolving 1 part of the product B and 0.5 part of 3- (dibutylamino) phenol in 50 parts of deionized water, stirring for 2 hours at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C at 700 ℃ for 1h to obtain MnMoO4And (3) micro-nano materials.
Example 4
According to the mass parts, 1 part of sodium molybdate, 0.5 part of polyvinylpyrrolidone and 1-4 parts of manganese acetate tetrahydrate are dissolved in 50 parts of deionized water to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 1h under the ultrasonic power of 100W, filtering, washing with water, and drying to obtain a product B. And (3) dissolving 1 part of the product B and 1 part of 3- (dibutylamino) phenol in 50 parts of deionized water according to parts by mass, stirring for 1 hour at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C at 800 ℃ for 1h to obtain MnMoO4And (3) micro-nano materials.
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.