CN111704169B - Preparation method of manganese molybdate nanosheet crystal - Google Patents
Preparation method of manganese molybdate nanosheet crystal Download PDFInfo
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- CN111704169B CN111704169B CN202010625656.8A CN202010625656A CN111704169B CN 111704169 B CN111704169 B CN 111704169B CN 202010625656 A CN202010625656 A CN 202010625656A CN 111704169 B CN111704169 B CN 111704169B
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- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 24
- 239000011572 manganese Substances 0.000 title claims abstract description 24
- 239000013078 crystal Substances 0.000 title claims abstract description 22
- 239000002135 nanosheet Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 61
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 39
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 39
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 39
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 39
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 30
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 30
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 30
- 239000011565 manganese chloride Substances 0.000 claims abstract description 30
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 30
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims abstract description 27
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims abstract description 27
- 238000001556 precipitation Methods 0.000 claims abstract description 23
- LAYZVIPDEOEIDY-ZVGUSBNCSA-L (2R,3R)-2,3-dihydroxybutanedioate manganese(2+) Chemical compound [Mn++].O[C@H]([C@@H](O)C([O-])=O)C([O-])=O LAYZVIPDEOEIDY-ZVGUSBNCSA-L 0.000 claims abstract description 20
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 15
- 229940074439 potassium sodium tartrate Drugs 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 4
- 239000002243 precursor Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000001476 sodium potassium tartrate Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a preparation method of a manganese molybdate nanosheet crystal, which mainly comprises the steps of respectively preparing sodium molybdate, manganese chloride, potassium sodium tartrate and a polyvinyl alcohol solution, then mixing the potassium sodium tartrate and the manganese chloride solution to obtain a manganese tartrate precipitation solution, and then carrying out hydrothermal treatment on the manganese tartrate precipitation solution to obtain a reaction precursor; and mixing the sodium molybdate solution with the polyvinyl alcohol solution, carrying out ultrasonic treatment, and carrying out hydrothermal treatment on the mixture and the obtained manganese tartrate precursor again to obtain the manganese molybdate nanosheet crystal. The preparation method of the manganese molybdate nanosheet crystal provided by the invention has the advantages of controllable morphology, simple process, low cost and the like, and is easy to realize industrial production.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a preparation method of a manganese molybdate nanosheet crystal.
Background
The molybdate has excellent magnetic, electric, optical and other properties, so that the molybdate has wide application prospects in the aspects of magnetic materials, luminescent materials, laser donor materials, catalytic materials, antibacterial materials and the like. Manganese molybdate is a very important functional material and has very wide application in the fields of catalysts, optoelectronic devices, sensors, supercapacitors, electrode materials and the like. As is well known, the performance of the nano material mainly depends on factors such as the morphology and the size of the nano crystal, and the like, so that the manganese molybdate nano crystal with a special morphology is prepared, and has very important significance in the aspects of theoretical basic research and practical application.
The wide application of nano devices has put higher demands on the diversification of the shapes of nano materials, the performances of the nano materials depend on the shapes and the sizes of the nano materials to a great extent, and therefore, the development of nano particles with brand-new shapes is still the research hotspot and the focus of scientific workers nowadays. The manganese molybdate nanosheet crystal prepared by the invention has a unique two-dimensional sheet structure and a large specific surface area, so that the manganese molybdate nanosheet crystal has a very good application prospect in the fields of catalysts, optoelectronic devices, sensors, supercapacitors, electrode materials and the like.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the preparation method of the manganese molybdate nanosheet crystal, which has the advantages of simple process, controllable morphology and easy realization of industrialization.
The purpose of the invention is realized by adopting the following technical scheme. The preparation method of the manganese molybdate nanosheet crystal provided by the invention comprises the following eight steps:
1) dissolving sodium potassium tartrate in deionized water to form a sodium potassium tartrate aqueous solution, and adjusting the concentration of the sodium potassium tartrate aqueous solution to 0.2-1.0 mol/L;
2) dissolving manganese chloride in deionized water to form a manganese chloride aqueous solution, and adjusting the concentration of the manganese chloride aqueous solution to be 0.2-1.0 mol/L;
3) mixing the potassium sodium tartrate aqueous solution prepared in the step 1) and the manganese chloride aqueous solution prepared in the step 2) to obtain a manganese tartrate precipitation solution, and then carrying out ultrasonic treatment on the manganese tartrate precipitation solution;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate aqueous solution to 0.2-1.0 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol aqueous solution to 0.5%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring the mixed solution;
7) adding the manganese tartrate precipitation solution subjected to ultrasonic treatment in the step 3) into the inner container of the reaction kettle, adjusting the volume of the reaction material by using distilled water, sealing, performing hydrothermal treatment on the reaction material, and cooling the reaction kettle to room temperature;
8) and (3) after the reaction kettle in the step 7) is opened, adding the mixed solution of the sodium molybdate solution and the polyvinyl alcohol obtained in the step 6) into the kettle, sealing, carrying out hydrothermal treatment on the mixed solution, then cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing the reaction product with distilled water, filtering and drying the reaction product, and obtaining the manganese molybdate nanosheet crystal.
Further, the molar ratio of potassium sodium tartrate to manganese chloride in the manganese tartrate precipitation solution obtained in the step 3) is 1: 1.
Further, the ultrasonic power for ultrasonic treatment of the manganese tartrate precipitation solution is 500-1000W, and the ultrasonic treatment time is 30-60 minutes.
Further, stirring the mixed solution of sodium molybdate and polyvinyl alcohol obtained in the step 6) for 30-60 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1.
Further, regulating the volume of the reaction materials in the inner container of the reaction kettle in the step 7) by using distilled water to make the volume of the reaction materials reach 40% of the volume of the inner container of the reaction kettle, and carrying out hydrothermal treatment on the reaction kettle at the temperature of 120-150 ℃ for 6-12 hours.
Further, regulating the volume of the reaction materials in the inner container of the reaction kettle in the step 8) by using distilled water to enable the volume to reach 80% of the volume of the inner container of the reaction kettle, and carrying out hydrothermal treatment on the reaction kettle at the temperature of 160-220 ℃ for 12-24 hours.
Further, mixing a potassium sodium tartrate aqueous solution and a manganese chloride aqueous solution, and performing hydrothermal treatment to obtain a manganese tartrate precipitation solution as a reaction precursor.
Furthermore, the purity of the sodium molybdate, the potassium sodium tartrate, the manganese chloride and the polyvinyl alcohol is not lower than the chemical purity.
By means of the technical scheme, the preparation method of the manganese molybdate nanosheet crystal has the advantages of controllable shape, simplicity in operation, low cost and the like, and is easy for industrial production.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following preferred embodiments are specifically described below with reference to the accompanying drawings.
Drawings
Figure 1 is an XRD spectrum of manganese molybdate nanosheet crystals synthesized in this example,
fig. 2 is a Transmission Electron Microscope (TEM) photograph of the manganese molybdate nanosheet crystals synthesized in this example.
Detailed Description
Referring to fig. 1 and fig. 2, the present invention will be further described with reference to the following examples.
Example 1:
1) dissolving sodium potassium tartrate in deionized water to form an aqueous solution, and adjusting the concentration of the sodium potassium tartrate in the aqueous solution to be 0.2 mol/L;
2) dissolving manganese chloride in deionized water to form a manganese chloride aqueous solution, and adjusting the concentration of the manganese chloride in the solution to be 0.2 mol/L;
3) mixing the aqueous solution of potassium sodium tartrate prepared in the step 1) with the aqueous solution of manganese chloride prepared in the step 2) to obtain a manganese tartrate precipitation solution (wherein the molar ratio of potassium sodium tartrate to manganese chloride is 1:1), and then putting a container filled with the manganese tartrate precipitation solution into ultrasonic waves for ultrasonic treatment, wherein the ultrasonic power is 500W, and the ultrasonic time is 30 minutes;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 0.2 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol in the solution to 0.5%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 30 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1;
7) adding the mixed precipitation solution subjected to ultrasonic treatment in the step 3) into a liner of a reaction kettle, adjusting the volume of reaction materials in the liner of the reaction kettle to 40% of the volume of the liner of the reaction kettle by using distilled water, sealing, preserving the temperature of the reaction kettle and the mixed precipitation solution inside the reaction kettle at 120 ℃ for 6 hours, performing hydrothermal treatment, and naturally cooling the reaction kettle to room temperature;
8) and (3) after the reaction kettle in the step 7) is opened, adding the mixed solution of the sodium molybdate solution and the polyvinyl alcohol obtained in the step 6) into the kettle, adjusting the volume of the reaction material in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using distilled water, sealing, preserving heat at 160 ℃ for 12 hours for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing the reaction product by using the distilled water, filtering and drying to obtain the manganese molybdate nanosheet crystal. The diameter of the manganese molybdate nano-sheet crystal is about 400-500nm, and the thickness is about 5-10 nm.
Example 2
1) Dissolving sodium potassium tartrate in deionized water to form an aqueous solution, and adjusting the concentration of the sodium potassium tartrate in the aqueous solution to be 0.5 mol/L;
2) dissolving manganese chloride in deionized water to form a manganese chloride aqueous solution, and adjusting the concentration of the manganese chloride in the solution to be 0.5 mol/L;
3) mixing the aqueous solution of potassium sodium tartrate prepared in the step 1) with the aqueous solution of manganese chloride prepared in the step 2) to obtain a manganese tartrate precipitation solution (wherein the molar ratio of potassium sodium tartrate to manganese chloride is 1:1), and then putting a container filled with the manganese tartrate precipitation solution into ultrasonic waves for ultrasonic treatment, wherein the ultrasonic power is 800W, and the ultrasonic time is 45 minutes;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 0.5 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol in the solution to 0.5%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 45 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1;
7) adding the mixed precipitation solution after the ultrasonic treatment in the step 3) into a liner of a reaction kettle, adjusting the volume of reaction materials in the liner of the reaction kettle to 40% of the volume of the liner of the reaction kettle by using distilled water, sealing, preserving the heat at 130 ℃ for 10 hours to perform hydrothermal treatment, and naturally cooling the reaction kettle to room temperature;
8) and (3) after the reaction kettle in the step 7) is opened, adding the mixed solution of the sodium molybdate solution and the polyvinyl alcohol obtained in the step 6) into the kettle, adjusting the volume of the reaction material in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using distilled water, sealing, preserving heat at 200 ℃ for 16 hours to perform hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing the reaction product by using the distilled water, filtering and drying to obtain the manganese molybdate nanosheet crystal.
Example 3
1) Dissolving sodium potassium tartrate in deionized water to form an aqueous solution, and adjusting the concentration of the sodium potassium tartrate in the aqueous solution to be 1.0 mol/L;
2) dissolving manganese chloride in deionized water to form a manganese chloride aqueous solution, and adjusting the concentration of the manganese chloride in the solution to be 1.0 mol/L;
3) mixing the aqueous solution of potassium sodium tartrate prepared in the step 1) with the aqueous solution of manganese chloride prepared in the step 2) to obtain a manganese tartrate precipitation solution (wherein the molar ratio of potassium sodium tartrate to manganese chloride is 1:1), and then putting a container filled with the manganese tartrate precipitation solution into ultrasonic waves for ultrasonic treatment, wherein the ultrasonic power is 1000W, and the ultrasonic time is 60 minutes;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate in the solution to be 1.0 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol in the solution to 0.5%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) with the polyvinyl alcohol aqueous solution prepared in the step 5) to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring for 60 minutes, wherein the volume ratio of the sodium molybdate solution to the polyvinyl alcohol solution is 1: 1;
7) adding the mixed precipitation solution after the ultrasonic treatment in the step 3) into a liner of a reaction kettle, adjusting the volume of reaction materials in the liner of the reaction kettle to 40% of the volume of the liner of the reaction kettle by using distilled water, sealing, preserving heat at 150 ℃ for 12 hours to perform hydrothermal treatment, and naturally cooling the reaction kettle to room temperature;
8) opening the reaction kettle in the step 7), adding the mixed solution of the sodium molybdate solution and the polyvinyl alcohol obtained in the step 6) into the kettle, adjusting the volume of the reaction material in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using distilled water, sealing, carrying out heat preservation at 220 ℃ for 24 hours for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing the reaction product by using distilled water, filtering and drying to obtain the manganese molybdate nanosheet crystal.
The above description is only a preferred embodiment of the present invention, and any person skilled in the art can make any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the present invention without departing from the scope of the present invention, and still fall within the scope of the present invention.
Claims (3)
1. A preparation method of manganese molybdate nanosheet crystals is characterized by comprising the following steps: comprises the following eight steps:
1) dissolving sodium potassium tartrate in deionized water to form a sodium potassium tartrate aqueous solution, and adjusting the concentration of the sodium potassium tartrate aqueous solution to 0.2-1.0 mol/L;
2) dissolving manganese chloride in deionized water to form a manganese chloride aqueous solution, and adjusting the concentration of the manganese chloride aqueous solution to 0.2-1.0 mol/L;
3) mixing the potassium sodium tartrate aqueous solution prepared in the step 1) and the manganese chloride aqueous solution prepared in the step 2) to obtain a manganese tartrate precipitation solution serving as a reaction precursor, and then carrying out ultrasonic treatment on the manganese tartrate precipitation solution, wherein the molar ratio of potassium sodium tartrate to manganese chloride in the manganese tartrate precipitation solution is 1: 1;
4) dissolving sodium molybdate in deionized water to form a sodium molybdate aqueous solution, and adjusting the concentration of the sodium molybdate aqueous solution to 0.2-1.0 mol/L;
5) dissolving polyvinyl alcohol in deionized water to form a polyvinyl alcohol aqueous solution, and adjusting the concentration of the polyvinyl alcohol aqueous solution to 0.5%;
6) mixing the sodium molybdate aqueous solution prepared in the step 4) and the polyvinyl alcohol aqueous solution prepared in the step 5) according to the volume ratio of 1:1 to obtain a mixed solution of sodium molybdate and polyvinyl alcohol, and stirring the mixed solution for 30-60 minutes;
7) adding the manganese tartrate precipitation solution subjected to the ultrasonic treatment in the step 3) into a reaction kettle liner, adjusting the volume of the reaction material by using distilled water to 40% of the volume of the reaction kettle liner, sealing, carrying out hydrothermal treatment on the reaction kettle at the temperature of 120-150 ℃ for 6-12 hours, and cooling the reaction kettle to room temperature;
8) opening the reaction kettle in the step 7), adding the mixed solution of the sodium molybdate solution and the polyvinyl alcohol obtained in the step 6) into the kettle, adjusting the volume of the reaction material in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using distilled water, sealing, then carrying out hydrothermal treatment on the reaction kettle at the temperature of 160-220 ℃ for 12-24 hours, cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing the reaction product by using distilled water, filtering and drying the reaction product to obtain the manganese molybdate nanosheet crystal.
2. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: the ultrasonic power for ultrasonic treatment of the manganese tartrate precipitation solution is 500-1000W, and the ultrasonic treatment time is 30-60 minutes.
3. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: the purities of the sodium molybdate, the sodium potassium tartrate, the manganese chloride and the polyvinyl alcohol are not lower than the chemical purity.
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2020
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| CN103833080A (en) * | 2014-03-25 | 2014-06-04 | 洛阳理工学院 | Preparation method for cadmium molybdate porous spheres |
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| CN104192914A (en) * | 2014-08-29 | 2014-12-10 | 洛阳理工学院 | Preparation method of manganese tungsten single-crystalline nanowire |
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