阅读说明：本技术 一种钼酸锰纳米片晶体的制备方法 (Preparation method of manganese molybdate nanosheet crystal ) 是由 王永刚 杨琳琳 胡淑静 王宜森 任慧慧 王玉江 于 2020-07-01 设计创作，主要内容包括：本发明一种钼酸锰纳米片晶体的制备方法,主要步骤是先分别制备出钼酸钠、氯化锰、酒石酸钾钠、聚乙烯醇溶液,然后将酒石酸钾钠和氯化锰溶液混合,得到酒石酸锰沉淀溶液,然后将酒石酸锰沉淀溶液水热处理后作为反应先驱体；另外将钼酸钠溶液与聚乙烯醇溶液混合,并进行超声处理后,与前面得到的酒石酸锰先驱体一起再次进行水热处理后,得到钼酸锰纳米片晶体。本发明提供的钼酸锰纳米片晶体的制备方法,具有形貌可控、工艺简单、成本低廉等优点,易于实现工业化生产。(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.)

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, 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.

2. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: the molar ratio of potassium sodium tartrate to manganese chloride in the manganese tartrate precipitation solution obtained in the step 3) is 1: 1.

3. 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.

4. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: 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.

5. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: regulating the volume of the reaction material in the inner container of the reaction kettle in the step 7) by using distilled water to make the volume of the reaction material 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.

6. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: regulating the volume of the reaction material 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.

7. The method for preparing a manganese molybdate nanosheet crystal according to claim 1, wherein: mixing the potassium sodium tartrate aqueous solution and the manganese chloride aqueous solution, and then carrying out hydrothermal treatment to obtain a manganese tartrate precipitation solution as a reaction precursor.

8. 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.

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 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 means 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 understandable, the following preferred embodiments are described in detail 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 embodiments.