A Mn2Mo3O8 nanotube and its preparation method

Abstract

The present invention discloses Mn2Mo3O8 nanotubes and a preparation method thereof, which pertains to the field of secondary battery micro-nanomaterial synthesis. Using inexpensive manganese and molybdenum sources as reaction materials, the Mn2Mo3O8 nanotubes are prepared using a simple microwave method combined with calcination. The disclosed method features readily available raw materials, a simple process, low cost, suitability for mass production, and broad application prospects. The prepared Mn2Mo3O8 nanotubes exhibit distinct morphological characteristics and good crystallinity, and have broad application prospects in catalysis, sensing, and as secondary battery electrode materials.

Description

Technical Field

[0001] The present invention belongs to the technical field of secondary battery micro-nano materials, and in particular relates to a Mn2Mo3O8 nanotube and a preparation method thereof. Background Art

[0002] As an important inorganic nanomaterial, molybdate nanomaterials have promising application prospects in energy storage, catalysis, metallurgy, optoelectronics, and other fields. In order to further improve the comprehensive performance of molybdate nanomaterials, nanostructure design and regulation are of great significance.

[0003] Manganese molybdate is an important class of molybdate nanomaterials. Its unique crystal structure and variable valence of molybdenum and manganese elements give it excellent photoelectric, magnetic, catalytic, and electrochemical properties. Consequently, manganese molybdate is widely used in photoelectrocatalysis, luminescence, humidity detectors, sensors, and electrochemical energy storage materials. It is a key inorganic functional material in the chemical, defense, and electronics industries.

[0004] There are also numerous reports on the preparation of manganese molybdate micro-nanomaterials and their composite materials. For example, Chinese patent CN201110048928.3 discloses the preparation of manganese molybdate-cobalt molybdate hierarchical heterostructure nanowires using a microemulsion method. CTAB is used as a surfactant during the preparation process. The preparation method is complex and costly, making it unsuitable for large-scale production. Chinese patent CN201210012024.X discloses a method for preparing manganese molybdate microcrystals. The product prepared by this method has a dispersed structure, is relatively large in size, and has poor uniformity. Mn2Mo3O8 is a type of hexagonal manganese molybdate compound with important application prospects in photoelectrocatalysis, sensors, and electrochemical energy storage materials. However, there are relatively few reports on this type of molybdate. Summary of the Invention

[0005] In order to overcome the shortcomings of the above-mentioned prior art, the purpose of the present invention is to provide a Mn2Mo3O8 nanotube and a preparation method thereof, so as to solve the technical problems of the existing preparation method, such as complex steps, high cost, unsuitability for large-scale production, and the obtained product having a dispersed structure and poor uniformity.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] The present invention discloses a method for preparing Mn2Mo3O8 nanotubes, comprising the following steps:

[0008] S1: dissolving sodium molybdate, tannic acid, tromethamine and manganese acetate tetrahydrate in deionized water to obtain a mixed solution A;

[0009] S2: reacting the mixed solution A under microwave conditions to obtain a precipitate; filtering, washing, and drying the obtained precipitate in sequence to obtain product B;

[0010] S3: calcining the product B to obtain Mn2Mo3O8 nanotubes.

[0011] Furthermore, in S1, the ratio of sodium molybdate, tannic acid, tromethamine, manganese acetate tetrahydrate and deionized water is 1:(0.5-1):(0.3-0.5):(1-2):50 in parts by mass.

[0012] Furthermore, in S2, the mixed solution A is stirred at room temperature and pressure for 1 to 3 hours before reacting under microwave conditions.

[0013] Furthermore, in S2, the reaction time under the microwave condition is 5 to 10 minutes.

[0014] Furthermore, in S2, the power of the microwave generator used for the reaction under the microwave condition is 100-200W.

[0015] Furthermore, in S2, the water washing is performed 3 to 6 times.

[0016] Furthermore, in S2, the drying temperature is 50-70°C and the drying time is 6-10 hours.

[0017] Furthermore, in S3, the calcination temperature is 400-600° C. and the calcination time is 1-3 hours.

[0018] The invention also discloses a Mn2Mo3O8 nanotube prepared by the preparation method.

[0019] Furthermore, the Mn2Mo3O8 nanotubes have a tubular structure.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The present invention discloses a method for preparing Mn2Mo3O8 nanotubes. Using inexpensive sodium molybdate and manganese acetate tetrahydrate as molybdenum and manganese sources, the method achieves the first self-assembly of Mn2Mo3O8 nanoparticles into unique Mn2Mo3O8 nanotubes by adjusting process parameters such as microwaves and calcination. The addition of tannic acid and tromethamine aids the formation of the unique morphology of the Mn2Mo3O8 nanotubes. After proper calcination, the product further enhances its purity and crystallinity. The preparation method is simple, easy to operate, low-cost, environmentally friendly, and suitable for industrial-scale production.

[0022] The present invention also discloses Mn2Mo3O8 nanotubes prepared by the above preparation method. The nanotubes prepared by the method have the characteristics of distinct morphology, high purity, high crystallinity, large specific surface area, good uniformity, etc., and have broad application prospects in the fields of photocatalytic materials, luminescent materials, sensing, new energy, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 XRD pattern of the Mn2Mo3O8 nanotubes prepared in the present invention;

[0024] Figure 2 This is a transmission electron microscope image of the Mn2Mo3O8 nanotubes prepared in the present invention;

[0025] Figure 3 This is the charge and discharge curve of the Mn2Mo3O8 nanotubes prepared in the present invention. DETAILED DESCRIPTION

[0026] To facilitate understanding of the features and effects of the present invention by those skilled in the art, the following provides a general description and definition of the terms and expressions used in the specification and claims. Unless otherwise indicated, all technical and scientific terms used herein have the ordinary meanings as understood by those skilled in the art regarding the present invention. In the event of conflict, the definitions in this specification shall prevail.

[0027] The theories or mechanisms described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, that is, the present invention can be implemented without being limited by any specific theory or mechanism.

[0028] Herein, all features such as values, amounts, amounts, and concentrations defined in numerical ranges or percentage ranges are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to include and specifically disclose all possible subranges and individual values ​​within the range (including integers and fractions).

[0029] In this document, unless otherwise specified, “include,” “including,” “contains,” “has” or similar terms cover the meanings of “consisting of” and “mainly consisting of,” for example, “A includes a” covers the meanings of “A includes a and other” and “A only includes a.”

[0030] In this document, for the sake of brevity, not all possible combinations of the various technical features in each embodiment or example are described. Therefore, as long as there are no contradictions in the combination of these technical features, the various technical features in each embodiment or example can be combined in any way, and all possible combinations should be considered to be within the scope of this specification.

[0031] Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiments are only used to illustrate the present invention and are not used in limiting the scope of the present invention.In addition, should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall equally within the scope limited by the appended claims of the application.

[0032] The following examples were prepared using conventional instruments and equipment in the art. Experimental methods in the following examples, where specific conditions are not specified, were generally performed under conventional conditions or according to the conditions recommended by the manufacturer. The various raw materials used in the following examples, unless otherwise specified, were conventional commercially available products, with specifications conventional in the art. In the present specification and the following examples, unless otherwise specified, "%" indicates percentage by weight, "part" indicates parts by weight, and "ratio" indicates weight ratio.

[0033] Example 1

[0034] A method for preparing Mn2Mo3O8 nanotubes comprises the following steps:

[0035] S1: Dissolve 1 part of sodium molybdate, 0.5 parts of tannic acid, 0.3 parts of tromethamine, and 1 part of manganese acetate tetrahydrate in 50 parts of deionized water to obtain a mixed solution A.

[0036] S2: Stir the mixed solution A at room temperature and pressure for 3 h, transfer it to a microwave generator, and react it at a microwave power of 100 W for 10 min to obtain a precipitate; the obtained precipitate is filtered, washed with water 5 times, and dried at 50°C for 8 h to obtain product B;

[0037] S3: calcining product B at 600°C in a muffle furnace for 1 h to obtain Mn2Mo3O8 nanotubes.

[0038] See also Figure 1 , Figure 1 The XRD pattern of the Mn2Mo3O8 nanotubes prepared in this invention is as follows: Figure 1 The phase composition of Mn2Mo3O8 nanotubes can be determined, and they have high purity.

[0039] See also Figure 2 , Figure 2 The transmission electron microscope image of the Mn2Mo3O8 nanotubes prepared in the present invention shows that the prepared product has distinct morphological characteristics and is a nanotube-like structure.

[0040] See also Figure 3 , Figure 3This is the charge and discharge curve of the Mn2Mo3O8 nanotubes prepared by the present invention. As the negative electrode material of sodium ion batteries, the first discharge and charge specific capacities of this product can reach 287 and 161 mAh g, respectively. -1 .

[0041] Example 2

[0042] A method for preparing Mn2Mo3O8 nanotubes comprises the following steps:

[0043] S1: Dissolve 1 part of sodium molybdate, 1 part of tannic acid, 0.5 parts of tromethamine, and 2 parts of manganese acetate tetrahydrate in 50 parts of deionized water to obtain a mixed solution A.

[0044] S2: Stir the mixed solution A at room temperature and pressure for 1 hour, transfer it to a microwave generator, and react it at a microwave power of 200 W for 5 minutes to obtain a precipitate; the obtained precipitate is filtered, washed with water 6 times, and dried at 70°C for 6 hours to obtain product B;

[0045] S3: calcining product B at 4000°C in a muffle furnace for 3 h to obtain Mn2Mo3O8 nanotubes.

[0046] Example 3

[0047] A method for preparing Mn2Mo3O8 nanotubes comprises the following steps:

[0048] S1: Dissolve 1 part of sodium molybdate, 0.6 parts of monotannic acid, 0.4 parts of tromethamine, and 1 part of manganese acetate tetrahydrate in 50 parts of deionized water to obtain a mixed solution A.

[0049] S2: The mixed solution A was stirred at room temperature and pressure for 2 h, transferred to a microwave generator, and reacted at a microwave power of 200 W for 8 min to obtain a precipitate; the obtained precipitate was filtered, washed with water three times, and dried at 50°C for 10 h to obtain product B;

[0050] S3: calcining product B at 500°C in a muffle furnace for 2 h to obtain Mn2Mo3O8 nanotubes.

[0051] Example 4

[0052] A method for preparing Mn2Mo3O8 nanotubes comprises the following steps:

[0053] S1: Dissolve 1 part of sodium molybdate, 0.7 parts of monotannic acid, 0.3 parts of tromethamine, and 1 part of manganese acetate tetrahydrate in 50 parts of deionized water to obtain a mixed solution A.

[0054] S2: Stir the mixed solution A at room temperature and pressure for 3 h, transfer it to a microwave generator, and react it at a microwave power of 200 W for 5 min to obtain a precipitate; the obtained precipitate is filtered, washed with water three times, and dried at 50°C for 10 h to obtain product B;

[0055] S3: calcining product B at 600°C in a muffle furnace for 1 h to obtain Mn2Mo3O8 nanotubes.

[0056] The above content is only for explaining the technical idea of ​​the present invention and cannot be used to limit the protection scope of the present invention. Any changes made on the basis of the technical solution in accordance with the technical idea proposed by the present invention shall fall within the protection scope of the claims of the present invention.

Claims

1. A method for preparing Mn2Mo3O8 nanotubes, characterized in that: The following steps are involved: S1: dissolving sodium molybdate, tannic acid, tromethamine and manganese acetate tetrahydrate in deionized water to obtain a mixed solution A; S2: reacting the mixed solution A under microwave conditions to obtain a precipitate; filtering, washing, and drying the obtained precipitate in sequence to obtain product B; S3: calcining the product B to obtain Mn2Mo3O8 nanotubes; In S2, the reaction time under the microwave condition is 5 to 10 minutes; the power of the microwave generator used for the reaction under the microwave condition is 100 to 200 W; In S3, the calcination temperature is 400-600° C. and the calcination time is 1-3 hours.

2. The method for preparing Mn2Mo3O8 nanotubes according to claim 1, characterized in that: In S1, the usage ratio of the sodium molybdate, tannic acid, tromethamine, manganese acetate tetrahydrate and deionized water is 1:(0.5-1):(0.3-0.5):(1-2):50, calculated by mass.

3. The method for preparing Mn2Mo3O8 nanotubes according to claim 1, characterized in that: In S2, the mixed solution A is stirred at room temperature and pressure for 1 to 3 hours before reacting under microwave conditions.

4. The method for preparing Mn2Mo3O8 nanotubes according to claim 1, characterized in that: In S2, the water washing is 3 to 6 times.

5. The method for preparing Mn2Mo3O8 nanotubes according to claim 1, characterized in that: In S2, the drying temperature is 50-70° C. and the drying time is 6-10 hours.

6. A Mn2Mo3O8 nanotube, characterized in that: The nanotubes are prepared by the method for preparing Mn2Mo3O8 nanotubes according to any one of claims 1 to 5.

7. The Mn2Mo3O8 nanotube according to claim 6, characterized in that: The Mn2Mo3O8 nanotubes have a tubular structure.

Images