Preparation method of crayon-shaped Mn3O4 microstructure and obtained product

A technology of microstructure and polyvinylpyrrolidone, applied in the direction of manganese oxide/manganese hydroxide, etc., can solve the problems of uneven product appearance, complicated process, and large energy consumption, and achieve uniform product appearance, strong controllability, good repeatability

Active Publication Date: 2018-01-09
UNIV OF JINAN
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Problems solved by technology

On the one hand, choosing conventional non-toxic chemical raw materials can not only reduce costs, but also avoid pollution and harm to the environment caused by potassium permanganate and other toxic reagents; on the other hand, the existing synthesis methods usually have large energy consumption, high Disadvantages such as complex process, uneven product appearance, poor repeatability, and low output need further improvement and innovative research

Method used

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  • Preparation method of crayon-shaped Mn3O4 microstructure and obtained product
  • Preparation method of crayon-shaped Mn3O4 microstructure and obtained product
  • Preparation method of crayon-shaped Mn3O4 microstructure and obtained product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1.1 Add 1.919 g of manganese chloride tetrahydrate, 1.979 g of sodium acetate trihydrate, 2.153 g of PVP and 3.610 g of EDTA-2Na into a mixed solvent of 20 mL of water, 4 mL of ethanolamine and 8 mL of glycerol and stir to clarification;

[0030] 1.2 Transfer the above solution to the reactor and react at 180 °C for 16 h;

[0031] 1.3 After the reaction, the product was obtained after centrifugation and washing.

[0032] The XRD pattern of the product is as figure 1 As shown, the XRD results are consistent with the standard XRD card (24-0734), proving that the crystal phase of the obtained product is Mn 3 o 4 Mutually. The SEM picture of the product is as follows figure 2 and 3 As shown, the obtained product has a regular appearance, a flat surface, a crayon-like structure, and no other appearance, specifically: the lower part of the crayon-like structure is a hexagonal prism, the hexagonal side length of the hexagonal prism bottom is 0.75-0.90 μm, and the edge ...

Embodiment 2

[0034] 2.1 Add 1.425 g of manganese chloride tetrahydrate, 1.029 g of sodium acetate trihydrate, 2.358 g of PVP and 1.474 g of EDTA-2Na into a mixed solvent of 20 mL of water, 6 mL of ethanolamine and 5 mL of glycerol and stir to clarification;

[0035] 2.2 Transfer the above solution to the reactor and react at 160 °C for 4 h;

[0036] 2.3 After the reaction, after centrifugation and washing, a single crayon-like Mn 3 o 4 Microstructure, specifically: the lower part of the crayon-shaped structure is a hexagonal prism, the hexagonal side length of the hexagonal prism bottom is 0.09-0.15 μm, and the edge length is 0.15-0.24 μm; the upper part of the crayon-shaped structure is a hexagonal platform, the hexagonal platform The edge length is 0.10-0.17 μm, and the side length of the top hexagon is 0.05-0.08 μm.

Embodiment 3

[0038] 3.1 Add 2.239 g of manganese chloride tetrahydrate, 3.002 g of sodium acetate trihydrate, 1.319 g of PVP and 6.106 g of EDTA-2Na into a mixed solvent of 20 mL of water, 2 mL of ethanolamine and 10 mL of glycerol and stir to clarification;

[0039] 3.2 Transfer the above solution to the reactor and react at 200 °C for 26 h;

[0040] 3.3 After the reaction, after centrifugation and washing, a single crayon-like Mn 3 o 4 Microstructure, specifically: the lower part of the crayon-shaped structure is a hexagonal prism, the hexagonal side length of the hexagonal prism bottom is 2.90-3.30 μm, and the edge length is 4.64-5.28 μm; the upper part of the crayon-shaped structure is a hexagonal platform, and the hexagonal platform The edge length is 3.19-3.63 μm, and the side length of the top hexagon is 1.45-1.65 μm.

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Abstract

The invention discloses a preparation method of a crayon-shaped Mn3O4 microstructure and an obtained product. The preparation method comprises the following steps of adding divalent manganese salt, sodium acetate, polyvinylpyrrolidone and disodium ethylenediaminetetraacetate into a mixed solvent including water, ethanolamine and glycerol, and stirring to obtain a transparent solution; heating thetransparent solution to carry out a solvothermal reaction; after the reaction, the product is centrifugally separated and washed to obtain the Mn3O4 microstructure. The raw materials used in the invention are all common chemicals and reagents in the market, which have the advantages of low price, simple synthesis process, and no need of high temperature and inert gas protection conditions and aresuitable for large-scale production. The crayon-shaped Mn3O4 obtained by the invention has the advantages of controllable microstructure, narrow size distribution range, high yield and good repeatability, and has potential application value in the fields of super capacitors, catalysis, sensing, lithium-ion batteries and the like.

Description

technical field [0001] The invention relates to a shape-controllable Mn 3 o 4 The preparation method of microscopic structure, be specifically related to a kind of simple and convenient crayon shape Mn 3 o 4 Preparation methods of microstructures and resulting products. Background technique [0002] Manganese oxide is an important class of functional materials and has broad application prospects in the fields of energy, catalysis, and optical detection. Among them, Mn 3 o 4 The design and regulation of micro-nano materials have been widely concerned by scholars at home and abroad, mainly because Mn 3 o 4 With excellent physical and chemical properties, it has great application prospects in supercapacitors, catalysis, sensing, lithium-ion batteries and many other aspects. [0003] Mn with different morphologies can be synthesized by using solvothermal method, pyrolysis method, precipitation method, vapor deposition method, etc. 3 o 4 Microstructures (such as spheric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02
Inventor 马谦陈迎李绘张进涛韩智峰褚姝姝王俊鹏车全德王刚杨萍
Owner UNIV OF JINAN
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