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Coralline porous delta-MnO2 and preparation method thereof

A coral-like, mixed solution technology, applied in the direction of manganese oxide/manganese hydroxide, etc., can solve the problems of long process flow, powder agglomeration, large product loss, etc., and achieve the effect of simple process, complete development and process control

Inactive Publication Date: 2017-01-11
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the liquid-phase precipitation method must be separated from the liquid-solid to obtain the precipitate, because SO 4 2- or Cl - The introduction of a large number of inorganic ions, such as, need to be washed repeatedly to remove these ions. There are disadvantages such as long process flow, large waste liquid, and large product loss. It is difficult to completely clean the inorganic ions. Therefore, the prepared MnO 2 The purity of the powder is not high; there are many reaction factors to be regulated in the sol-gel method, including the concentration of the precursor solution, pH value, calcination temperature, calcination time, etc., so the synthesized MnO 2 The crystal form and morphology of the powder are difficult to control, and the calcination process is easy to cause the agglomeration of the powder; the powder obtained by the solid-state reaction method is easy to agglomerate, and the shape is difficult to control

Method used

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  • Coralline porous delta-MnO2 and preparation method thereof
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  • Coralline porous delta-MnO2 and preparation method thereof

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Effect test

Embodiment 1

[0024] Coral-like porous δ-MnO 2 The preparation method comprises the following steps:

[0025] Step 1. Put 8×10 -4 mol KMnO 4 Add 20 mL of deionized water and stir to obtain a homogeneous solution;

[0026] Step 2. Put 2×10 -4 mol MnSO 4 Add 20 mL of deionized water and stir to obtain a homogeneous solution, which is mixed with the KMnO obtained in step 1 4 The solution is mixed evenly, in which KMnO 4 with MnSO 4 The molar ratio is 4:1;

[0027] Step 3, using 0.1M dilute hydrochloric acid to adjust the pH value of the mixed solution obtained in step 2 to 3.0;

[0028] Step 4, transfer the mixed solution whose pH value is 3.0 in step 3 to the autoclave, and the mixed solution volume is controlled at 70% of the reactor volume;

[0029] Step 5: After reacting at 140°C for 36 hours, cool down the temperature, wash the obtained product with distilled water to neutrality, then wash once with absolute ethanol, and finally dry it in an oven at 80°C to obtain coral-like poro...

Embodiment 2

[0031] Coral-like porous δ-MnO 2 The preparation method comprises the following steps:

[0032] Step 1. Put 1.2×10 -3 mol KMnO 4 Add 20 mL of deionized water and stir to obtain a homogeneous solution;

[0033] Step 2. Put 2×10 -4 mol MnSO 4 Add 20 mL of deionized water and stir to obtain a homogeneous solution, which is mixed with the KMnO obtained in step 1 4 The solution is mixed evenly, in which KMnO 4 with MnSO 4 The molar ratio is 6:1;

[0034] Step 3, using 0.1M dilute hydrochloric acid to adjust the pH value of the mixed solution obtained in step 2 to 4.0;

[0035] Step 4, transfer the mixed solution whose pH value is 4.0 in step 3 to the autoclave, and the volume of the mixed solution is controlled at 65% of the reactor volume;

[0036] Step 5. After reacting at 160°C for 24 hours, cool down the temperature, wash the obtained product with distilled water to neutrality, then wash once with absolute ethanol, and finally dry it in an oven at 80°C to obtain coral-...

Embodiment 3

[0038] Coral-like porous δ-MnO 2 The preparation method comprises the following steps:

[0039] Step 1. Put 1.6×10 -3 mol KMnO 4 Add 20 mL of deionized water and stir to obtain a homogeneous solution;

[0040] Step 2. Put 2×10 -4 mol MnSO 4 Add 20 mL of deionized water and stir to obtain a homogeneous solution, which is mixed with the KMnO obtained in step 1 4 The solution is mixed evenly, in which KMnO 4 with MnSO 4 The molar ratio is 8:1;

[0041] Step 3, using 0.1M dilute hydrochloric acid to adjust the pH value of the mixed solution obtained in step 2 to 5.0;

[0042] Step 4, transfer the mixed solution whose pH value is 5.0 in the step 3 to the autoclave, and the volume of the mixed solution is controlled at 60% of the reactor volume;

[0043] Step 5. After the reaction kettle was reacted at 180°C for 12 hours, the temperature was cooled, and the obtained product was washed with distilled water to neutrality and then washed once with absolute ethanol, and finally...

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Abstract

The invention relates to a preparation method of MnO2, in particular to coralline porous delta-MnO2 and a preparation method thereof. The preparation method includes the following steps that KMnO4 is added into deionized water, and the materials are stirred to be uniform; MnSO4 is added into deionized water, the materials are stirred to be uniform, and the two solutions are mixed to be uniform; the pH value of the mixed solution is adjusted with diluted hydrochloric acid; the mixed solution with the pH value adjusted is transferred into a high-pressure reaction still; after the reaction of the high-pressure reaction still, cooling is carried out, the obtained product is washed with distilled water to be neutral and then washed with absolute ethyl alcohol, the product is dried through an oven, and coralline porous delta-MnO2 powder is obtained. The preparation method is achieved through a hydrothermal method, no high-temperature calcination is needed by the hydrothermal method, the superfine powder material without clusters or with fewer clusters and with complete crystallization and controllable shapes can be prepared, the process is simple, efficiency is high, and the course is controllable; in addition, the obtained product is complete in crystal phase development and high in purity.

Description

technical field [0001] The present invention relates to MnO 2 The preparation method of, especially relates to a coral-like porous δ-MnO 2 and its preparation method. Background technique [0002] MnO 2 There are many different types of crystal structures, which are represented by [MnO 6 ] octahedron as the basis, O atoms are distributed on the corners of the octahedron, and Mn atoms are located in the center of the octahedron. The vertices, edges or faces of these octahedra are connected in different forms to form different crystal forms. Common crystal forms include α, β, γ, λ, and δ crystal forms. MnO 2 The synthesis cost is low, the performance is stable, and it is non-polluting to the environment. It is currently receiving high attention in the fields of supercapacitors, lithium-ion batteries, and photocatalysis. [0003] MnO 2 The preparation methods of powder mainly include liquid phase precipitation method, sol-gel method, solid phase reaction method and so on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02
CPCC01G45/02C01P2002/72C01P2004/03
Inventor 夏傲刘宗怀
Owner SHAANXI NORMAL UNIV
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