Method for preparing nanometer manganese dioxide by microwave reflux method

A technology of nano-manganese dioxide and microwave heating, applied in the direction of manganese oxide/manganese hydroxide, nanotechnology, etc., can solve the problems of high cost, difficult large-scale preparation, complicated operation, etc., and achieve low cost, controllable product quality, The effect of simple process

Inactive Publication Date: 2012-06-20
INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, sealed reaction vessels are required, the operation is more compl

Method used

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  • Method for preparing nanometer manganese dioxide by microwave reflux method
  • Method for preparing nanometer manganese dioxide by microwave reflux method
  • Method for preparing nanometer manganese dioxide by microwave reflux method

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Experimental program
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Effect test

Embodiment 1

[0027] Take by weighing 2.7g potassium persulfate (analytical pure) and 1.69g manganese sulfate monohydrate (analytical pure) respectively, be dissolved in 150ml deionized water, the divalent manganese ion concentration is 0.067mol / L; The flask was then placed in the cavity of a microwave oven for heating, and the three-neck flask was connected with a condensation reflux device. The microwave power is 800W, the reaction temperature is 98°C, and the reaction time is 5min. During the reaction, a magnetic stirrer was used to stir. After the reaction, the reaction product was suction filtered, washed and dried. figure 1 and figure 2 It is the result of characterizing the product obtained in Example 1. in, figure 1 Curve a in the figure shows the XRD pattern of the product, which is very consistent with the spectral line of γ-phase manganese dioxide with structure in the JCPDS database, indicating that the product is γ-phase manganese dioxide. Such as figure 2 As shown, the...

Embodiment 2

[0029] Take by weighing 4.05g potassium persulfate (analytical pure) and 2.535g manganese sulfate monohydrate (analytical pure), be dissolved in 150ml deionized water, the divalent manganese ion concentration is 0.1mol / L; Transfer to a three-necked flask, and then place it in a microwave oven cavity for heating, and the three-necked flask is externally connected to a condensation reflux device. The microwave power is 850W, the reaction temperature is 100°C, and the reaction time is 10min. During the reaction, a magnetic stirrer was used to stir. After the reaction, the reaction product was suction filtered, washed and dried. figure 1 Curve b in the figure shows the XRD pattern of the product, which is very consistent with the spectral line of γ-phase manganese dioxide with structure in the JCPDS database, indicating that the product is γ-phase manganese dioxide.

Embodiment 3

[0031] Weigh 0.405g potassium persulfate (analytical pure) and 0.2535g manganese sulfate monohydrate (analytical pure) respectively, be dissolved in 150ml deionized water, the divalent manganese ion concentration is 0.01mol / L; Transfer to a three-necked flask, and then place it in a microwave oven cavity for heating, and the three-necked flask is externally connected to a condensation reflux device. The microwave power is 100W, the reaction temperature is 90°C, and the reaction time is 30min. During the reaction, a magnetic stirrer was used to stir. After the reaction, the reaction product was suction filtered, washed and dried. figure 1 Curve c in the figure shows the XRD pattern of the product, which is very consistent with the spectral line of γ-phase manganese dioxide with structure in the JCPDS database, indicating that the product is γ-phase manganese dioxide.

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Abstract

A method for preparing nanometer manganese dioxide by microwave heating reflux comprises the following steps: (1) preparing a reaction solution by soluble divalent manganese salt and soluble persulfate; (2) putting the reaction solution in a microwave oven with a microwave frequency of 2.45 GHz, a microwave power of 100-850 W, a reaction temperature of 90-100 DEG C and reaction time of 5-30 min; after the reaction, separating, washing and drying the product to obtain a gamma-MnO2 nano-material. In step (1), 1-5 mL concentrated sulfuric acid is added into the reaction solution of soluble divalent manganese salt and soluble persulfate, and the obtained reaction product is a sea urchin-shaped alpha-MnO2 micro-sphere. The manganese dioxide material prepared by the invention is applicable to the fields of super capacitor electrode materials, battery electrode materials, catalysts, and the like.

Description

technical field [0001] The invention relates to a method for preparing nano manganese dioxide, in particular to a method for preparing nano manganese dioxide with different crystal forms and shapes by microwave heating and reflux. Background technique [0002] Due to its rich and unique physical and chemical properties, manganese dioxide is widely used in ion sieves, molecular sieves, biosensors, catalysis, magnetic materials, and energy storage. Due to its environmental friendliness, simple preparation process, and cheap and easy-to-obtain raw materials, it has been used as an electrode material for lithium-ion batteries and supercapacitors in recent years. Manganese dioxide is an oxide with a relatively complex lattice structure, which has various crystal forms such as α, β, γ, and δ. Different crystal forms of manganese dioxide have the same structural unit: [MnO 6 ] octahedron. These [MnO 6 ] Octahedrons form tunnel-like or layered manganese dioxide crystalline compo...

Claims

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Application Information

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IPC IPC(8): C01G45/02B82Y40/00
Inventor 张熊马衍伟孙现众
Owner INST OF ELECTRICAL ENG CHINESE ACAD OF SCI
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