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Method for preparing trimanganese tetroxide with micro-nanostructure

A technology of trimanganese tetraoxide and micro-nano structure, which is applied in the direction of manganese oxide/manganese hydroxide, etc., can solve the problem of low specific surface area of ​​trimanganese tetraoxide, and achieve the effects of low pollution, simple process and convenient operation

Active Publication Date: 2017-01-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In order to solve the existing defects such as low specific surface area of ​​trimanganese tetraoxide and easy introduction of impurities such as surfactants and sulfates in the preparation process, the present invention provides a preparation method of trimanganese tetraoxide with micro-nano structure, aiming at improving the The specific surface area of ​​the manganese manganese tetraoxide obtained improves the product purity

Method used

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  • Method for preparing trimanganese tetroxide with micro-nanostructure
  • Method for preparing trimanganese tetroxide with micro-nanostructure
  • Method for preparing trimanganese tetroxide with micro-nanostructure

Examples

Experimental program
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Effect test

Embodiment 1

[0067] Add 1 part of manganese powder to 200 parts of ethanol at 40°C, add 1.4 parts of ammonium acetate catalyst, add 10 parts of distilled water and stir for 12 hours, adjust the pH to 7-9, and stir with air for 5 hours: centrifuge, wash, dry, grind After getting the product. The yield of trimanganese tetraoxide obtained was 99%.

[0068] The product has been tested and the specific surface area of ​​the manganese tetraoxide product is 103.3m 2 / g, Mn element content 71.30%, CaO content 0.0008%, K content 0.0007%, Na content 0.0025%, S content 0.0050%. The scanning electron microscope and transmission electron microscope photos of the product are shown in Figure 2. It can be seen from Figure 2 (a), (b) and (c) that the trimanganese tetraoxide product is a hollow dumbbell structure, and Figure 2 (d) can be seen that the product is made of 10 ~ 15nm grain composition. XRD spectrum and Mn of trimanganese tetraoxide 3 o 4 The standard diffraction pattern of Figure 5 shown...

Embodiment 2

[0070] Add 5 parts of manganese powder to 180 parts of ethanol at 80~~85°C, add 8 parts of ammonium acetate catalyst, add 30 parts of distilled water and stir for 9 hours, adjust the pH to 7~9, and stir with air for 5 hours; centrifuge, wash, and dry The product is obtained after drying and grinding. The yield of trimanganese tetraoxide obtained was 99%.

[0071] The product has been tested and the specific surface area of ​​the manganese tetraoxide product is 84.5m 2 / g, Mn element content 70.50%, CaO content 0.0010%, K content 0.0006%, Na content 0.0020%, S content 0.0070%. The transmission electron microscope photos of the products are shown in image 3 ,Depend on image 3 It can be seen that the product is a nano hollow tube structure.

Embodiment 3

[0073] Add 10 parts of manganese powder to 150 parts of ethanol at 80-85°C, add 10 parts of ammonium acetate catalyst, add 60 parts of distilled water and stir for 10 hours, adjust the pH to 7-9, and stir with air for 2-6 hours; centrifuge, wash, The product is obtained after drying and grinding. The yield of trimanganese tetraoxide obtained was 99%.

[0074] The product has been tested and the specific surface area of ​​the manganese tetraoxide product is 72.8m 2 / g, Mn element content 70.80%, CaO content 0.0015%, K content 0.0005%, Na content 0.0025%, S content 0.0080%. Scanning electron microscope and transmission electron microscope photos see Figure 4 ,Depend on Figure 4 (a), (b) it can be seen that the product is a folded nanosheet, by Figure 4 (c) and (d), it can be seen that the product is composed of crystal grains of 10-15nm. XRD spectrum and Mn of trimanganese tetraoxide 3 o 4 The standard diffraction pattern of Figure 6 shown.

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Abstract

The invention discloses a method for preparing trimanganese tetroxide with a micro-nanostructure. The method comprises the steps: adding a manganese powder to an alcohol-water mixed solution, taking an ammonium salt as a catalyst, heating to 40-115 DEG C, and carrying out a stirring reaction for a period of time to obtain white manganese hydroxide; and then introducing air to a manganese hydroxide solution for 2-10 h, washing and drying, and grinding to obtain the trimanganese tetroxide product with the micro-nanostructure. The reaction is carried out at low temperature and ordinary pressure, the preparation process is simple, and the cost is low. The prepared trimanganese tetroxide product has relatively high specific surface area.

Description

[0001] Technical field: [0002] The invention relates to the field of preparation of trimanganese tetraoxide, in particular to a preparation method of trimanganese tetraoxide with a high specific surface area. [0003] technical background: [0004] Trimanganese tetraoxide is a high-performance material, which is widely used in electronics, batteries, food, paint and catalyst industries. Among them, as an important raw material for the production of soft ferrite and lithium manganese oxide batteries, trimanganese tetroxide is in great demand in the international and domestic markets. It is a high-tech material product encouraged by my country and has high commercial value. [0005] The general industrial production methods of manganese tetraoxide include manganese powder method and manganese sulfate method. Chinese patents CN 1935673, CN103466720, and CN 101898797 all use the manganese sulfate method to prepare trimanganese tetroxide. The steps are: remove impurities with man...

Claims

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Application Information

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IPC IPC(8): C01G45/02
CPCC01G45/02C01P2002/72C01P2004/03C01P2004/04C01P2004/13C01P2004/32C01P2004/61C01P2004/62C01P2006/12C01P2006/80
Inventor 钟宏江占王帅蒋崇文
Owner CENT SOUTH UNIV
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