Preparation method for manganic manganous oxide

Abstract

The invention relates to a preparation method for manganic manganous oxide. The method is as follows: in an enclosed reaction container, a manganese source with an average valence of manganese being less than 8 / 3 is placed in a reaction solution, the reaction is carried out with heating, the situation is kept that the pressure or partial pressure of oxidizing gases in the reaction system is more than or equal to 1 standard atmospheric pressure, and a crude product of manganic manganous oxide can be prepared after the reaction is completed. Optionally, the enclosed reaction container has an oxidizing gas inlet or has an oxidizing gas inlet and a generation gas outlet simultaneously. The oxidation reaction rate is raised, the oxidation reaction time is shortened, the manganic manganous oxide crystal growth integrality is raised, the crystal defect is reduced, and high purity and high quality are obtained.

Description

technical field

[0001] The present invention belongs to the field of preparation of trimanganese tetraoxide, and in particular relates to a preparation method of trimanganese tetraoxide and trimanganese tetraoxide prepared therefrom. The preparation method of trimanganese tetraoxide can obviously shorten the reaction time and improve Manganese content, reduce the formation of impurities and improve the purity of manganese tetraoxide. Background technique

[0002] Manganese is one of the common variable-valence metal elements, and its oxide forms are manganese monoxide, trimanganese tetraoxide, manganese trioxide, and manganese dioxide. The primary structural units of manganese oxides are basically the same, all of which are manganese-oxygen octahedra; the secondary structural units are similar, and are connected by shared-edge manganese-oxygen octahedral chains or ribbon chains. Due to the variable valence of manganese (such as Mn 3+ and Mn 4+ Interconversion between) and...

Examples

Embodiment 1

[0087] Weigh 9.0g of manganese hydroxide solid and 200mL of pure water and mix to obtain a reaction solution, add it into a sealed reactor (the reaction process does not have any form of gas exchange with the external connection), adjust the gas phase pressure of the air in the sealed reactor to 3.2-3.4MPa , heating the reaction solution to 100°C for 0.5h to obtain the crude trimanganese tetraoxide;

[0088] The crude trimanganese tetraoxide is subjected to solid-liquid separation, washing and drying to obtain trimanganese tetraoxide powder.

[0089] figure 1 is the particle size and morphology of the crystals of trimanganese tetraoxide prepared in Example 1 of the present invention;

[0090] figure 2 is the crystal XRD pattern of trimanganese tetraoxide prepared in Example 1 of the present invention.

Embodiment 2

[0092] Weigh 7.0g of manganese monoxide solid and 100mL of pure water to mix to obtain the reaction solution, add it into a sealed reactor (the reaction process does not have any form of gas exchange with the external connection), and feed oxygen into the sealed reactor until the gas phase pressure of oxygen is 2.92 ~2.93MPa, raise the temperature of the slurry to 230°C and react for 0.1h to obtain the crude manganese tetraoxide;

[0093] The crude trimanganese tetraoxide is subjected to solid-liquid separation, washing and drying to obtain trimanganese tetraoxide powder.

Embodiment 3

[0095] Take by weighing manganese monoxide solid 7.0g and pure water 100mL and mix to obtain the reaction solution, add in the sealed reactor (the reaction process does not have any form of gas exchange with the external connection), feed air into the sealed reactor, so that the gas phase pressure is 50.0 Between ~52.0MPa, react the reaction liquid at 25°C for 1.0h to obtain the crude trimanganese tetraoxide;

[0096] The crude trimanganese tetraoxide is subjected to solid-liquid separation, washing and drying to obtain trimanganese tetraoxide powder.

technical field

[0001] The present invention belongs to the field of preparation of trimanganese tetraoxide, and in particular relates to a preparation method of trimanganese tetraoxide and trimanganese tetraoxide prepared therefrom. The preparation method of trimanganese tetraoxide can obviously shorten the reaction time and improve Manganese content, reduce the formation of impurities and improve the purity of manganese tetraoxide. Background technique

[0002] Manganese is one of the common variable-valence metal elements, and its oxide forms are manganese monoxide, trimanganese tetraoxide, manganese trioxide, and manganese dioxide. The primary structural units of manganese oxides are basically the same, all of which are manganese-oxygen octahedra; the secondary structural units are similar, and are connected by shared-edge manganese-oxygen octahedral chains or ribbon chains. Due to the variable valence of manganese (such as Mn 3+ and Mn 4+ Interconversion between) and...

Examples

Embodiment 1

[0087] Weigh 9.0g of manganese hydroxide solid and 200mL of pure water and mix to obtain a reaction solution, add it into a sealed reactor (the reaction process does not have any form of gas exchange with the external connection), adjust the gas phase pressure of the air in the sealed reactor to 3.2-3.4MPa , heating the reaction solution to 100°C for 0.5h to obtain the crude trimanganese tetraoxide;

[0088] The crude trimanganese tetraoxide is subjected to solid-liquid separation, washing and drying to obtain trimanganese tetraoxide powder.

[0089] figure 1 is the particle size and morphology of the crystals of trimanganese tetraoxide prepared in Example 1 of the present invention;

[0090] figure 2 is the crystal XRD pattern of trimanganese tetraoxide prepared in Example 1 of the present invention.

Embodiment 2

[0092] Weigh 7.0g of manganese monoxide solid and 100mL of pure water to mix to obtain the reaction solution, add it into a sealed reactor (the reaction process does not have any form of gas exchange with the external connection), and feed oxygen into the sealed reactor until the gas phase pressure of oxygen is 2.92 ~2.93MPa, raise the temperature of the slurry to 230°C and react for 0.1h to obtain the crude manganese tetraoxide;

[0093] The crude trimanganese tetraoxide is subjected to solid-liquid separation, washing and drying to obtain trimanganese tetraoxide powder.

Embodiment 3

[0095] Take by weighing manganese monoxide solid 7.0g and pure water 100mL and mix to obtain the reaction solution, add in the sealed reactor (the reaction process does not have any form of gas exchange with the external connection), feed air into the sealed reactor, so that the gas phase pressure is 50.0 Between ~52.0MPa, react the reaction liquid at 25°C for 1.0h to obtain the crude trimanganese tetraoxide;

[0096] The crude trimanganese tetraoxide is subjected to solid-liquid separation, washing and drying to obtain trimanganese tetraoxide powder.

Images