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A kind of preparation method of trimanganese tetraoxide

A technology of manganese tetroxide and equipment, applied in manganese oxide/manganese hydroxide and other directions, can solve the problems of complicated operation, low temperature and energy consumption, low production cost, etc., and achieves lower reaction temperature, easy process control, and reaction process. thorough effect

Inactive Publication Date: 2015-12-09
湖南隆泰环保能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to this patent, high-valent manganese oxides such as manganese dioxide, manganese trioxide and similar high-valent oxides of manganese are heated in the presence of methane gas in the kiln, and the temperature is limited to 250-550 ° C to prevent the The generated trimanganese tetroxide is further reduced to manganese monoxide. The advantages of this method are simpler than the corresponding wet process, and the impurity content is less. Compared with the high temperature fire method, the temperature and energy consumption are low, but it requires high-priced manganese oxide and Methane is a reactant, high cost, low economic benefit, and poor crystallization performance at low temperature
[0005] 2. Oxidation method: as the publication number CN101177304A, the publication date is the Chinese invention patent on May 14, 2008. In this patent, manganese carbonate is used as raw material at 120-800°C, and manganese carbonate is decomposed by thermal oxidation with air or oxygen into A mixture of manganese dioxide, manganese monoxide and manganese carbonate, etc., and then roast the mixture of manganese at 800-1200°C to form manganese tetraoxide; and this method is divided into two steps, with high energy consumption, and it is difficult to avoid sintering occurrence, the specific surface area and activity of the product are low
[0007]The maximum temperature of this method is controlled at 1100°C, which requires strict atmosphere and complex operation, which is not easy to realize in practical industrialization
[0008] 3. Wet method: such as the Chinese invention patent with publication number CN101948138A, whose publication date is January 19, 2011. This patent belongs to hydrometallurgy. Alkaline substances are used to adjust the pH value of manganese sulfate to easily convert the manganese sulfate It is easy to obtain manganese hydroxide; add ionic liquid, carry out microwave-assisted heating under the condition of being exposed to air, oxidize manganese hydroxide to trimanganese tetraoxide, obtain brown-red trimanganese tetraoxide solid after filtering, washing and drying. The method has low energy consumption and low production cost, but the process is too complicated and the specific surface area is not stable

Method used

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  • A kind of preparation method of trimanganese tetraoxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment one: get the manganese carbonate (its water content is 5%) of 500kg and mix evenly with the starch (carbon source) of 50kg, then it is put into continuous microwave steel belt kiln and carry out microwave heating, control its heating rate to be 10 ℃ / min, and the temperature is controlled at 700°C for sintering, and the holding time of sintering is controlled for about 60 minutes. After cooling, trimanganese tetraoxide is obtained, and then the trimanganese tetraoxide is wet-milled to 1000 mesh, and obtained through testing. The manganese content of the product is 71.3%, the unit energy consumption is 4500 degrees / ton, and the specific surface area is 7.8m 2 / g, and it is pure trimanganese tetraoxide after XRD analysis.

[0018] In the HG / T2835-1997 standard, the quality standard of trimanganese tetraoxide is stipulated, see the table below.

[0019] Indicator name Superior product First grade Qualified product Manganese content%≥ 71 70 ...

Embodiment 2

[0023] Embodiment two: get the manganese carbonate of 1kg (its water content is 5%) and the starch (carbon source) of 0.1kg is evenly mixed, then it is put into batch type microwave test furnace and carries out microwave heating, controls its heating rate to be 20 ℃ / min, and the temperature is controlled at 700°C, the holding time of sintering is controlled for about 60 minutes, and then trimanganese tetraoxide is obtained after cooling, and then the trimanganese tetraoxide is wet-milled to 1000 mesh, and the product manganese is obtained after testing The content is 71.5%, the unit energy consumption is 5000 degrees / ton, and the specific surface area is 7.5m 2 / g, and it is pure trimanganese tetraoxide by XRD analysis, and its specific indicators are shown in the table below.

[0024] Indicator name Trimanganese tetraoxide Manganese content% 71.5 Silica% 0.009 Potassium content% 0.002 Sodium content% 0.005 Calcium content% 0.002 M...

Embodiment 3

[0026] Embodiment three: the manganese carbonate (its water content is 5%) that gets 500kg is evenly mixed with the glucose (carbon source) of 40kg, then it is put into the continuous type microwave steel strip kiln and carries out microwave heating, controls its heating rate to be 10 ℃ / min, and the temperature is controlled at 650°C, and the sintering holding time is controlled for about 120 minutes, and then the manganese tetraoxide is obtained after cooling, and then the manganese tetraoxide is wet-milled to 1000 mesh, and the product manganese is obtained after testing The content is 71.2%, the unit energy consumption is 4600 degrees / ton, and the specific surface area is 7.8m 2 / g, and it is pure trimanganese tetraoxide by XRD analysis, and its specific indicators are shown in the table below.

[0027] Indicator name Trimanganese tetraoxide Manganese content% 71.2 Silica% 0.009 Potassium content% 0.002 Sodium content% 0.005 Calcium c...

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Abstract

The invention discloses a method for preparing trimanganese tetroxide. Manganese carbonate is used as a raw material, added with a carbon source, placed in sealed microwave equipment, then heated to 650-750 DEG C with a heating rate of 8-20 DEG C / min, and sintered for 0.5-2 h; and the product is ground by a wet grinding after tapping, so as to obtain trimanganese tetroxide. According to the present invention, rapid and comprehensive heating of the microwave equipment and ''non-thermal effect'' enable carbon dioxide generated from decomposition of manganese carbonate to timely react with manganese oxide at a low temperature, so as to produce trimanganese tetroxide; and the method has the advantages of simple process, easy control process, low energy consumption, complete reaction process and stable specific surface area.

Description

technical field [0001] The invention relates to the technical field of inorganic non-metallic materials, in particular to a preparation method of trimanganese tetraoxide. Background technique [0002] Trimanganese tetraoxide is one of the important raw materials for the preparation of soft magnetic materials such as manganese zinc ferrite. Since soft magnetic materials are widely used in the electronics industry, the preparation of high-quality trimanganese tetraoxide has been approved by the National Development and Planning Commission It is listed as a current high-tech industrialization project by the Ministry of Science and Technology, and is a high-tech product encouraged by the state to optimize its development. [0003] At present, the methods for preparing trimanganese tetraoxide in the prior art generally include the following types. [0004] 1. Reduction method: under the preparation method of trimanganese tetraoxide introduced in US Patent No. 4411878, the oxides...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/02
Inventor 王雄张晓东杨军陈斌王哲
Owner 湖南隆泰环保能源科技有限公司
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