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Low BET ball-type manganic manganous oxide and its preparation method

A manganese tetroxide, spherical technology, used in manganese oxide/manganese hydroxide, chemical/physical/physical-chemical fixed reactors, thin material processing, etc. Lithium) materials, etc.

Active Publication Date: 2012-10-17
SHENZHEN MODERN SKY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Disclosed in CN1814551A by in MnSO 4 / H 2 Ammonia was added to the O solution to prepare Mn 3 o 4 method, although the oxidation rate of divalent manganese and the recovery rate of manganese have been greatly improved, but the pure phase of Mn cannot be guaranteed. 3 o 4 , while due to the unprepared Mn 3 o 4 Physical indicators such as particle size distribution and specific surface area are subject to research and technical control, and are not suitable for the preparation of LMO (lithium manganese oxide) materials

Method used

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  • Low BET ball-type manganic manganous oxide and its preparation method
  • Low BET ball-type manganic manganous oxide and its preparation method
  • Low BET ball-type manganic manganous oxide and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0086] (1) Pretreatment process of manganese sulfate solution

[0087] will be 100m 3 MnSO 4 Adjust the solution to a concentration of 130g / L, add MnS at a rate of 2.5 kg per cubic meter of solution, and stir and react at 90°C for 3 hours to convert heavy metal impurity ions in the solution into insoluble sulfides. After that, press Separate by filtration, discard the filter residue, adjust the pH of the filtrate to 2.5-3.0 by sulfuric acid, add 2.5L of 27.5% by weight hydrogen peroxide per cubic meter into hydrogen peroxide, maintain slight boiling for 50 minutes under stirring, and use 2mol / L Ba(OH) 2 Neutralize to pH 5.0, separate by pressure filtration, and discard the filter residue.

[0088] (2) Oxidation reaction process

[0089] Place the above filtrate at the bottom of the reactor 1, cool it to 25-26°C through the coil on the reactor 1, open the exhaust valve 2, and open the oxygen valve 10 and the ammonia valve 11 with O 2 -NH 3 After the air in the tower is rep...

Embodiment 2

[0093] (1) Pretreatment process of manganese sulfate solution

[0094] will be 100m 3 MnSO 4 Adjust the solution to a concentration of 170g / L, add MnS at a rate of 3.0 kg per cubic meter of solution, and stir and react at 95°C for 4 hours to convert heavy metal impurity ions in the solution into insoluble sulfides. After that, press Separate by filtration, discard the filter residue, adjust the pH of the filtrate to 2.5-3.0 by sulfuric acid, add hydrogen peroxide at 2.5L 27.5% by weight per cubic meter of hydrogen peroxide, maintain slight boiling for 60 minutes under stirring, and use 2mol / L Ba(OH) 2 Neutralize to pH 5.5, separate by pressure filtration, and discard the filter residue.

[0095] (2) Oxidation reaction process

[0096] Place the above-mentioned filtrate at the bottom of the reactor 1, cool it to 27-28°C through the coil on the reactor 1, open the exhaust valve 2, and open the oxygen valve 10 and the ammonia valve 11 with O 2 -NH 3 After the air in the towe...

Embodiment 3

[0100] (1) Pretreatment process of manganese sulfate solution

[0101] will be 100m 3 MnSO 4 The solution was adjusted to a concentration of 200g / L, and MnS was added at a rate of 2.8 kg per cubic meter of solution, and stirred and reacted at 93°C for 4 hours to convert heavy metal impurity ions in the solution into insoluble sulfides, and then press Separate by filtration, discard the filter residue, adjust the pH of the filtrate to 2.5-3.0 by sulfuric acid, add hydrogen peroxide at 2.5L 27.5% by weight per cubic meter of hydrogen peroxide, maintain slight boiling for 55 minutes under stirring, and use 2mol / L Ba(OH) 2 Neutralize to pH 5.3, separate by pressure filtration, and discard the filter residue.

[0102] (2) Oxidation reaction process

[0103] Place the above filtrate at the bottom of the reactor 1, cool it to 28-30°C through the coil on the reactor 1, open the exhaust valve 2, and open the oxygen valve 10 and the ammonia valve 11 with O 2 -NH 3 After the air in ...

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Abstract

The invention provides a low BET ball-type manganic manganous oxide and its preparation method. The preparation method of the present invention comprises: 1) a pretreatment process, adding MnS in a MnSO4 solution with concentration of 130-200g / L, removing the impurities of peroxides, then neutralizing, performing solid-liquid separation to obtain a manganese sulfate filtrate; 2) an oxidation reaction process, placing the filtrate in a reactor, keeping the temperature at 25-30 DEG C, performing spraying interface reaction in 500-1000mm of H2O on a mixed gas of oxygen and ammonia gas through spraying by a spray head, wherein the reaction is stopped until [Mn<2+>] is less than or equal to 1.5g / L, and the mole ratio of O2 and NH3 of gas is 1: 12; and 3) a finished product process, performing a solid-liquid separation on the solution after finishing the reaction, washing the solid and drying to obtain the Mn3O4 product. According to the invention, manganic manganous oxide has the advantages of narrow particle size distribution, pure phase and small impurity content, Mn% is 71.44-71.08wt%, the BET specific surface area is less than 1m<2> / g, D90 is 7.0-8.5mum, D10 is 2.6-3.2mum, D50 is 4.0-5.5mum and Dmax is 15.138mum.

Description

technical field [0001] The invention relates to a preparation method of low BET spherical trimanganese tetraoxide and the spherical trimanganese tetraoxide obtained by the method. Background technique [0002] The manganese tetraoxide raw materials commonly used in the preparation of manganese-based cathode materials for lithium-ion secondary batteries require small specific surface area, low impurity content, spherical particles, and pure crystal phase crystal structure. Improvement puts forward further requirements on the particle size distribution. [0003] Disclosed in CN1814551A by in MnSO 4 / H 2 Ammonia was added to the O solution to prepare Mn 3 o 4 method, although the oxidation rate of divalent manganese and the recovery rate of manganese have been greatly improved, but the pure phase of Mn cannot be guaranteed. 3 o 4 , while due to the unprepared Mn 3 o 4 Physical indicators such as particle size distribution and specific surface area are subject to researc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02
CPCC01P2002/72C01P2004/51C01G45/02Y10T428/2982B01J19/24
Inventor 吴筱菁
Owner SHENZHEN MODERN SKY TECH CO LTD
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