Method for preparing three-dimensional microporous structure spinel cobalt manganese binary oxide

A technology of binary oxides and three-dimensional macropores, applied in cobalt compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of low yield and inconvenient mass production, and achieve high specific surface area, low environmental pollution, and solvent-free The effect of recycling

Active Publication Date: 2019-01-11
UNIVERSITY OF CHINESE ACADEMY OF SCIENCES
2 Cites 4 Cited by

AI-Extracted Technical Summary

Problems solved by technology

The main problem is that the output is low, it is not conveni...
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Abstract

The invention relates to a method for preparing spinel manganese binary oxide with a spatial three-dimensional microporous structure, and belongs to the technical field of inorganic chemistry. The method is simple in synthesizing process, an organic precursor is prepared under a low-temperature liquid-phase stirring condition, and the spinel cobalt manganese binary oxide material with a spatial three-dimensional microporous structure can be prepared by strictly controlling the calcining temperature, heating speed and sintering during heating. The product has high purity, good chemical stability and excellent space structure. Compared with a conventional bulk cobalt manganese acid material, the cobalt-manganese binary oxide has the advantages of high specific surface area, uniform spatial duct distribution and maximized active site exposure. The raw materials used in the method are low in cost, easily available, small in environmental pollution, mild in reacting condition and easy to control, and lower alcohol can be recycled, so that industrial production can be easily realized, and no more protection is required in the producing process.

Application Domain

Material nanotechnologyCobalt compounds

Technology Topic

OxideLiquid phase +10

Image

  • Method for preparing three-dimensional microporous structure spinel cobalt manganese binary oxide
  • Method for preparing three-dimensional microporous structure spinel cobalt manganese binary oxide
  • Method for preparing three-dimensional microporous structure spinel cobalt manganese binary oxide

Examples

  • Experimental program(11)

Example Embodiment

[0019] The preparation method of the spinel cobalt manganese binary oxide with three-dimensional macroporous structure prepared by the method of the present invention comprises the following steps:
[0020] (1) Slowly preheat the low-carbon alcohol solvent to 30~60 ℃, add the mixed acetate whose mass is 0.5%~2% of the solvent mass to the warm alcohol at one time, and stir vigorously until the cobalt acetate and manganese acetate are all Dissolve to obtain a pink solution, continue to stir vigorously at constant temperature for 3 to 6 hours, slowly cool down to room temperature, and age for 24 to 48 hours to obtain a suspension;
[0021] (2) Centrifuge the suspension of the above-mentioned step (1), wash the precursor three times with the same solvent as the above-mentioned step (1), remove the residual cobalt acetate and manganese acetate, and place it in an 80-degree oven to dry for 12-24 minutes hours, the pink organic salt precursor is obtained, and the solvent is recovered and reused;
[0022] (3) grinding the dried precursor of the above step (2), passing through a 300-mesh sieve, and heating the precursor after grinding and sieving in flowing air at a heating rate of 0.1°C to 2.5°C/min The temperature is 270-350° C., calcined for 9-13 hours, and cooled to room temperature to obtain a spinel cobalt-manganese binary oxide material with a three-dimensional macroporous structure.
[0023] The low-carbon alcohol solvent in the above preparation method can be ethanol, n-propanol or n-butanol.
[0024] The mixed acetate in the above-mentioned preparation method is Co(Ac) 2 ·4H 2 O and Mn(Ac) 2 ·4H 2 A mixture of O, in which the molar ratio of cobalt ions to manganese ions is greater than 1.0.

Example Embodiment

[0026] Example 1:
[0027] (1) Preparation of organic cobalt salt precursor: 100 g of ethanol was slowly preheated to 40° C., 1 g of mixed acetate (the mixture was Co(Ac) 2 ·4H 2 O and Mn(Ac) 2 ·4H 2 O, wherein the molar ratio of cobalt and manganese is 2:1) add it to the warm alcohol at one time, stir vigorously until the cobalt acetate and manganese acetate are all dissolved to obtain a pink solution. After continuous vigorous stirring at constant temperature for 3 hours, the temperature was slowly lowered to room temperature and aged for 36 hours. The suspension was centrifuged, and the precursor was washed three times with ethanol to remove residual cobalt acetate and manganese acetate, and dried in an oven at 80 degrees for 24 hours to obtain a pink organic salt precursor. The solvent can be recycled and reused;
[0028] (2) The precursor is ground finely and passed through a 300-mesh sieve. At a heating rate of 0.5 °C/min, the temperature was raised to 270 °C in the air, calcined for 9 hours, and cooled to room temperature with the furnace to obtain a spinel cobalt-manganese binary oxide cathode catalyst with a three-dimensional macroporous structure.

Example Embodiment

[0029] Embodiment 2:
[0030] (1) Preparation of organic cobalt salt precursor: 100 g of ethanol was slowly preheated to 40° C., 1 g of mixed acetate (the mixture was Co(Ac) 2 ·4H 2 O and Mn(Ac) 2 ·4H 2 (O, wherein the molar ratio of cobalt and manganese is 3:1) is added to the warm alcohol at one time, and vigorously stirred until the cobalt acetate and manganese acetate are all dissolved to obtain a pink solution. After continuous vigorous stirring at constant temperature for 3 hours, the temperature was slowly lowered to room temperature and aged for 26 hours. The suspension was centrifuged, and the precursor was washed three times with ethanol to remove residual cobalt acetate and manganese acetate, and dried in an oven at 80 degrees for 24 hours to obtain a pink organic salt precursor. The solvent can be recycled and reused;
[0031] (2) The precursor is ground finely and passed through a 300-mesh sieve. At a heating rate of 0.5°C/min, the temperature was raised to 270°C in the air, calcined for 9 hours, and cooled to room temperature with the furnace to obtain a spinel cobalt manganese binary oxide material with a three-dimensional macroporous structure.
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Description & Claims & Application Information

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