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Preparation method of cobalt manganese spinel microspheres

A technology of cobalt-manganese spinel and spinel, which is applied in chemical instruments and methods, cobalt compounds, and hydrocarbon production from carbon oxides, etc., can solve problems such as affecting catalytic efficiency, limiting contact area, and high conversion reaction, and achieve environmental protection Friendly, lower reaction temperature, high selectivity effect

Active Publication Date: 2018-07-10
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the temperature of the catalyst depends on a complex external concentrating device, the cost is high, and the conversion reaction requires a high temperature (above 1000 degrees), and there are still many problems in practical application.
[0003] The inventors have also used NiFe 2 o 4 Spinel studies thermocatalytic reduction of CO 2 conversion reaction (RSC Adv., 2016, 6, 83814), it was found that oxygen vacancies are an important factor affecting the thermal catalytic reaction, but the specific surface area of ​​the material is low, which limits the contact area with the reaction gas, thereby affecting the catalytic efficiency

Method used

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  • Preparation method of cobalt manganese spinel microspheres
  • Preparation method of cobalt manganese spinel microspheres
  • Preparation method of cobalt manganese spinel microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Measure 2.63g of manganese chloride and 0.35g of cobalt chloride and dissolve them in deionized water, measure 3.5g of ammonium bicarbonate as a pH adjuster, mix and stir the two for 10 minutes, and carry out water at 120°C. Heat pretreatment. After the reaction product is naturally cooled, it is centrifugally filtered, and the obtained precipitate is washed with deionized water and ethanol in turn, and then dried to obtain cobalt carbonate and manganese carbonate precursors;

[0025] (2) Calcining the precursor in a muffle furnace for 5 hours at a temperature of 500°C to obtain cobalt manganate spinel microspheres;

[0026] figure 1 It is the scanning electron microscope spectrum of the cobalt-manganese spinel microsphere synthesized in embodiment 1. The shape is spherical, figure 2 It is a TEM image. By calculating the d value of about 0.45nm, the crystal phase index represented by this particle corresponds to the XRD pattern, and the crystal plane is (1 11). ...

Embodiment 2

[0028] (1) Measure 1.75g ​​of manganese chloride and 1.4g of cobalt chloride and dissolve them in deionized water, measure 3.5g of ammonium bicarbonate as a pH regulator, mix and stir the two for 20 minutes, and carry out water at 100°C. Heat pretreatment. After the reaction product is naturally cooled, it is centrifugally filtered, and the resulting precipitate is washed with deionized water and ethanol successively, and then dried to obtain cobalt carbonate and manganese carbonate precursors;

[0029] (2) Calcining the precursor in a muffle furnace for 3 hours at a temperature of 600°C to obtain cobalt manganate spinel microspheres; image 3 It is the nitrogen adsorption-desorption curve of the cobalt-manganese spinel microsphere synthesized in embodiment 2, and the specific surface area of ​​sample S46 (m (cobalt): m (manganese)=4:6) is 48.17m 2 / g.

Embodiment 3

[0031] (1) Measure 0.29g of manganese chloride and 3.16g of cobalt chloride and dissolve them in deionized water, measure 3.5g of ammonium bicarbonate as a pH adjuster, mix and stir the two for 30 minutes, and carry out water at 150°C. Heat pretreatment. After the reaction product is naturally cooled, it is centrifugally filtered, and the obtained precipitate is washed with deionized water and ethanol in turn, and then dried to obtain cobalt carbonate and manganese carbonate precursors;

[0032] (2) Calcining the precursor in a muffle furnace for 0.5h at a temperature of 700°C to obtain cobalt manganate spinel microspheres; Figure 4 XRD pattern of the prepared manganese-cobalt spinel microspheres. Obvious diffraction peaks appeared at 18.20°, 29.35°, 31.25°, 36.36°, 38.87°, 44.78°, 59.01°, 60.67° and 65.18°, and the largest diffraction peak appeared at 36.36°. It can be attributed to the tetragonal crystal structure of Co3O4 (JCPDS file no.180408T), corresponding to (111), ...

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Abstract

The invention provides a preparation method of cobalt manganese spinel microspheres. The method comprises weighing manganese chloride and cobalt chloride, dissolving the manganese chloride and cobaltchloride in deionized water, weighing ammonium hydrogen carbonate as a pH adjuster, carrying out mixing through stirring, carrying out hydrothermal pretreatment at 100-150 DEG C, after the reaction product is naturally cooled, carrying out centrifugal filtration, orderly washing the precipitates through deionized water and ethanol, carrying out drying to obtain cobalt carbonate and manganese carbonate precursors, and calcining the cobalt carbonate and manganese carbonate precursors through a muffle furnace at a temperature of 500 to 700 DEG C for 1-3h to obtain the cobalt manganese spinel microspheres. The cobalt manganese spinel microspheres are used for research on thermal catalytic CO2 reduction and can produce synthetic organic fuel (methane). The cobalt manganese spinel obtained by the preparation method is a pure phase and spherical, has a high specific surface area, obvious exposes the high-energy crystal surface, reduces the temperature of thermal catalytic CO2 reduction and has high product selectivity.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a cobalt-manganese spinel microsphere, specifically a preparation method of the cobalt-manganese spinel microsphere. Background technique [0002] Carbon is an important raw material in the chemical industry. The main component of a large number of chemical products is carbon. It is of great economic and social significance to replace oil, natural gas and many polymer materials with carbon dioxide as the future "carbon source". Toyota Central Research Institute uses water and carbon dioxide as raw materials to synthesize useful substances using sunlight, and the energy conversion efficiency has increased to 4.6%, the highest in the world (2016). BASF of Germany converts carbon dioxide into carbonate polymer materials with wide application. Bayer can use carbon dioxide in the flue gas of thermal power plants as the main raw material for the production of polyurethane materials. Car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00B01J23/889C07C1/12C07C9/04
CPCB01J23/005B01J23/8892C01G51/40C01P2004/32C07C1/12C07C2523/889C07C9/04
Inventor 刘志福李昊臻卢瑛
Owner SHANGHAI INST OF TECH
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