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Method for preparing nano-scale catalyst cobaltous oxide

A cobalt oxide, nano-scale technology, applied in chemical instruments and methods, cobalt oxide/cobalt hydroxide, physical/chemical process catalysts, etc., can solve the problem of long production process routes, uncontrollable cobalt oxide morphology and particle size , low catalytic activity of catalysts, etc., to reduce production costs, meet industrial production needs, and improve catalytic activity.

Inactive Publication Date: 2016-08-24
吴迪
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem mainly solved by the present invention: Aiming at the problems that occur in the preparation process of the current cobaltous oxide material, the production process route is long, the morphology and particle size of the obtained cobaltous oxide are uncontrollable, resulting in low catalytic activity of the prepared catalyst, providing A preparation method of nano-scale cobaltous oxide is proposed. The present invention first uses cobalt chloride solution as raw material, uses malic acid to complex with cobalt ions in the solution, and slowly releases cobalt ions. Using polystyrene acrylic acid as a template, poly -COOH groups on the surface of styrene acrylic acid and CoCl 2 Solution hydrolysis product Co(OH) 2 Electrostatic and chemical adsorption of colloidal particles, the Co(OH) produced by hydrolysis 2 The colloidal particles are uniformly adsorbed on the surface of polystyrene acrylic acid particles to form a sol. Under heating conditions, Co(OH) 2 The colloidal particles are dehydrated to form CoO crystal nuclei, and the grown CoO crystals are evenly wrapped on the surface of the polystyrene acrylic template, and then transferred to anaerobic conditions for calcination to remove the polystyrene acrylic core to obtain the product cobaltous oxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0015] Weigh 0.5g of polystyrene acrylic acid and 0.2g of malic acid in turn, add them to a closed container containing 100mL of deionized water, move the closed container into a constant temperature water bath at 75°C, stir for 0.5h at 300r / min, and then Pour nitrogen into the airtight container at a rate of 5mL / min until all the air is replaced to make a polystyrene acrylic water emulsion; measure 40mL with a concentration of 0.2mol / L CoCl 2 The solution, while stirring, is slowly added dropwise to the polystyrene acrylic aqueous emulsion obtained above through a dropping funnel, and the dropwise addition is completed within 0.5h, keeping the constant temperature of 75℃ unchanged, after continuing to stir for 1h, the mixture is transferred to the vacuum In the environment, naturally cool to room temperature, filter with suction, wash the filter residue with deionized water until the washing water becomes neutral, and then rinse twice with absolute ethanol; put the filter residu...

example 2

[0018] Weigh 0.8g polystyrene acrylic acid and 0.3g malic acid in turn, add them to a closed container filled with 120mL deionized water, move the closed container into a constant temperature water bath at 80°C, stir at a constant temperature for 1 hour at a speed of 400r / min, and then Blow nitrogen into the airtight container at a rate of 8mL / min until all the air is replaced to make a polystyrene acrylic water emulsion; measure 50mL to a concentration of 0.3mol / L CoCl 2 The solution, while stirring, was slowly added dropwise to the polystyrene acrylic water emulsion obtained above through the dropping funnel, and the addition was completed within 0.8h, keeping the constant temperature of 80℃ unchanged, and after stirring for 1.2h, the mixed solution was transferred into In a vacuum environment, naturally cool to room temperature, filter with suction, wash the filter residue with deionized water until the washing water becomes neutral, and then rinse twice with absolute ethanol;...

example 3

[0021] Weigh 1.0g polystyrene acrylic acid and 0.5g malic acid in turn, add them to a closed container filled with 150mL deionized water, move the closed container into a thermostat water bath at 85℃, stir for 1.5h at 500r / min, and then Pour nitrogen into the airtight container at a rate of 10mL / min until all the air is replaced to make a polystyrene acrylic water emulsion; measure 60mL to a concentration of 0.4mol / L CoCl 2 The solution, while stirring, was slowly added dropwise to the polystyrene acrylic aqueous emulsion obtained above through the dropping funnel, and the addition was completed within 1.0h, keeping the constant temperature of 85°C unchanged, after continuing to stir for 2h, the mixed solution was transferred to the vacuum In the environment, cool to room temperature naturally, filter by suction, wash the filter residue with deionized water until the washing water becomes neutral, and then rinse with absolute ethanol 3 times; put the filter residue obtained above...

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Abstract

The invention discloses a method for preparing a nano-scale catalyst cobaltous oxide and belongs to the field of inorganic chemical synthesis. The method comprises: using cobalt chloride solution as raw material, complexing citric acid with cobalt ions in the solution so that the cobalt ions are released slowly, using poly(styrene acrylic acid) as a template, evenly adsorbing Co(OH)2 colloid particles generated by hydrolysis to the surface of poly(styrene acrylic acid) particles through static and chemical adsorption of -COOH groups on the surface of the poly(styrene acrylic acid) against CoCl2 solution hydrolysate Co(OH)2 colloid particles to form a sol, dewatering the Co(OH)2 colloid particles by heating to generate CoO crystal nuclei, evenly covering the surface of the poly(styrene acrylic acid) template by the grown-up CoO crystal nuclei, subjecting to calcining under anaerobic condition, and removing the poly(styrene acrylic acid) cores to obtain a product, cobaltous oxide. The preparation process is simple, the obtained cobaltous oxide has homogeneous morphology, particle size is simple to control, and particle size distribution range is narrow and is all of nano level.

Description

Technical field [0001] The invention discloses a preparation method of nano-level catalyst cobalt oxide, which belongs to the field of inorganic chemical synthesis. Background technique [0002] Cobalt oxide is a black powder, insoluble in water and alcohol, but soluble in dilute acid and hot concentrated sodium hydroxide solution. It is usually used as the main raw material for the production of cemented carbide, super heat-resistant alloys, insulating materials and magnetic materials, as well as catalysts and dyes in the chemical industry. In industry, CoCl is often used 2 Solution is cobalt source, NH 4 HCO 3 Or NaCO 3 As a precipitant, CoCO is produced 3 , First set CoCO 3 Calcined at 700~800℃ to produce Co 3 O 4 , And then by Co 3 O 4 In a reducing atmosphere, heating to 950 ℃ calcination to obtain CoO, the entire production process line is long, it is easy to bring more impurities, and directly precipitate the obtained CoCO 3 The morphology is complicated, and the particle ...

Claims

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Application Information

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IPC IPC(8): B01J23/75C01G51/04B82Y40/00B01D53/94B01D53/56
CPCB01D53/9413C01G51/04B01J23/75C01P2004/64B01D2258/01B01J35/40
Inventor 吴迪许博伟
Owner 吴迪
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