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Method for large-scale preparation of transition metal oxide porous microsphere

A technology of porous microspheres and transition metals, applied in iron oxide, microsphere preparation, nickel oxide/nickel hydroxide, etc.

Inactive Publication Date: 2016-02-03
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem solved by the present invention is to provide a method for large-scale preparation of porous transition metal oxide microspheres, which solves the problem of large-scale production of nanoparticles in the prior art, and the method provided can realize porous transition metal oxides Large-Scale Preparation of Microspheres

Method used

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  • Method for large-scale preparation of transition metal oxide porous microsphere
  • Method for large-scale preparation of transition metal oxide porous microsphere
  • Method for large-scale preparation of transition metal oxide porous microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0022] co 3 o 4 Preparation of porous microspheres

[0023] 1) Use a 50mL graduated cylinder to measure 30mL of ethylene glycol and dissolve it in a 200mL beaker with 120mL of isopropanol, stir for 2 hours to form a homogeneous solution with a mass concentration of ethylene glycol of 26.8%;

[0024] 2) Under stirring conditions, 3.35g of cobalt nitrate hexahydrate was added to the homogeneous solution, and a homogeneous precursor solution was obtained after stirring for 1 hour;

[0025] 3) Transfer the obtained precursor solution to Yacheng YC-018 spray dryer for drying. The air inlet temperature is 350°C, the air outlet is 90°C, the drying gas is nitrogen, and the feed rate is 4mL / min. The obtained powder Collected from the bottom of the drying tower and cyclone separator;

[0026] 4) The obtained powder was placed in a muffle furnace at a heating rate of 2 °C / min to 350 °C for 3 h, and then naturally cooled to room temperature to obtain Co with an average diameter of 4.79...

Embodiment 2

[0029] NiCo 2 o 4 Preparation of porous microspheres

[0030] 1) Use a 10mL graduated cylinder to measure 10mL of ethylene glycol and dissolve it in a 100mL beaker filled with 80mL of ethanol, and stir for 1 hour to form a homogeneous solution with a mass concentration of ethylene glycol of 11.1%;

[0031] 2) Under stirring conditions, dissolve 3.57g of cobalt nitrate hexahydrate and 1.79g of nickel nitrate hexahydrate into the homogeneous solution, and keep stirring for 2 hours to obtain a homogeneous precursor solution;

[0032] 3) Transfer the obtained precursor solution to Yacheng YC-018 spray dryer for drying. The air inlet temperature is 300°C, the air outlet is 100°C, the drying gas is nitrogen, and the feed rate is 2mL / min. The obtained powder Collected from the bottom of the drying tower and cyclone separator;

[0033] 4) Put the obtained powder in a muffle furnace to heat up to 400°C for 2 hours at a rate of 1°C / min for calcination, and then naturally cool to room t...

Embodiment 3

[0037] Fe 2 o 3 Preparation of porous microspheres

[0038] 1) Use a 10mL graduated cylinder to measure 5mL glycerol and dissolve it in a 100mL beaker filled with 80mL isopropanol, and stir for 1 hour to form a homogeneous solution with a mass concentration of glycerol of 7.4%;

[0039] 2) Under stirring conditions, add 3.64g of ferric nitrate nonahydrate into the homogeneous solution, and keep stirring for 2 hours to obtain a homogeneous precursor solution;

[0040] 3) Transfer the obtained precursor solution to Yacheng YC-018 spray dryer for drying. The air inlet temperature is 220°C, the air outlet is 90°C, the drying gas is nitrogen, and the feed rate is 2.5mL / min. The obtained powder The body is collected by the bottom of the drying tower and the cyclone separator;

[0041] 4) Put the obtained powder in a muffle furnace to heat up to 650°C for 2 hours at a rate of 3°C / min, and then cool naturally to room temperature to obtain Fe with an average diameter of 380nm. 2 o ...

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Abstract

The invention discloses a method for large-scale preparation of a transition metal oxide porous microsphere, and belongs to the technical field of synthesis of nano materials. The key points of the technical scheme of the invention are as below: dissolving polyhydric alcohol in an organic solvent under room temperature to form a uniform solution; adding the transition metal salt to the uniform solution under the condition of stirring, and uniformly mixing to obtain a precursor solution; transferring the precursor solution for drying in a spray dryer, and collecting the powder at the bottom of a drying tower by a cyclone separator; placing the powder in a muffle furnace, heating to 350-650 DEG C at heating rate of 1-8 DEG C / min, calcining 0.5-5 h and naturally cooling to room temperature obtain the transition metal oxide porous microsphere. The invention realizes the large-scale preparation of transition metal oxide porous microsphere; spray drying can realize continuous process in nanomaterial preparation; and the prepared transition metal oxide porous microsphere can be used directly, without crushing or grinding.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nanometer materials, and in particular relates to a method for large-scale preparation of transition metal oxide porous microspheres. Background technique [0002] Transition metal oxide nanoparticles are extremely small, showing different surface properties from bulk transition metal oxide materials, which have unique physical and chemical properties, which in turn enable nano-transition metal oxides to be used in catalysis, drug release, gas sensors and environmental Pollution treatment and other fields also show great potential application value. [0003] However, as the particle size of nano-transition metal oxide nanoparticles decreases, the surface energy of nanoparticles increases sharply, which leads to the agglomeration of nanoparticles very easily, which also reduces the specific surface area and reactivity of the particles. In order to overcome the phenomenon that nanoparticles ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02C01G49/06C01G51/04C01G53/04C01G3/02
Inventor 苏莉于心爱董文佩张艳吴呈珂毛国江龚毅君冯素玲
Owner HENAN NORMAL UNIV
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