Universal synthesis method for porous hollow metallic oxide

An oxide and hollow technology, applied in the field of preparation of inorganic non-metallic materials, can solve the problems of complex process, many steps, unfavorable for industrial scale up, etc., and achieve the effects of low preparation cost, good dispersibility, and easy industrial production.

Inactive Publication Date: 2008-10-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process of this method is more complicated, and there are many steps, which is not conducive to industrial scale-up.

Method used

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  • Universal synthesis method for porous hollow metallic oxide
  • Universal synthesis method for porous hollow metallic oxide
  • Universal synthesis method for porous hollow metallic oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1.2~4.8g Cu(NO 3 ) 2 ·3H 2 O was added to the reaction vessel, 25 mL of dimethyl sulfoxide was slowly added at room temperature, and the reaction was stirred at a stirring speed of 120 rpm for 10 minutes. After the dissolution is complete, 0-2 g of polyvinylpyrrolidone (Mw=80000) and 0.38-1.52 g of thiourea are added respectively. After the solution has completely dissolved and turned into a clear solution, put it into a 30mL autoclave, heat up to 80-180°C at a heating rate of 5°C / min, and then react for 5-48h. Cool naturally at room temperature after the reaction is complete, centrifugally filter the obtained black solution, wash with distilled water and absolute ethanol, and dry at 60° C. for 4 hours to obtain a cake-shaped copper sulfide precursor. The temperature was raised to 400°C at a heating rate of 20°C / min and then calcined for 4 hours to obtain a porous cake-like CuO hollow structure. It has been determined that its average diameter is about 1.7 μm and it...

Embodiment 2

[0025] 1.2~4.8g Cu(NO 3) 2 ·3H 2 O was added to the reaction vessel, 25 mL of dimethylformamide was slowly added at room temperature, and the reaction was stirred at a stirring speed of 120 rpm for 10 minutes. After the dissolution is complete, 0-2 g of polyvinylpyrrolidone (Mw=80000) and 0.38-1.52 g of thiourea are added respectively. After the solution has completely dissolved and turned into a clear solution, put it into a 30mL autoclave, heat up to 80-180°C at a heating rate of 5°C / min, and then react for 5-48h. Cool naturally at room temperature after the reaction is complete, centrifugally filter the obtained black solution, wash with distilled water and absolute ethanol, and dry at 60° C. for 4 hours to obtain a spherical cuprous sulfide precursor. The temperature was raised to 400°C at a heating rate of 20°C / min and then calcined for 4 hours to obtain a porous spherical CuO hollow structure. Its average diameter was determined to be about 900nm.

Embodiment 3

[0027] 1.2~4.8g Cu(NO 3 ) 2 ·3H 2 O was added to the reaction vessel, 25 mL of formamide was slowly added at room temperature, and the reaction was stirred at a stirring speed of 120 rpm for 10 minutes. After the dissolution is complete, 0-2 g of polyvinylpyrrolidone (Mw=80000) and 0.8-2 g of sodium selenite are added respectively. After the dissolution is complete, put it into a 30mL autoclave, raise the temperature to 80-180°C at a heating rate of 5°C / min, and then react for 5-48h. Cool naturally at room temperature after the reaction is complete, filter the obtained solution, wash with distilled water and absolute ethanol, and dry at 60°C for 4 hours to obtain a fibrous copper selenide precursor. The temperature was raised to 400° C. at a heating rate of 20° C. / min and then calcined for 4 hours to obtain porous CuO hollow fibers. It has been determined that its diameter is 3-5 μm and its length is 30-40 μm.

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Abstract

The invention belongs to to the field of the preparation of inorganic non-metallic material, more particularly relates to a common method for synthesizing hollow metal oxide with high porosity. The method of the invention adopts soluble transition metal nitrate (MNO3, M is equal to Cu, Ni, Co), soluble sulfur source (thiourea) and selenium source (sodium selenite, Na2SeO3) as raw materials; metal sulfides (CuS, Cu2S, NiS, CoS) and the precursor of a selenide (CuSe) are first prepared and then treated with temperature programming and high temperature oxidation to obtain a corresponding porous metal oxide hollow framework (CuO, NiO and Co3O4). The method of the invention overcomes the defects such as high cost of material and production and complex process, etc., in the prior preparation method and the prepared metal oxides has large specific surface area, high thermal stability and good dispersity without need of being added with costly macromolecular organic templates and is easy to achieve industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic non-metallic materials, and in particular relates to a general method for synthesizing hollow metal oxides with high porosity. Background technique [0002] Inorganic materials with porous or hollow structures have been extensively studied due to their great application value in catalysis, drug release, gas sensors, and environmental pollution treatment. Transition metal oxides such as copper oxide (CuO), tricobalt tetroxide (Co 3 o 4 ), and nickel oxide (NiO) are a very important class of semiconductor materials. Among them, CuO, as a multifunctional fine inorganic material, has a history of decades in the fields of catalysis, printing and dyeing, ceramics, glass and medicine. Using CuO as the film material can well control the selectivity of the device, such as improving the sensitivity to carbon monoxide (CO). As the main active ingredient in industrial catalysts, CuO has been widely...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01G3/02C01G51/04C01G53/04
Inventor 薛冬峰刘军
Owner DALIAN UNIV OF TECH
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