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Preparation method of nickel oxide/alumina and nickel/alumina nanometer compound microparticle

A technology of alumina nano and composite microspheres, which is applied in the preparation of nickel oxide/alumina nanocomposite microspheres and the field of nickel/alumina Poor spherical uniformity, weak combination of catalytic particles and carrier, etc., to achieve the effect of firm combination and good particle distribution uniformity

Inactive Publication Date: 2013-07-24
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of nickel oxide / alumina nanocomposite microspheres, which solves the problem of the poor uniformity of the nickel oxide / alumina nanocomposite microspheres prepared in the prior art and the weak combination of catalytic particles and the carrier, which is easy to shedding problem

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  • Preparation method of nickel oxide/alumina and nickel/alumina nanometer compound microparticle
  • Preparation method of nickel oxide/alumina and nickel/alumina nanometer compound microparticle
  • Preparation method of nickel oxide/alumina and nickel/alumina nanometer compound microparticle

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preparation example Construction

[0028] The preparation method of the nickel oxide / alumina nanocomposite microsphere of the present invention, concrete steps are as follows:

[0029] Step 1, prepare 0.03mol / L of Al(NO 3 ) 3 9H 2 0, the mixed solution of cetyltrimethylammonium bromide of 0.045mol / L and the NaOH of 1.0mol / L, solvent is the mixed solvent of deionized water and alcohol, and the volume ratio of deionized water and alcohol is 2: 1-20:1, choose methanol or n-butanol as the alcohol, then add ethyl acetate, the volume ratio of ethyl acetate to solvent is 1:10, and get a colorless transparent liquid after magnetic stirring for 30min, add 30ml colorless transparent liquid Put the solvent into a hydrothermal kettle with a polytetrafluoroethylene liner of 100ml, and then put it into the MDS-8 multi-channel closed microwave chemical station to carry out microwave hydrothermal reaction at 160°C for 60min, then centrifuge and use deionized water and Wash with absolute ethanol several times, and finally va...

Embodiment 1

[0037] Step 1, 0.35g of Al(NO 3 ) 3 9H 2 O, 0.5g of cetyltrimethylammonium bromide and 1.2g of NaOH were dissolved in 30ml of deionized water and methanol in a mixed solvent with a volume ratio of 2:1 in a stirring state, and then 3ml of ethyl acetate was added , after magnetic stirring for 30 minutes, a colorless and transparent liquid was obtained. Take 30ml of the colorless and transparent liquid and add it to a 100ml hydrothermal kettle with a polytetrafluoroethylene liner as the solvent, and then put it into the MDS-8 multi-channel closed microwave chemical station. Perform microwave hydrothermal reaction at 160°C for 60 minutes, centrifuge, wash with deionized water and absolute ethanol several times, and finally vacuum-dry at 80°C for 24 hours to obtain boehmite self-assembled microsphere powder;

[0038] Step 2, weigh 1.2g of the boehmite self-assembled microsphere powder obtained in step 1 and add it to 50ml of nickel nitrate hexahydrate solution with a concentratio...

Embodiment 2

[0041] Step 1, 0.35g of Al(NO 3 ) 3 9H 2 O, 0.5g of cetyltrimethylammonium bromide and 1.2g of NaOH were dissolved in 30ml of deionized water and methanol in a mixed solvent with a volume ratio of 10:1 in a stirring state, and then 3ml of ethyl acetate was added , after magnetic stirring for 30 minutes, a colorless and transparent liquid was obtained. Take 30ml of the colorless and transparent liquid and add it to a 100ml hydrothermal kettle with a polytetrafluoroethylene liner as the solvent, and then put it into the MDS-8 multi-channel closed microwave chemical station. Perform microwave hydrothermal reaction at 160°C for 60 minutes, centrifuge, wash with deionized water and absolute ethanol several times, and finally vacuum-dry at 80°C for 24 hours to obtain boehmite self-assembled microsphere powder;

[0042] Step 2, weigh 1.2g of the boehmite self-assembled microsphere powder obtained in step 1 and add it to 50ml of nickel nitrate hexahydrate solution with a concentrati...

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Abstract

A preparation method of nickel oxide / alumina and nickel / alumina nanometer compound microparticle specifically comprises the following steps of: (1) orderly dissolving aluminum nitrate nonahydrate, cetyl trimethyl ammonium bromide and sodium hydroxide to solvent and adding ethyl acetate, carrying out microwave hydrothermal reaction after magnetic stirring, centrifugally separating and washing for multiple times by using deionized water and absolute ethyl alcohol, and finally carrying out vacuum drying to obtain Boehmite self-assembly microparticle powder; and (2) adding the Boehmite self-assembly microparticle powder obtained in the step (1) to nickel nitrate hexahydrate for ultrasonic vibration, then centrifugally separating and washing for multiple times by using deionized water for vacuum drying, naturally cooling the product after calcining to obtain nickel oxide / alumina nanometer compound microparticle; preparing nicel / alumina nanometer compound microparticle after heating reduction of the nickel oxide / alumina nanometer compound microparticle. The particles of the nickel oxide / alumina and nickel / alumina nanometer compound microparticle prepared by the method are good in distribution uniformity and firmly combined with carriers.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a preparation method of nickel oxide / alumina nanocomposite microspheres, and also relates to a method for preparing nickel / alumina nanocomposite microspheres by using the nickel oxide / alumina nanocomposite microspheres Methods. Background technique [0002] The research on nano-assembly system has become a hotspot in the research of nano-materials, that is, nano-particles or nano-wires, nano-tubes, and nano-sheets are assembled and arranged in one-dimensional, two-dimensional and three-dimensional spaces to form a system with nanostructures, such as nanomicrostructures. Spherical materials, nano-clusters and nano-ordered arrays. The nano-assembly composite material is an important research object of the current nano-assembly system. Its main design idea is to use the quantum size effect and seepage effect of small particles to tailor the overall performance of the mat...

Claims

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Application Information

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IPC IPC(8): B01J23/755
Inventor 何选盟刘辉李军奇朱振峰李广军董晓楠
Owner SHAANXI UNIV OF SCI & TECH
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