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Preparation method of porous metallic oxide stacked by nano-particles

A porous metal and nanoparticle technology, applied in the direction of magnesium oxide, ferrous oxide, nanotechnology, etc., can solve the problems of expensive use, complicated process, high cost, etc., and achieve the effect of reducing cost and simple preparation process

Inactive Publication Date: 2015-03-25
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this solvent evaporation method not only uses relatively expensive organic solvents, but also takes a long time, which also limits the practical application of this method.
[0003] Therefore, both the hard template and the solvent evaporation method have the defects of complicated process, long production cycle and high cost.

Method used

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  • Preparation method of porous metallic oxide stacked by nano-particles

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Embodiment 1

[0019] Mesoporous alumina (abbreviated as MA) uses cetyltrimethylammonium bromide (CTAB, analytically pure) as a template agent, sodium tartrate (ST, analytically pure) or sodium citrate (analytical pure) or succinate Sodium acid (analytical pure) is auxiliary agent, Al 2 (SO 4 ) 3 .18H 2 O (analytical pure) is the aluminum source, and urea is the precipitating agent. During the synthesis, the molar composition of the solution is first determined as: Al 2 (SO 4 ) 3 / CTAB / ST / CO(NH) 2 / H2O=1.0 / 0.1 / x / 2 / 140, the sodium tartrate / aluminum molar ratio (x) varied from 0 to 0.5. Then the solution was transferred into a polytetrafluoroethylene autoclave, and the reaction kettle was maintained at 165°C for 3 hours, then cooled to room temperature, filtered, washed and then dried at 80°C for 12 hours to obtain a sample. The obtained samples are denoted as MAT-x. The prepared mesoporous aluminum oxide was calcined at 550°C to remove the template and the obtained alumina was denote...

Embodiment 2

[0026] Mesoporous magnesia uses octadecyltrimethylammonium bromide (OTAB analytical pure) as template agent, sodium tartrate (ST, analytical pure) as auxiliary agent, Mg(NO 3 ) 2 (Analytical pure) is the magnesium source, and urea or ammonia water is the precipitating agent. During the synthesis, the molar composition of the solution is firstly determined as: Mg(NO 3 ) 2 / OTAB / ST / CO(NH) 2 / H2O=1.0 / 0.2 / x / 2 / 120, the molar ratio (x) of sodium tartrate / magnesium varies from 0 to 0.4. Then the solution was transferred into a polytetrafluoroethylene autoclave, and the reaction kettle was maintained at 120° C. for 2 hours, then cooled to room temperature, filtered, washed and then dried at 100° C. for 12 hours to obtain a sample. The obtained samples were denoted as MMgO-x. The prepared mesoporous magnesium oxide was calcined at 500°C to remove the template and the obtained magnesium oxide was denoted as MMgO-xC.

[0027] T1: OTAB (0.005mol), Mg (NO 3 ) 2 (0.025mol), CO(NH) ...

Embodiment 3

[0033] Mesoporous copper oxide uses cetyltrimethylammonium bromide (CTAB analytical grade) as template agent, sodium citrate (CA, analytical grade) as auxiliary agent, CuSO 4 .5H 2 O (analytical pure) is the copper source, and ammonia water is the precipitating agent. During the synthesis, the molar composition of the solution is first determined as: CuSO 4 / CTAB / CA / NH 3 / H 2 O=1.0 / 0.1 / x / 3 / 120, the sodium citrate / copper molar ratio (x) varied from 0 to 0.4. Then the solution was transferred to a glass round bottom flask, a reflux condenser was installed, the solution was refluxed at 100°C for 2 hours, then cooled to room temperature, filtered, washed and then dried at 100°C for 12 hours to obtain a sample. The obtained samples are denoted as MCuO-x. The prepared mesoporous copper oxide was calcined at 550°C to remove the template and the obtained copper oxide was denoted as MCuO-xC.

[0034] T1: CTAB (0.005mol), CuSO 4 (0.05mol) and a certain amount of sodium citrate we...

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Abstract

The invention relates to a preparation method of porous metallic oxide stacked by nano-particles. The preparation method comprises the following steps: mixing a cationic surface active agent, a metal salt, hydroxycarboxylic acid and a precipitating agent for reaction, and recovering an intermediate product; and roasting the intermediate product to obtain the porous metallic oxide stacked by the nano-particles. By adopting the preparation method provided by the invention, the aim of quickly preparing the porous metallic oxide stacked by the nano-particles is achieved by adding hydroxycarboxylic acid into an aqueous solution of the cationic surface active agent to react with a metallic matrix. By adding the hydroxycarboxylic acid, the size of first-grade nano-particles is controlled, the assembly of nano-particles is assisted to form second-grade micron particles, and rich mesopores are constructed. By introducing the mesopores, the characteristic of a high specific surface of a nano material is kept, the problem that the nano material is difficult to filter and recover is solved, and three processes of preparation, assembly and pore forming of the nano-particles are realized in one kettle. The preparation method disclosed by the invention is simple in process, and water is adopted as a solvent, so that the preparation method is environment-friendly and the cost is greatly reduced.

Description

technical field [0001] The invention relates to the field of metal oxidation preparation, in particular to a method for preparing porous metal oxides packed with nanoparticles. Background technique [0002] Currently, the preparation of porous metal oxides is mostly based on the use of hard templates and solvent evaporation. The so-called hard template refers to a skeleton with voids, such as colloidal crystals, mesoporous carbon materials, etc. When the voids are filled with precursors, the original skeleton is removed to obtain a porous structure opposite to the original structure, which is widely used in non-silicon Synthesis of Porous Materials. However, the production process of this method is cumbersome. For example, using mesoporous carbon as a template, mesoporous silicon oxide is usually prepared through soft template guidance, and then the mesoporous carbon is obtained by turning the mold, and then the non-silicon mesoporous material is obtained by turning the mol...

Claims

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Application Information

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IPC IPC(8): C01F7/02C01F5/02C01G3/02C01G49/04C01G53/04B82Y30/00
Inventor 岳明波李雪妮李言信马令娟任丹丹
Owner QUFU NORMAL UNIV
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