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Porous oxide and preparation method thereof

A technology of porous oxide and porous structure, applied in the field of porous materials, can solve the problems of complex post-processing, easy collapse, low yield and so on

Inactive Publication Date: 2017-09-08
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, using existing methods to prepare porous oxides, the yield is low, the shape is not easy to maintain, the post-treatment is very complicated, it is easy to introduce heterogeneous impurities, and it is easy to collapse at high temperature

Method used

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  • Porous oxide and preparation method thereof
  • Porous oxide and preparation method thereof
  • Porous oxide and preparation method thereof

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preparation example Construction

[0047] The invention provides a method for preparing a porous oxide, comprising the following steps:

[0048] mixing the inorganic salt solution and the polymer solution to obtain a precursor solution;

[0049] The precursor solution is sequentially subjected to freezing treatment and drying treatment to obtain a porous structure precursor;

[0050] The porous structure precursor is calcined to obtain a porous oxide.

[0051] The invention mixes the inorganic salt solution and the polymer solution to obtain the precursor solution. In the present invention, the inorganic salt is preferably a soluble salt, more preferably one or more of bismuth nitrate, nickel nitrate, phosphotungstic heteropolyacid (HPW), zinc acetate and tin chloride; The mass concentration of the solution is preferably 1-10%, more preferably 2-9%, most preferably 4-6%. The present invention does not have any special requirements on the source of the inorganic salt, and commercially available products of th...

Embodiment 1

[0063] 2.5wt% PVA aqueous solution and 9wt% HPW aqueous solution were mixed according to a mass ratio of 0.25:1, and magnetically stirred at a speed of 800r / min for 12h to obtain a precursor solution.

[0064] Put the precursor solution in a centrifuge tube, insert it into liquid nitrogen quickly in an orientation, and quickly move it into a vacuum drying device, keep the vacuum degree below 20Pa, and dry it at -60°C for 48 hours to obtain HPW / PVA with a regular pore structure Precursor.

[0065] The above precursors were stabilized at 100 °C in air for 24 h.

[0066] After stabilization treatment, the HPW / PVA precursor was placed in a muffle furnace, raised from room temperature to 300 °C, and kept for 1 h, and raised from 300 °C to 600 °C in an air environment, and kept for 2 h, and the temperature was naturally lowered. During the process, the heating rate was 2° C. / min, and macroporous tungsten trioxide with a pore diameter of about 4.3 microns was obtained.

[0067] The...

Embodiment 2

[0070] Mix 5wt% PVA aqueous solution and 9wt% HPW aqueous solution at a mass ratio of 1.8:1, and magnetically stir at 850r / min for 12h to obtain a precursor solution.

[0071] Put the precursor solution in a centrifuge tube, insert it into liquid nitrogen quickly in an orientation, and quickly move it into a vacuum drying device, keep the vacuum degree below 20Pa, and dry it at -55°C for 40 hours to obtain HPW / PVA with regular pore structure Precursor.

[0072] The above precursors were stabilized at 110 °C in air for 24 h.

[0073] After stabilization treatment, the HPW / PVA precursor was placed in a muffle furnace, raised from room temperature to 300 °C, and kept for 1 h, and raised from 300 °C to 600 °C in an air environment, and kept for 2 h, and the temperature was naturally lowered. During the process, the heating rate is 2° C. / min, and the macroporous tungsten trioxide with a pore diameter of 3 to 10 μm and a fishbone three-dimensional structure is obtained.

[0074] T...

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Abstract

The invention provides a porous oxide and a preparation method thereof. The preparation method comprises the following steps of mixing an inorganic salt solution with a polymer solution, so as to obtain a precursor solution; carrying out freezing treatment and drying treatment on the precursor solution in sequence, so as to obtain a porous-structure predecessor; carrying out calcination on the porous-structure predecessor, so as to obtain the porous oxide. According to the preparation method, through the assistance of a polymer, the polymer is closely combined with an inorganic salt together; the growth of an ice crystal is impeded; a porous precursor is formed; the polymer is removed in a high-temperature calcination process; the inorganic salt is decomposed into an oxide and grows by using the porous precursor as a template, so as to obtain a porous oxide material which has a macroscopic three-dimensional structural feature and is uniform in pore canal.

Description

technical field [0001] The invention relates to the technical field of porous materials, in particular to a porous oxide and a preparation method thereof. Background technique [0002] Porous materials are a class of functional materials with obvious pore characteristics and a uniform pore structure. Due to the special porous structure of porous materials, it has the characteristics of high specific surface area, high porosity, high permeability, high adsorption and assembleability, and has high thermal conductivity, high electrical conductivity, corrosion resistance and fatigue resistance. And many other excellent physical and chemical properties, so it is widely used in chemical industry, biomedicine, environmental protection, functional materials and other fields. [0003] Porous oxide materials have received a lot of attention in the past few decades, and great progress has been made in this field. The high specific surface area and rich pore structure of porous oxides...

Claims

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Application Information

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IPC IPC(8): C01B13/18
CPCC01B13/18C01P2002/72C01P2004/03C01P2004/30C01P2006/16
Inventor 孙威邵长路刘益春李兴华魏诗琪
Owner NORTHEAST NORMAL UNIVERSITY
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