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Preparation method of oxide porous material

A technology of porous materials and oxides, which is applied in the field of preparation of oxide porous materials, can solve the complex process of colloidal crystal templates, the difficulty of large-scale control of the properties of the target material, such as pore size, porosity and wall thickness, and difficulty in large-scale production and other problems to achieve the effect of avoiding the instability of the overall structure, improving stability and functionality, and suitable operation

Active Publication Date: 2016-04-13
WUHAN UNIV OF SCI & TECH
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Problems solved by technology

When the colloidal crystal template method is used, it is usually necessary to prepare the colloidal crystal template in advance, and the process of preparing the colloidal crystal template is relatively complicated, and it is difficult to produce on a large scale. Properties such as porosity and wall thickness are not easy to control in a large range

Method used

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  • Preparation method of oxide porous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of manganese dioxide porous material. The preparation method is:

[0027] 1) Dissolve manganese nitrate tetrahydrate in tert-butanol at a concentration of 5 to 6.5 mol / L, stir for 3 to 5 hours to obtain solution I.

[0028] 2) According to the mass ratio of manganese nitrate tetrahydrate and ethyl cellulose of 1: (0.01~0.04), add ethyl cellulose to solution I and stir for 1 to 2 hours to obtain solution II.

[0029] 3) According to the mass ratio of manganese nitrate tetrahydrate to silicon dioxide of 1:(0.25~0.35), add silicon dioxide to solution II and stir for 3~5 hours to obtain solution III.

[0030] 4) The solution III is subjected to liquid nitrogen freezing treatment, and then dried in a vacuum freeze dryer for 48 to 72 hours to obtain a dried product.

[0031] 5) Put the dried product in a tube furnace, heat it up to 300~500℃ at a rate of 4~5℃ / min in an argon atmosphere or air atmosphere, keep it for 4~7h, and cool down naturally with the furnace to...

Embodiment 2

[0034] A preparation method of titanium dioxide porous material. The preparation method is:

[0035] 1) According to the concentration of 6.5~8.0mol / L, dissolve titanium sulfate in tert-butanol and stir for 3~5 hours to obtain solution I.

[0036] 2) According to the mass ratio of titanium sulfate to polyvinylpyrrolidone of 1:(0.04~0.07), add polyvinylpyrrolidone to solution I and stir for 1~2 hours to obtain solution II.

[0037] 3) According to the mass ratio of titanium sulfate to polymethyl methacrylate of 1: (0.15-0.25), add polymethyl methacrylate to solution II, stir for 3 to 5 hours to obtain solution III.

[0038] 4) The solution III is subjected to liquid nitrogen freezing treatment, and then dried in a vacuum freeze dryer for 48 to 72 hours to obtain a dried product;

[0039] 5) Put the dried product in a tube furnace, heat it up to 500~700℃ at a rate of 4~5℃ / min in an argon atmosphere or air atmosphere, keep it for 7~10h, cool naturally with the furnace, and remove the temp...

Embodiment 3

[0042] A preparation method of lithium titanate porous material. The preparation method is:

[0043] 1) According to the concentration of each substance of 8.0~10.0mol / L, dissolve tetrabutyl titanate and lithium acetate dihydrate in an organic solvent successively, and stir for 3~5 hours to obtain solution I.

[0044] The organic solvent is a mixed solvent of ethanol and glacial acetic acid, and the volume ratio of ethanol and glacial acetic acid in the mixed solvent is 1:1.

[0045] 2) According to the mass ratio of the mixed salt of tetrabutyl titanate and lithium acetate dihydrate to ethyl cellulose is 1: (0.07~0.10), add ethyl cellulose to solution I and stir for 1 to 2 hours to obtain Solution II.

[0046] 3) According to the mass ratio of the mixed salt of tetrabutyl titanate and lithium acetate dihydrate to polystyrene of 1:(0.10~0.15), add polystyrene to solution II and stir for 3~5 hours to obtain solution III .

[0047] 4) The solution III is subjected to liquid nitrogen fr...

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Abstract

The invention relates to a preparation method of an oxide porous material. According to the technical scheme, the method comprises the steps that an oxide precursor salt is dissolved in organic solvent according to the concentration ranging from 5 mol / L to 10 mol / L, stirring is conducted, and a solution I is obtained; a binder is added into the solution I according to the mass ratio of the oxide precursor salt to the binder of 1 to 0.01-0.1, stirring is conducted, and a solution II is obtained; a template agent is added into the solution II according to the mass ratio of the oxide precursor salt to the template agent of 1 to 0.1-0.35, stirring is conducted, and a solution III is obtained; liquid nitrogen freezing treatment is conducted on the solution III, drying is conducted in a vacuum freezing dryer, and a dried product is obtained; the product is put in a tube furnace, the temperature rapidly rises to 300-800 DEG C at the speed of 4-5 DEG C / min in an argon atmosphere or air atmosphere, heat preservation is conducted for 4-12 h, natural cooling is conducted along with the furnace, the template agent is removed, and the oxide porous material is obtained. The preparation method of the oxide porous material is convenient to operate and suitable for industrial production, and the hole size, the porosity and the wall thickness of the product can be regulated in a larger range.

Description

Technical field [0001] The invention belongs to the technical field of porous material preparation. Specifically, it relates to a method for preparing porous oxide materials. Background technique [0002] Porous materials have the characteristics of high specific surface area, low relative density, good permeability, light weight, unique pore structure and excellent adsorption performance. They are used in many aspects such as energy storage and conversion, catalytic reaction, adsorption, separation, filtration, noise reduction and heat insulation. It is widely used. Therefore, the development of a simple and effective preparation method to control the pore structure of porous materials is the key to their application in these fields. [0003] At present, porous materials are mainly prepared by colloidal crystal template method, including hard template method and soft template method. When using the colloidal crystal template method, it is usually necessary to prepare the colloi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01G45/02C01G23/08C01G23/00
CPCC01B13/14C01G23/005C01G23/08C01G45/02C01P2002/72C01P2004/03C01P2006/12C01P2006/16
Inventor 周盈科田小慧胡敏涂晓峰都国栋
Owner WUHAN UNIV OF SCI & TECH
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