Dual-scale pore structure nanocrystalline cobalt titanate powder and preparation method thereof

A pore structure, cobalt titanate technology, applied in the field of porous materials, can solve the problems of complex preparation process, unfavorable industrialization, single pore structure, etc., and achieve the effects of simple operation, low cost and low synthesis temperature

Active Publication Date: 2018-01-19
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The template method uses the template as the main configuration, and the pore structure is single; the preparation process of the molten salt-assisted self-assembly method is complicated, the production cost is high, and it is not conducive to industrialization
There are no relevant reports on the nanocrystalline cobalt titanate powder material with dual-scale pore structure and its preparation method.

Method used

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  • Dual-scale pore structure nanocrystalline cobalt titanate powder and preparation method thereof
  • Dual-scale pore structure nanocrystalline cobalt titanate powder and preparation method thereof
  • Dual-scale pore structure nanocrystalline cobalt titanate powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Adopt 1.94g cobalt nitrate hexahydrate, cobalt nitrate and water are mixed according to the ratio of molar ratio 1:20, obtain cobalt nitrate aqueous solution;

[0029] Stir and mix absolute ethanol, tetrabutyl titanate and complexing agent diethanolamine evenly to prepare solution A, the molar ratio of tetrabutyl titanate to complexing agent is 1:0.7; absolute ethanol and tetrabutyl titanate The mass ratio of ester is 18:1;

[0030] Under stirring conditions, drop glacial acetic acid into solution A until the pH value is 4.5 to prepare solution B;

[0031] Under the condition of a stirring speed of 500rpm, drop the cobalt nitrate aqueous solution into the B solution, the dropping speed is 1mL / min, the amount of the cobalt nitrate aqueous solution is 1:1 according to the molar ratio of cobalt nitrate and tetrabutyl titanate Continue stirring until the formation of cobalt titanate sol (according to Tyndall phenomenon);

[0032] Place the container containing the cobalt ...

Embodiment 2

[0036] Method is with embodiment 1, and difference is:

[0037] (1) The mol ratio of cobalt nitrate and water is 1:12;

[0038] (2) The molar ratio of tetrabutyl titanate and complexing agent in A solution is 1:1.5; The mass ratio of absolute ethanol and tetrabutyl titanate is 21:1;

[0039] (3) Glacial acetic acid is dripped into solution A until the pH value is 3.5;

[0040] (4) Under the condition of a stirring speed of 600rpm, the cobalt nitrate aqueous solution was dropped into the B solution, and the dropping speed was 1.5mL / min;

[0041] (5) The temperature of the water bath is 45°C;

[0042] (6) Drying temperature 105°C, time 2h; roasting temperature 650°C, time 2h;

[0043] The specific surface area of ​​nanocrystalline cobalt titanate powder with double-scale pore structure is 102.5m 2 / g, cobalt titanate weight content 98.9%;

[0044] Phase composition XRD analysis such as figure 1 It can be seen from the figure that the cobalt titanate obtained by calcination...

Embodiment 3

[0048] Method is with embodiment 1, and difference is:

[0049] (1) The mol ratio of cobalt nitrate and water is 1:50;

[0050] (2) The molar ratio of tetrabutyl titanate and complexing agent in solution A is 1:2; the mass ratio of absolute ethanol and tetrabutyl titanate is 15:1;

[0051] (3) Glacial acetic acid is dripped into solution A until the pH value is 2.5;

[0052] (4) Under the condition of a stirring speed of 700rpm, the cobalt nitrate aqueous solution was dropped into the B solution, and the dropping speed was 2mL / min;

[0053] (5) The temperature of the water bath is 50°C;

[0054] (6) Drying temperature 95°C, time 4h; roasting temperature 600°C, time 3.5h;

[0055] The specific surface area of ​​nanocrystalline cobalt titanate powder with double-scale pore structure is 95.3m 2 / g, the weight content of cobalt titanate is 98.3%.

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Abstract

The invention discloses dual-scale pore structure nanocrystalline cobalt titanate powder and a preparation method thereof, and belongs to the technical field of materials. The crystal particle size ofthe dual-scale pore structure nanocrystalline cobalt titanate powder is 50 to 100nm, a space structure is formed by accumulating crystal particles and has big pores of which the size is 150 to 500nmand a mesoporus structure of which the size is 2 to 40nm, and a dual-scale pore structure is formed. The preparation method comprises the following steps: (1) preparing cobalt nitrate and water into acobalt nitrate water solution; (2) stirring and uniformly mixing absolute ethanol, tetrabutyl titanate and a complexing agent, and preparing an A solution; (3) adding glacial acetic acid, thus preparing a B solution; (4) dropwise adding the cobalt nitrate water solution in the B solution, thus forming cobalt titanate sol; (5) stirring in a water bath until obtaining gel; (6) roasting at 550 to 750 DEG C after drying. A product disclosed by the invention has the advantages that the specific surface area is large, diffusion and transportation of a gas can be easily carried out, the effective utilization rate of the specific surface area is high, and the like; the preparation method is simple in operation, is low in synthesis temperature and is low in cost, and complicated equipment is not needed.

Description

technical field [0001] The invention belongs to the technical field of porous materials, and in particular relates to a nanocrystalline cobalt titanate powder with a double-scale pore structure and a preparation method thereof. Background technique [0002] Cobalt titanate with a perovskite structure is a new type of inorganic functional material, which has a wide range of applications in gas sensing, gasoline desulfurization catalysis, humidity sensing, and photocatalytic degradation. Because of its large specific surface area, surface effect, small size effect and quantum size effect, nanocrystalline cobalt titanate has better performance than ordinary cobalt titanate. At present, the methods for preparing cobalt titanate nanomaterials include liquid phase method, gas phase method and solid phase method. The main problems in the application of cobalt titanate nanomaterials prepared by these methods in gas sensing are poor sensitivity at low concentrations of gas, low selec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00B82Y30/00
Inventor 李明春宋兰婷雷一鸣李淑钰
Owner SHENYANG POLYTECHNIC UNIV
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