Nano zirconium dioxide with high specific surface area and synthesis method thereof

A nano-zirconia, high specific surface area technology, applied in zirconia, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problems of reducing the specific surface area of ​​products, amorphous, low specific surface area, etc.

Inactive Publication Date: 2014-12-17
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It is currently reported that adding carboxyl-containing organic coating agents (such as oleic acid, capric acid, etc.) in the hydrothermal synthesis to prevent particle agglomeration and obtain a certain dispersion effect, but the subsequent processing is complicated and the product is amorphous , although the crystalline product can be obtained after high-temperature calcination, the specific surface area of ​​the product is also reduced; there are also reports of adding a cationic organic coating agent in the synthesis, and the results show that the crystal product with good dispersion is synthesized, but its particle size The diameter is about 10nm and the specific surface area is not high (no more than 300m 2 / g)
Obviously, it is still a big challenge to synthesize nano-zirconia with high crystallinity, high dispersion, ultra-fine particle size and high specific surface area.

Method used

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  • Nano zirconium dioxide with high specific surface area and synthesis method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0018] Weigh 11.14g cyclohexanol and put it into a beaker, and get another 0.959g of Zr(OC 4 h 9 ) 4 Drop into a beaker, mix and stir the two solutions for 10 minutes, pour into a 30ml weighing bottle; then put the weighing bottle containing the above mixed solution into a polytetrafluoroethylene liner pre-filled with 15ml distilled water, and seal it in In a stainless steel reactor, react in an oven at 120°C for 24 hours; take it out, cool the reactor with cold water, wash the solid product with ethanol, centrifuge, and dry it in an oven at 60°C for 12 hours. The crystal phase of the obtained sample is a tetragonal phase, and the grain size is 2.4nm, the BET surface area is 399 m 2 g -1 .

Embodiment approach 2

[0020] Weigh 11.14g cyclohexanol and put it into a beaker, and get another 0.959g of Zr(OC 4 h 9 ) 4 Drop into a beaker, mix and stir the two solutions for 10 minutes, pour into a 30ml weighing bottle; then put the weighing bottle containing the above mixed solution into a polytetrafluoroethylene liner pre-filled with 15ml distilled water, and seal it in In a stainless steel reactor, react in an oven at 140°C for 24 hours; take it out, cool the reactor with cold water, wash the solid product with ethanol, centrifuge, and dry it in an oven at 60°C for 12 hours. The crystal phase of the obtained sample is a tetragonal phase, and the grain size is 2.9nm, the BET surface area is 433 m 2 g -1 .

Embodiment approach 3

[0022] Weigh 11.14g cyclohexanol and put it into a beaker, and get another 0.959g of Zr(OC 4 h 9 ) 4 Drop into a beaker, mix and stir the two solutions for 10 minutes, pour into a 30ml weighing bottle; then put the weighing bottle containing the above mixed solution into a polytetrafluoroethylene liner pre-filled with 15ml distilled water, and seal it in In a stainless steel reactor, react in an oven at 160°C for 24 hours; take it out, cool the reactor with cold water, wash the solid product with ethanol, centrifuge, and dry it in an oven at 60°C for 12 hours. The crystal phase of the obtained sample is tetragonal and monoclinic coexistence, the grain size is 3.8nm, and the BET surface area is 188 m 2 g -1 .

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Abstract

The invention discloses a nano zirconium dioxide with high specific surface area and a synthesis method thereof and belongs to the field of synthesis of nano materials and catalysts. The method is characterized in that an organic solvent serves as an auxiliary agent, and the nano zirconium dioxide with high specific surface area is synthesized by the combination of vapor phase hydrolysis and a hydrothermal method, wherein the obtained sample is high in crystallinity, has the particle size of 2.0-4.3nm, and the specific surface area of 448m<2>.g<-1>. The synthesis method comprises the following steps: mixing a zirconium source (Zr(OC4H9)4) and an organic solvent according to a certain rate, stirring for a certain time, isolating the mixture from distilled water, filling in a high-pressure reaction kettle for reacting in an air-tight mode, and synthesizing the nano zirconium dioxide. Because the vapor phase hydrolysis can be combined with the hydrothermal method, the reaction temperature, reaction time and organic solvent are regulated so as to control the hydrolysis and crystallization speed of the zirconium source in a synergetic mode; and therefore, the nano zirconium dioxide has the characteristic of small and adjustable grain size, particularly has high specific surface area and has more advantages when applied to catalysts and catalyst carriers.

Description

technical field [0001] The invention discloses a high specific surface area nano zirconium dioxide and a synthesis method thereof, belonging to the field of synthesis of nanometer materials and catalysts. Specifically, it relates to a technical scheme of nano-zirconium dioxide with high specific surface area, high crystallinity, high dispersion, controllable grain size and crystal phase and its synthesis method. Background technique [0002] Nano zirconium dioxide not only has the structural characteristics of small size effect, surface effect and quantum size effect of nanomaterials, but also has its inherent high hardness, good chemical stability, surface acidity, alkalinity, oxidation and reduction, etc. Excellent performance makes this kind of material have broad application prospects in ceramic toughening, photoelectric devices, solar cells, gas sensors, adsorption, acid-base catalysis and photocatalysis. Especially in the application of acid-base catalytic reaction sy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82Y30/00
Inventor 李瑞丰石国亮于峰张继龙白亚东苗海霞马静红
Owner TAIYUAN UNIV OF TECH
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