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A Porous ZrO2 Mesoscopic Crystal with Large Specific Surface

A technology of mesoscopic crystals and large specific surface, applied in catalyst carrier, inorganic chemistry, zirconia and other directions, can solve the problems of unfavorable active metal loading, low specific surface area, and no ZrO2 mesocrystals, etc., to achieve excellent catalytic performance, Good monodispersity and rich pores

Active Publication Date: 2018-07-17
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for supported catalysts, traditional oxide supports generally have a polycrystalline structure, and there is no preferred exposed crystal plane; while single crystal oxides have specific exposed crystal planes, but their specific surface area is extremely low, and there are no pores inside. Not conducive to the loading of active metals
However, there is no ZrO 2 Public reports on mesoscopic crystals and their preparation techniques and applications

Method used

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  • A Porous ZrO2 Mesoscopic Crystal with Large Specific Surface
  • A Porous ZrO2 Mesoscopic Crystal with Large Specific Surface
  • A Porous ZrO2 Mesoscopic Crystal with Large Specific Surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 1.28 g of cetyltrimethylammonium bromide, 11.28 g of zirconium oxychloride octahydrate and 4.2 g of urea in 50 mL of deionized water to prepare a mixed solution, and calibrate the above mixed solution to 70 mL with deionized water Then transfer to a high-temperature reactor with a volume of 100 mL (that is, the molar concentration of zirconium oxychloride octahydrate is 0.5 mol / L, and the molar ratio of zirconium oxychloride octahydrate to cetyltrimethylammonium bromide and urea 1:0.05:2). The reaction kettle was put into a blast drying oven, the reaction temperature was controlled at 150 °C, and the reaction time was 24 h. The obtained product was washed by centrifugation to remove impurity ions and then dried at 60 °C for 8 h to obtain ZrO 2 mesoscopic crystals.

[0026] figure 1 Is the ZrO prepared in this embodiment 2 XRD patterns of mesoscopic crystals. Depend on figure 1 It can be seen that the prepared ZrO 2 Was monoclinic phase.

[0027] figur...

Embodiment 2

[0031] Dissolve 2.04 g of cetyltrimethylammonium bromide, 4.51 g of zirconium oxychloride octahydrate and 1.68 g of urea in 50 mL of deionized water to prepare a mixed solution, and calibrate the above mixed solution to 70 mL with deionized water Transfer volume to be in the high-temperature reactor of 100 mL (namely zirconium oxychloride octahydrate molar concentration is 0.2 mol / L, the molar ratio of zirconium oxychloride octahydrate and cetyltrimethylammonium bromide, urea is 1:0.4:2). The reaction kettle was put into a blast drying oven, the reaction temperature was controlled at 130 °C, and the reaction time was 48 h. The obtained product was washed by centrifugation to remove impurity ions and then dried at 60 °C for 8 h to obtain ZrO 2 mesoscopic crystals.

[0032] Figure 5 Is the ZrO prepared in this embodiment 2 SEM images of mesoscopic crystals. Figure 5 It shows that the prepared ZrO 2 The particles are also rice-like mesoscopic crystals.

[0033] N 2 -Phy...

Embodiment 3

[0035] Dissolve 2.55 g of cetyltrimethylammonium bromide, 22.56 g of zirconium oxychloride octahydrate and 8.48 g of urea in 50 mL of deionized water to prepare a mixed solution, and calibrate the above mixed solution to 70 mL with deionized water Transfer to a high-temperature reactor with a volume of 100 mL (that is, the molar concentration of zirconium oxychloride octahydrate is 1 mol / L, and the molar ratio of zirconium oxychloride octahydrate to cetyltrimethylammonium bromide and urea is 1 :0.1:2). The reaction kettle was put into a blast drying oven, the reaction temperature was controlled at 200 °C, and the reaction time was 3 h. The obtained product was washed by centrifugation to remove impurity ions, and then dried at 60 °C for 8 h to obtain ZrO 2 mesoscopic crystals.

[0036] Figure 6 Is the ZrO prepared in this embodiment 2 SEM images of mesoscopic crystals. Figure 6 It shows that the prepared ZrO 2 The particles are also rice-like mesoscopic crystals.

[0...

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Abstract

The invention discloses a large specific surface porous ZrO2 mesoscopic crystal and its preparation method and application, and belongs to the field of metal oxide functional material preparation. In the present invention, cetyltrimethylammonium bromide, zirconium oxychloride octahydrate and urea are dissolved in water in proportion to form a mixed solution, and the ZrO2 mesoscopic material is prepared through hydrothermal reaction at 130-200°C for 3-48 hours. crystal. The preparation method of the invention is simple and easy to implement, has low cost, and has a high mesoscopic crystal yield; and the ZrO2 mesoscopic crystals produced have good monodispersity, are in the shape of rice grains, are porous internally, and have a BET specific surface area as high as 126~157 m2 / g, is an excellent water gas shift catalyst carrier.

Description

technical field [0001] The invention belongs to the field of preparation of metal oxide functional materials, in particular to a large specific surface porous ZrO 2 Mesoscopic crystals and their preparation methods and applications. Background technique [0002] ZrO 2 It is the only metal oxide that has four properties of surface acidity, surface alkalinity, oxidation and reduction at the same time. It is also a P-type semiconductor, and oxygen vacancies are easily generated inside and on the surface. Controlling different calcination temperatures can realize the transformation between monoclinic, tetragonal and cubic phases. At the same time, its surface is also rich in hydroxyl groups. These special properties make it widely used as a catalyst carrier, and even outperform the traditional SiO2 in many fields. 2 、Al 2 o 3 catalytic performance of the support. In addition, with ZrO 2 Catalysts made of supported transition metals have attracted more and more attention ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/06B01J35/10B01J37/10C01B3/16B01J32/00C01G25/02
CPCC01B3/16C01G25/02B01J21/066B01J37/10B01J35/615Y02P20/52
Inventor 张燕杰林棋娄本勇郑国才
Owner MINJIANG UNIV
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