a mesoporous so 4 2‑ /zro 2 preparation method

A mesoporous, zirconium-based technology is applied in the field of preparation of mesoporous SO42-/ZrO2, which can solve the problems of loss of loaded sulfur species, poor thermal stability of the carrier, easy collapse of the pore structure, etc., and achieves a simple and easy preparation method and improves stability. The effect of the uniform and uniform mesoporous structure

Active Publication Date: 2017-11-28
TAIYUAN UNIV OF TECH
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Problems solved by technology

Mesoporous ZrO 2 The preparation of can be obtained through the synthetic route of soft template or hard template [A. Sinhamahapatra, N. Sutradhara, M. Ghoshb, H. C.Bajaj and A. B. Panda, Appl. Catal. A, 2011, 402, 87-93; J. L. Shi, Chem .Rev., 2013, 113, 2139-2181], but these methods are not only complicated to operate, but also the prepared ZrO 2 The thermal stability of the carrier is poor, and its pore structure is easy to collapse during the process of removing the template or vulcanization and roasting
In response to these problems, people use mesoporous silicon-based materials with high specific surface area and regular nanopore structure as scaffolds, and use methods such as impregnation, precipitation, or steam-induced hydrolysis to synthesize ZrO 2 coatings on these materials [A. Osatiashtiani, A. F. Lee, M. Granollers, D. R. Brown, L. Olivi, G. Morales, J. A. Melero and K. Wilson, ACS Catal, 2015, 5, 4345-4352; M. A. Ecormier, A. F. Lee and K. Wilson, Micropor.Mesopor. Mater. 2005, 80, 301−310.], but this method is not only complicated to operate, but also needs to adopt multiple methods to fine-tune the coating process to avoid ZrO 2 uneven distribution of and clogged stent channels
[0005] Also, on SO 4 2- / ZrO 2 Another important problem in the process of using is the loss of loaded sulfur species in the reaction process

Method used

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  • a mesoporous so <sub>4</sub> <sup>2‑</sup> /zro <sub>2</sub> preparation method
  • a mesoporous so <sub>4</sub> <sup>2‑</sup> /zro <sub>2</sub> preparation method
  • a mesoporous so <sub>4</sub> <sup>2‑</sup> /zro <sub>2</sub> preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 25mmol ZrCl 4 , 25mmol terephthalic acid, 25mmol concentrated HCl, 5mL 1mol / L H 2 SO 4 Add the solution together to 150mL N,N-dimethylformamide and stir evenly, put it into a 200mL stainless steel reaction kettle with a polytetrafluoroethylene liner, conduct a crystallization reaction at 160°C for 3 days, and take out the obtained white powder. Vacuum drying at 150°C yielded sulfur-containing zirconium-based MOFs material UiO-66-S.

[0025] Put UiO-66-S in a muffle furnace, heat up to 500 °C at a rate of 2 °C / min, and bake for 6 h to obtain mesoporous SO 4 2- / ZrO 2 .

[0026] The prepared samples were characterized by XRD. figure 1 (a) It can be seen that the as-prepared sulfur-containing zirconium-based MOFs material UiO-66-S shows the same properties as UiO-66 reported in the literature [J.H. Cavka, S. Jakobsen, U. Olsbye, N. Guillou, C.Lamberti, S. Bordiga, K.P. Lillerud, J. Am. Chem. Soc. 2008.130. 13850-13851] consistent with the characteristic diffrac...

Embodiment 2

[0030] Take 25mmol ZrCl 4 , 25mmol terephthalic acid, 25mmol concentrated HCl, 5mmol (NH 4 ) 2 SO 4 , added together to 150mL N,N-dimethylformamide and stirred evenly, put into a 200mL stainless steel reaction kettle with a polytetrafluoroethylene liner, crystallize at 160°C for 6 days, take out the obtained white powder, 150 ℃ vacuum drying to obtain the sulfur-containing zirconium-based MOFs material UiO-66-S.

[0031] Put UiO-66-S in a muffle furnace, heat up to 500 °C at a rate of 2 °C / min, and bake for 6 h to obtain mesoporous SO 4 2- / ZrO 2 .

Embodiment 3

[0033] Take 0.227mmol ZrCl 4 , 0.227mmol terephthalic acid, 0.1mL 0.5mol / L H 2 SO 4 Add the solution together to 340mmol N,N-dimethylformamide and stir evenly, put it into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene liner, conduct a crystallization reaction at 200°C for 5 days, and take out the obtained white powder. Vacuum drying at 150°C yielded sulfur-containing zirconium-based MOFs material UiO-66-S.

[0034] Put UiO-66-S in a muffle furnace, heat up to 600 °C at a rate of 2 °C / min, and bake for 6 h to obtain mesoporous SO 4 2- / ZrO 2 .

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Abstract

The invention discloses a preparation method of mesoporous SO4<2-> / ZrO2. According to the preparation method, in-suit introduction of a sulfur-containing compound into a synthesis system of a zirconium-based MOFs material is carried out, and the sulfur-containing zirconium-based MOFs material is roasted in an oxygen-containing atmosphere at a certain temperature to prepare mesoporous SO4<2-> / ZrO2. The preparation method is simple and convenient; the prepared mesoporous SO4<2-> / ZrO2 possesses a uniform mesoporous structure, large specific surface, and specific morphology characteristics; and stability of loaded sulfur obtained via the preparation method is high, leaching is not easily caused, and the preparation method is an effective method used for preparing mesoporous SO4<2-> / ZrO2.

Description

technical field [0001] The present invention relates to mesoporous SO 4 2- / ZrO 2 The preparation method, especially involving the introduction of sulfur-containing compounds in the synthesis system of zirconium-based MOFs materials, and the preparation of mesoporous SO with sulfur-containing zirconium-based MOFs materials 4 2- / ZrO 2 Methods. Background technique [0002] SO 4 2- / ZrO 2 It is a potential heterogeneous solid acid catalyst, because of its high acid strength and the synergistic effect of acid centers (Bronsted acid and Lewis acid), it can be used in esterification reaction, etherification reaction, hydration-dehydration reaction, cracking reaction and hydrocracking and other chemical reactions [B. M. Reddy and M. K. Patil, Chem. Rev., 2009, 109, 2185–2208; G. D. Yadav and J. J. Nair, Micropor. Mesopor. Mater., 1999, 33 , 1-48]. [0003] SO 4 2- / ZrO 2 The preparation of ZrO usually adopts the following method: first, the precipitation method is us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/02
Inventor 范彬彬路宁悦闫晓亮吕文苗李瑞丰
Owner TAIYUAN UNIV OF TECH
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