Ti incorporation in MCM-41 mesoporous molecular sieves using hydrothermal synthesis

doi:10.1007/s11705-014-1405-2

Front Chem Sci Eng

2014, Vol. 8

Issue (1) : 95-103 https://doi.org/10.1007/s11705-014-1405-2

RESEARCH ARTICLE

Ti incorporation in MCM-41 mesoporous molecular sieves using hydrothermal synthesis

Shengping WANG¹(

), Changqing MA¹, Yun SHI^1,2, Xinbin MA¹

1. Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University; Collaborative Innovation Center of Chemical Science and Engineering, Tianjin 300072, China; 2. Patent Examination Cooperation Center of the Patent Office, SIPO, Beijing 100088, China

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Abstract

Titanium-containing mesoporous materials (Ti-MCM-41) were obtained by hydrothermal synthesis. Such materials are active catalysts for the transesterification of dimethyl oxalate and phenol to produce diphenyl oxalate. To understand the role of the Ti in the catalytic process, Ti-MCM-41 samples with different Si/Ti ratios (from 5 to 100) were prepared and the samples were analyzed by Fourier transform infrared spectroscopy, UV-visible spectroscopy, and ammonia temperature programmed desorption. It was concluded that the Ti is incorporated into the framework of the MCM-41 and formed weak Lewis acid sites. In addition, the number of Ti(IV) sites increased as the amount of titanium increased. X-ray powder diffraction, N₂ adsorption-desorption and transmission electron microscopy results showed that the Ti-MCM-41 samples have a hexagonal arrangement of mono-dimensional pores. A large number of Ti(IV) sites coupled with the mesoporous structure and large pore diameters are favorable for the transesterification catalytic properties of Ti-MCM-41.

Keywords Ti-MCM-41 mesoporous molecular sieve acid sites transesterification hydrothermal synthesis

Corresponding Author(s): WANG Shengping,Email:spwang@tju.edu.cn

Issue Date: 05 March 2014

Cite this article:

Shengping WANG,Changqing MA,Yun SHI, et al. Ti incorporation in MCM-41 mesoporous molecular sieves using hydrothermal synthesis[J]. Front Chem Sci Eng, 2014, 8(1): 95-103.

URL:

https://academic.hep.com.cn/fcse/EN/10.1007/s11705-014-1405-2
https://academic.hep.com.cn/fcse/EN/Y2014/V8/I1/95

Fig.1 Small-angle XRD patterns of MCM-41 and Ti-MCM-41 molecular sieves: (A) MCM-41, (B) Ti-MCM-41-100, (C) Ti-MCM-41-70, (D) Ti-MCM-41-50, (E) Ti-MCM-41-30, (F) Ti-MCM-41-10, and (G) Ti-MCM-41-5.

Tab.1 Textural properties of Ti-MCM-41 molecular sieves

Fig.2 Nitrogen adsorption-desorption isotherms (a) and pore size distribution curves (b) of Ti-MCM-41 molecular sieves: (A) Ti-MCM-41-100, (B) Ti-MCM-41-70, (C) Ti-MCM-41-50, (D) Ti-MCM-41-30, (E) Ti-MCM-41-10, and (F) Ti-MCM-41-5

Fig.3 TEM images of Ti-MCM-41molecular sieves: (a) and (b) Ti-MCM-41-5; (c) and (d) Ti-MCM-41-50; (e) and (f) Ti-MCM-41-100

Fig.4 FT-IR spectra of MCM-41 and Ti-MCM-41 molecular sieves: (A) MCM-41, (B) Ti-MCM-41-100, (C) Ti-MCM-41-70, (D) Ti-MCM-41-50, (E) Ti-MCM-41-30, (F) Ti-MCM-41-10, and (G) Ti-MCM-41-5

Fig.5 UV-visible diffuse re?ectance spectra of Ti-MCM-41 molecular sieves: (A) Ti-MCM-41-100, (B) Ti-MCM-41-70, (C) Ti-MCM-41-50, (D) Ti-MCM-41-30, (E) Ti-MCM-41-10, (F) Ti-MCM-41-5, and (G) TiO

Fig.6 FTIR spectra of pyridine adsorbed on Ti-MCM-41 molecular sieves: (A) Ti-MCM-41-100, (B) Ti-MCM-41-70, (C) Ti-MCM-41-50, (D) Ti-MCM-41-30, (E) Ti-MCM-41-10, and (F) Ti-MCM-41-5

Fig.7 NH-TPD profiles of Ti-MCM-41 molecular sieves: (A) Ti-MCM-41-100, (B) Ti-MCM-41-70, (C) Ti-MCM-41-50, (D) Ti-MCM-41-30, (E) Ti-MCM-41-10, and (F) Ti-MCM-41-5

Tab.2 Catalytic activities of Ti-MCM-41 molecular sieves for the transesterification of dimethyl oxalate with phenol

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