Copper tellurolate clusters in trimethylsilylated MCM-41 — Preparation and condensation

2006 ◽  
Vol 84 (2) ◽  
pp. 196-204 ◽  
Author(s):  
Collin M Kowalchuk ◽  
Harald Rösner ◽  
Dieter Fenske ◽  
Yining Huang ◽  
John F Corrigan
Keyword(s):  
Nmr Spectroscopy ◽  
Sorption Isotherms ◽  
Nitrogen Adsorption ◽  
Mas Nmr ◽  
Condensation Process ◽  
X Ray ◽  
Edx Analysis ◽  
Transmission Electron ◽  
Cp Mas Nmr ◽  
Mcm 41

The copper tellurolate cluster [(Cu6(TePh)6(PEtPh2)5] (1) has been loaded into the pores of a trimethylsilylated MCM-41 (TMS–MCM-41) framework. Solutions of 1 in tetrahydrofuran lead to good impregnation weight % (~10 wt%, 1). The resulting material was analysed by powder X-ray diffraction (PXRD), nitrogen sorption isotherms, thermogravimetric analysis (TGA), energy dispersive X-ray (EDX) analysis, 31P CP MAS NMR spectroscopy, and transmission electron microscopy (TEM). It was observed that the loading process proceeds with the intact cluster 1 being present within the hexagonal architecture. The intact nature of 1 makes it an ideal candidate for condensation by photochemical or thermal means. Both of these condensation treatments increase the Cu:Te ratio of 1 to approach that observed in binary semiconductor Cu2Te. The condensation process was analysed by GC–MS spectrometry and characterization of the condensed, isolated composites was performed by TGA, EDX analysis, 31P CP MAS NMR spectroscopy, nitrogen adsorption, and TEM measurements. Thermal condensation results in the formation of Cu2Te particles, whereas photochemical condensation yields larger copper-tellurolate nanoclusters.Key words: copper, tellurium, cluster, MCM-41, trimethylsilylated, photolysis, thermolysis, Cu2Te, composite, mesoporous material.

Synthesis and Characterization of Mesoporous Molecular Sieve Al-MCM-41 Using Kaolin as Raw Material

2013 ◽  
Vol 779-780 ◽  
pp. 201-204
Author(s):  
Miao Li ◽  
Hong Wang ◽  
Xian Qing Li ◽  
Jin Rong Liu
Keyword(s):  
Molecular Sieve ◽  
Nitrogen Adsorption ◽  
Mesoporous Molecular Sieve ◽  
Raw Material ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Adsorption Desorption ◽  
Calcined Kaolin ◽  
Mcm 41

Ordered hexagonally mesoporous molecular sieve Al-MCM-41 with Si/Al (atom) ratio=9 was prepared by hydrothermal synthesis using raw kaolin. X-ray diffraction (XRD), Nitrogen adsorption desorption, Transmission Electron Microscope (TEM) and Energy Dispersive X-ray Detector (EDX) were employed to characterise raw kaolin, calcined kaolin, as-synthesized and calcined Al-MCM-41. The results indicated that characteristic reflections of raw kaolin disappeared after calcination, both of as-synthesized and calcined Al-MCM-41 exhibited well ordered hexagonally mesoporous molecular sieve structure.

Studies of the series of cellooligosaccharide peracetates as a model for cellulose triacetate by 13C CP/MAS NMR spectroscopy and X-ray analyses

1999 ◽  
Vol 322 (3-4) ◽  
pp. 256-263 ◽  
Author(s):  
Hiroyuki Kono ◽  
Yukari Numata ◽  
Nobuhiro Nagai ◽  
Tomoki Erata ◽  
Mitsuo Takai
Keyword(s):  
Nmr Spectroscopy ◽  
Cellulose Triacetate ◽  
Mas Nmr ◽  
X Ray ◽  
Cp Mas Nmr ◽  
13C Cp Mas Nmr

Textural features of highly ordered Al-MCM-41 molecular sieve studied by X-ray diffraction, nitrogen adsorption and transmission electron microscopy

2006 ◽  
Vol 60 (21-22) ◽  
pp. 2682-2685 ◽  
Author(s):  
Marcelo J.B. Souza ◽  
Antonio S. Araujo ◽  
Anne M.G. Pedrosa ◽  
Bojan A. Marinkovic ◽  
Paula M. Jardim ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Molecular Sieve ◽  
Nitrogen Adsorption ◽  
Textural Features ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Mcm 41

Combination of CP/MAS NMR Spectroscopy and X-ray Crystallography:  Structure and Dynamics in Molecular Crystals of Hydrogen, Lithium, Sodium, Rubidium, and Cesium Penicillin V

1997 ◽  
Vol 119 (41) ◽  
pp. 9793-9803 ◽  
Author(s):  
Michaela Wendeler ◽  
Jamila Fattah ◽  
J. Mark Twyman ◽  
Alison J. Edwards ◽  
Christopher M. Dobson ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Molecular Crystals ◽  
Mas Nmr ◽  
X Ray ◽  
X Ray Crystallography ◽  
Structure And Dynamics ◽  
Penicillin V ◽  
Cp Mas Nmr

scholarly journals Mineralogical characterization and preliminary assessment of the hydrocarbon potential of sedimentary rock from the western part of the Central Kongo

2018 ◽  
Vol 7 (2) ◽  
pp. 93-104 ◽  
Author(s):  
Rajae Bouamoud ◽  
Adnane El Hamidi ◽  
Mohammed Halim ◽  
Raphael Mulongo Masamba ◽  
Roger Antoine Kobo Nlandu ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Sedimentary Rock ◽  
Mas Nmr ◽  
Mineralogical Characterization ◽  
Petroleum Potential ◽  
X Ray ◽  
Oil Shales ◽  
Rock Eval ◽  
Cp Mas Nmr ◽  
13C Cp Mas Nmr

In this work, the mineralogical characteristics and the assessment of the petroleum potential of organic carbon-rich sedimentary rock (CK sample) originating from the western part of the Central Kongo were the subject of a preliminary analysis and the results were compared with those of Moroccan oil shales. The mineralogical characterization was carried out using X-Ray Diffraction (XRD), X-Ray Fluorescence (XRF), Fourier Transform Infra-Red (FTIR) spectroscopy, Thermal Gravimetry/Differential Thermal Analysis (TG/DTA) and Scanning Electronic Microscopy (SEM-EDX). The results show that the examined sedimentary rock contain a significant part of minerals, about 80%, consisting of quartz, clays and pyrite, similar to those frequently found in oil shales. The pyrolysis also indicates the presence of volatile matter between 250 and 580°C, attributed to the Organic Matter (OM) disseminated within the sedimentary rock as was shown in several carbon-rich materials. The detection of pyrite in the CK sample reveals the existence of a reducing environment during the preservation period of OM in the source rock. The assessment of the petroleum potential using the basic Rock-Eval method associated with the elemental analysis and 13C Cross Polarization/Magic Angle Spinning Nuclear Magnetic Resonance (13C CP/MAS NMR) spectroscopy indicated a very good organic richness (TOC=10.77%), very good petroleum potential (S2=80.4 mgHC/g rock) with the sapropelic OM described as type I kerogen (H/C molar ratio of 1.71) characterized by high hydrogen index (HI=746 mgHC/g TOC) and low oxygen index (OI=13 mgCO2/g TOC) values. The Rock-Eval results were confirmed by 13C CP/MAS NMR spectroscopy which shows the exclusive presence of aliphatics. The mineralogical and petroleum characteristics of CK sample show a great resemblance with those of known oil shales such as Moroccan oil shales and its kerogen is probably related to a marine or lacustrine environment which formed in anoxic sedimentary rocks and with a thermal evolution that has just reached the early stage of the oil window

Synthesis and structures of monomeric group 14 triols and their reactivity

2014 ◽  
Vol 92 (6) ◽  
pp. 542-548 ◽  
Author(s):  
Lucian-Cristian Pop ◽  
Nobuaki Kurokawa ◽  
Hiroaki Ebata ◽  
Katsuya Tomizawa ◽  
Tomoyuki Tajima ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
Crystalline State ◽  
Mas Nmr ◽  
X Ray Diffraction ◽  
Group 14 ◽  
Silicone Grease ◽  
X Ray ◽  
Hydrolysis Of ◽  
Cp Mas Nmr

The first stable stannanetriol and germanetriol bearing sterically congested aryl groups were synthesized by hydrolysis of the corresponding trichloro-stannane and -germane. The stannanetriol is monomeric in solution as well as in the crystalline state, as evidenced by X-ray diffraction analysis and CP-MAS NMR spectroscopy. The stannanetriol reacted with silicone grease to afford a cagelike compound having three Sn–O–Si–O–Sn linkages in the molecule. All the group 14 triols can be converted to the corresponding trihalo compounds in good yields.

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