Synthesis and Structural Characterization of a Series of Group 11 2,2-Dialkyl-1,3-dicyclohexylguanidinate Complexes

2014 ◽  
Vol 67 (7) ◽  
pp. 1021 ◽  
Author(s):  
Sonya K. Adas ◽  
Jesus A. Ocana ◽  
Scott D. Bunge

The addition of either lithium dimethylamide or lithium diethylamide to a tetrahydrofuran (THF) solution of 1,3-dicyclohexylcarbodiimide yielded THF adducts of lithium 2,2-dimethyl-1,3-dicyclohexylguandidinate (1) and lithium 2,2-diethyl-1,3-dicyclohexylguandidinate (2), respectively. One equivalent of either 1 or 2 was subsequently reacted with one equivalent of Group 11 halide (CuCl, AgBr, and AuCl) to generate oligonuclear complexes with the general formula {M[CyNC(NR2)NCy]}n where M, R, and n are respectively Cu, CH3, 2 (3); Cu, CH2CH3, 2 (4); Ag, CH3, 3 (5); Ag, CH2CH3, 3 (6); Au, CH3, 2 (7); and Au, CH2CH3, 2 (8). Compounds 1–8 were characterized by single-crystal X-ray diffraction. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, Fourier transform infrared spectroscopy, and 1H, 13C, and 7Li NMR studies. The unique structural aspects of this family of Group 11 complexes are highlighted.

2003 ◽  
Vol 18 (2) ◽  
pp. 482-486 ◽  
Author(s):  
Guangming Chen ◽  
Nobuo Iyi ◽  
Taketoshi Fujita

New noncovalent bonding polymer/clay hybrids were prepared, including the polymer poly(tetramethyl-p-phenylenediamine) (poly-TMPD). Polymerization occurred in the interlayer space of clay mineral successively after intercalation of monomers. Two types of clay minerals with different surface properties—a hydrophilic lithium fluorotaeniolite (TN) and four kinds of organophilic fluorotaeniolites (org-TNs)—were used as the hosts. Powder x-ray diffraction results showed an increase of 0.7–1.0 nm in the basal spacings, indicating the formation of poly–TMPD in the interlayer space of the hosts. Intercalative polymerization was also supported by Fourier transform infrared spectroscopy. The orientation of the poly-TMPD and thermal behavior were also discussed.


2012 ◽  
Vol 548 ◽  
pp. 77-81
Author(s):  
Jia Hua Ma ◽  
Cheng Jia Tan ◽  
Xia Deng ◽  
Chao Xin

Preparation techniques of chitosan from Catharsius molossus L. processing discards were studied by orthogonal design. Preparation techniques were as follows:demineralizing: soaked for 30 min at 80 °C with 1.3 mol•L-1 HCl, then kept for 12 h under room temperature. Deproteinization and delipidation: treated for 6 h at 90 °C with 4 mol•L-1 NaOH. Decolorizing: soaked at room temperature with 3% KMnO4, then treated with 2% oxalic acid at 70 °C. Deacetylation: treated for 6 h at 110 °Cwith 14 mol•L-1 NaOH. Properties of chitosan were characterized by Fourier transform infrared spectroscopy(FTIR), X-ray diffraction (XRD), etc. It proved the technique was stable and feasible. The result also preliminarily showed that chitosan from Catharsius molossus L. was better than shrimp’s. It will be widely applicated in biomedical and other industrial areas with such exiciting properties.


2021 ◽  
Vol 12 (1) ◽  
pp. 53-64
Author(s):  
Zilfa Zilfa ◽  
Safni Safni ◽  
Febi Rahmi

An investigation on modification of natural zeolite with ZnO for the degradation of tartrazine. In this study, ZnO as a semiconductor is modified into a natural zeolite as support to form ZnO/zeolite that can increase the efficiency degradation of tartrazine. Further, the formed catalyst was added to tartrazine by determining the variation in ozonolysis time, the amount of addition of the catalyst, and the addition of a catalyst time. The results of degradation were determined by UV-Vis spectrophotometer at 424 nm. The result showed that the percentage of degradation obtained on each catalyst in the degradation. The resulted percent degradation of 20 ml of tartrazine at concentration of 15 mg/L using 20 mg ZnO/zeolite was 56.80%, while using 0.77 mg ZnO was 42.25%, and with the addition of 19.23 mg of Zeolite was 31.18%, all of that condition was proceeded by 40 minutes of ozonolysis. Thus, the result indicates that the ZnO/zeolite catalyst can increase percentages of tartrazine degradation by ozonolysis. It is known that the catalyst ZnO/zeolite is very effective in increasing the degradation of tartrazine. Analysis of tartrazine compounds using fourier-transform infrared spectroscopy (FTIR) after degradation changes in wavenumber indicates that there is a breaking of the bonds of tartrazine compounds. Characterization of ZnO/zeolite catalyst using FTIR, X-Ray diffraction (XRD) and scanning electron microscope (SEM), in each spectrum there was no shift, indicating that there is no change in ZnO/zeolite structure


2015 ◽  
Vol 70 (3) ◽  
pp. 165-169 ◽  
Author(s):  
Gao-Feng Wang

AbstractThe synthesis of two new copper(II) complexes with benzimidazole type ligands, Cu(tta)2(L1)2 (1) and Cu(tta)2(L1) (2) (where L1 is 3-(4-(1H-benzo[d]imidazol-1-yl)-4-methoxy phenyl)-1-phenylprop-2-en-1-one; tta is 2-thenoyltrifluoroacetonate), are reported. Their structures have been characterized by infrared spectroscopy, elemental analyses and single-crystal X-ray diffraction. The copper(II) ion of 1 is in a distorted octahedral environment, while that of 2 is in a distorted square-pyramidal environment. In both cases, the donor atoms are provided by oxygen atoms of the tta ligands and nitrogen atoms of the L1 ligands.


2014 ◽  
Vol 556-562 ◽  
pp. 109-112
Author(s):  
Shu Min Zheng ◽  
Kai Ming Wang

Lizardite were synthesized by hydrothermal reaction in an Fe3+doped solution/environment using nanometer SiO2and MgO as precursors. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), fourier transform infrared spectroscopy (FTIR). The results show that: the synthetic samples are lizardite with a thickness ranging from 60 nm to 200 nm in the temperature range 200°C~230°C.


2019 ◽  
Vol 958 ◽  
pp. 47-51
Author(s):  
Suellen Signer Bartolomei ◽  
Helio Wiebeck

This work aims to characterize the post-consumption plaster and compare it with virgin plaster. Burrs from plaster frames manufacturing were collected at the manufacturer. These samples were dried in a drying oven. Then, they were milled in a ball mill, until forming a fine and homogeneous powder. The samples were returned to the drying oven at three different temperatures, 100, 150 and 200°C, to define the best drying temperature, because the water removed in this process changes the structure of the semi-hydrated calcium sulfate gypsum into bihydrated. Then, vibrational Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) were performed to characterize the virgin plaster and the reused plaster, making it possible to know the structure and the groups present in the components.


2019 ◽  
Vol >15 (5) ◽  
pp. 512-524 ◽  
Author(s):  
Alexandros K. Nikolaidis ◽  
Elisabeth A. Koulaouzidou ◽  
Dimitris S. Achilias

Background: Nanoclays incorporated in dental resins have been previously investigated. However, limited reports are associated with nanoclays that exhibit high functionality. Objective: The aim of this study was the targeted synthesis and characterization of organomodified nanoclays with methacrylic groups suitable for incorporation in dental nanocomposite resins. Methods: Quaternary ammonium methacrylates were synthesized and characterized by means of proton nuclear magnetic resonance and Fourier-transform infrared spectroscopy. Consequently, they were inserted into the interlayer space of nanoclay through a cation exchange reaction, while silane was also used for simultaneous surface modification. The produced organomodified nanoclays were characterized by means of X-ray diffraction, Fourier-transform infrared spectroscopy and thermogravimetric analysis. Results: Fourier-transform infrared spectra confirmed the successful synthesis of the quaternary ammonium methacrylates. X-ray diffraction analysis showed that organoclays exhibited higher d001- values (up to 1.78 nm) compared to raw nanoclay (1.37 nm), indicating an accomplished intercalation in each case. X-ray diffraction spectra mainly disclosed the presence of methacrylic functional groups in all nanoclays. Thermogravimetric analysis curves verified the different thermal stability of organoclays due to the diversity of their organic modifiers. Conclusion: The experimental results showed that nanoclay was successfully modified with ammonium methacrylates and silane. Τhe combination of X-ray diffraction and thermogravimetric analysis data revealed a high degree of intercalation and methacrylated organic loading as well. These phenomena may favor a good dispersion and high polymerization degree of nanoclays with dental resin monomers, rendering them potentially useful materials for the development of advanced dental nanocomposites resins.


2020 ◽  
Vol 6 (3) ◽  
pp. 905-907
Author(s):  
S.S. Gautam ◽  
G.P. Satsangi ◽  
V.R. Satsangi

This research work is attempted to synthesize, functionalize and to characterize multi walled carbon nanotubes (MWCNTs). The synthesis of multi walled carbon nanotubes was done by chemical vapor deposition (CVD) method. The characterization of MWCNTs was done by adopting the following techniques such as field emission scanning electron microscope, X-ray diffraction, Fourier-transform infrared spectroscopy. The crystalline quality of MWCNTs was confirmed from the analysis of X-ray diffraction pattern. FE-SEM image obtained for MWCNTs and functionalized MWCNTs and it has been seen that dimeter of most of the MWCNTs lies around 90 nm, where as, functionalized MWCNTs diameter is smaller i.e., around 35 nm only. Fourier-transform infrared spectroscopy study confirmed the presence of –COOH and H- bonded –OH in functionalized MWCNTs.


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