scholarly journals Carboxylated dithiafulvenes and tetrathiafulvalene vinylogues: synthesis, electronic properties, and complexation with zinc ions

2015 ◽  
Vol 11 ◽  
pp. 957-965 ◽  
Author(s):  
Yunfei Wang ◽  
Yuming Zhao

A class of carboxyl and carboxylate ester-substituted dithiafulvene (DTF) derivatives and tetrathiafulvalene vinylogues (TTFVs) has been synthesized and their electronic and electrochemical redox properties were characterized by UV–vis spectroscopic and cyclic voltammetric analyses. The carboxyl-TTFV was applied as a redox-active ligand to complex with Zn(II) ions, forming a stable Zn-TTFV coordination polymer. The structural, electrochemical, and thermal properties of the coordination polymer were investigated by infrared spectroscopy, cyclic voltammetry, powder X-ray diffraction, and differential scanning calorimetric analyses. Furthermore, the microscopic porosity and surface area of the Zn-TTFV coordination polymer were measured by nitrogen gas adsorption analysis, showing a BET surface of 148.2 m2 g−1 and an average pore diameter of 10.2 nm.

NANO ◽  
2020 ◽  
Vol 15 (02) ◽  
pp. 2050017
Author(s):  
Ke-Cheng Yang ◽  
Li-Hui Xu ◽  
Hong Pan ◽  
Li-Ming Wang ◽  
Yong Shen ◽  
...  

In this study, CuS/SiO2 composite modified aerogel was prepared by the incorporation of hollow spherical CuS into methyltrimethoxysilane-based SiO2 sol and modification with hexadecafluorodecyltriethoxysilane via acid-base catalyzed sol–gel reaction and drying under ambient pressure. The CuS/SiO2 composite modified aerogel was characterized by Fourier-transform infrared (FT-IR) spectrometry, scanning electron microscope (SEM), nitrogen gas adsorption and desorption and X-ray diffraction (XRD), respectively. The effects of CuS and fluorosilane concentration on density and porosity of aerogel, oleophobic and photocatalytic properties were evaluated. The results showed that structure and physical properties of aerogel had some effect by introducing CuS and fluorosilane, and the CuS/SiO2 composite modified aerogel with density of 0.146[Formula: see text]g/cm3 and specific surface area of 241[Formula: see text]m2/g achieved super-oleophobicity with oil contact angle of 152.8∘ and sliding angle of 10∘, and good photocatalytic properties for methylene blue.


2013 ◽  
Vol 575-576 ◽  
pp. 30-36 ◽  
Author(s):  
Ning Ning Wu ◽  
Can Xiong Guo ◽  
Gui An Wu ◽  
Zhao Cai ◽  
Wan Hong He

A novel one-dimensional metal-organic coordination polymer, [Zn (NH3)2(BDC)]n (BDC=1,4-benzenedicaboxylate), has been synthesized by solvent evaporation method through self-assembly of Zn (II) salts with terephthalic acid ligand in ammonia aqueous solution. Single crystal X-ray diffraction analysis indicated that each Zn (II) was coordinated by two nitrogen donors from two NH3 and two oxygen counter donors from terephthalic acid ligand. The adjacent zigzag chains are arranged in a parallel fashion and linked by interchain hydrogen bonding interaction and π-π stacking interactions into higher-dimensional framework. The compound has also been characterized by CHN elemental analyses, Single crystal X-ray diffraction analysis, powder X-ray diffraction (PXRD) analysis, Fourier transform infrared (FT-IR) spectra, Thermalgravimetric-differential scanning calorimetric (TG-DSC) and Solid-state nuclear magnetic resonance (NMR), etc. Results showed that the framework of compound was stable at the temperature up to 246°C. The desolvated product [Zn (BDC)]n, which was obtained by removal of molecular NH3 from [Zn (NH3)2(BDC)]n, can be transferred to the different skeleton structures through coordinating different small hydrogen-bond-forming molecules.


2021 ◽  
Vol 47 (5) ◽  
pp. 307-318
Author(s):  
I. N. Meshcheryakova ◽  
O. Yu. Trofimova ◽  
N. O. Druzhkov ◽  
K. I. Pashanova ◽  
I. A. Yakushev ◽  
...  

Abstract Poorly soluble in the most part of organic solvents dimeric complexes $${\text{M}}{{{\text{g}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$·4DMF (I) and $${\text{N}}{{{\text{i}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$·4DMF (II) (L is 4,4'-(1,4-phenylenebis(azanylylidene))bis(3,6-di-tert-butyl-2-hydroxycyclohexa-2,5-dien-1-one dianion)) are synthesized by the reactions of magnesium and nickel acetates with the ditopic redox-active ligand of the hydroxy-para-iminoquinone type in a DMF solution. The molecular and crystal structures of the synthesized compounds are determined by X-ray diffraction analysis (CIF files CCDC nos. 2045665 (I) and 2045666 (II·3DMF)). The thermal stability is studied by thermogravimetry. The redox-active character of the organic bridging ligand in the dimeric complexes $${\text{M}}{{{\text{g}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$·4DMF and $${\text{N}}{{{\text{i}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$·4DMF is confirmed by the data of solid-phase electrochemistry.


2014 ◽  
Vol 14 (3) ◽  
pp. 253-261
Author(s):  
Tutik Setianingsih ◽  
Indriana Kartini ◽  
Yateman Arryanto

Mesoporous carbon was prepared from fructose using zinc borosilicate (ZBS) activator. The synthesis involves caramelization and carbonization processes. The effect of both process temperature toward porosity and functional group of carbon surface are investigated in this research. The caramelization was conducted hydrothermally at 85 and 100 °C, followed by thermally 130 °C. The carbonization was conducted at various temperatures (450–750 °C). The carbon-ZBS composite were washed by using HF 48% solution, 1M HCl solution, and aquadest respectively to remove ZBS from the carbon. The carbon products were characterized with nitrogen gas adsorption-desorption method, FTIR spectrophotometry, X-ray diffraction, and Transmission Electron Microscopy. The highest mesopore characteristics is achieved at 100 °C (caramelization) and 450 °C (carbonization), including Vmeso about 2.21 cm3/g (pore cage) and 2.32 cm3/g (pore window) with pore uniformity centered at 300 Å (pore cage) and 200 Å (pore window), containing the surface functional groups of C=O and OH, degree of graphitization about 57% and aromaticity fraction about 0.68.


2021 ◽  
Author(s):  
ALI NEMATI KHARAT ◽  
Mehrnaz Aliahmadi

Abstract Cerium dioxide nanoparticles were prepared by the sol-gel method using cellulose as a template and used in the synthesis of 2-oxazolidinone from urea and 2-aminoethanol under solvent-free conditions. All the reaction parameters were optimized to obtain the best selectivity and conversion. The selectivity of 100 % to 2-oxazolidinone with a pretty complete conversion of about 98.4 % was achieved. The prepared catalyst was characterized by Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), and volumetric isothermal nitrogen gas adsorption-desorption method (BET).


2015 ◽  
Vol 670 ◽  
pp. 3-8 ◽  
Author(s):  
Valentina V. Smirnova ◽  
Alexander P. Ilyin ◽  
Anton S. Brichkov ◽  
Anastasiya V. Zabolotskaya

This article deals with the study of direct current (DC), ultrasonic, and of electrolyte of the influence on the change of titanium dioxide sorption properties. The TiO2 prepared by the TiCl4 hydrolysis method. Attention is drawn to charging exchange processes the surface of titanium dioxide particles after they pass through a layer of counter ions in an aqueous medium under the influence of a DC. The stages of the end product’s formation using methods of the X-ray diffraction, the differential thermal and the infrared spectrometric and the gas adsorption analysis were proposed. Dependence of redistribution sorption active centers at the surface of TiO2 was proved.


2011 ◽  
Vol 11 (3) ◽  
pp. 207-211 ◽  
Author(s):  
Emi Shaqiza Azizi ◽  
Mohd Noor Ahmad ◽  
A.K.M. Shafiqul Islam ◽  
Dahyar Arbain ◽  
Iqmal Tahir

Molecularly imprinted polymer (MIP) is gaining importance in separation technology. In this study, curcumin has been selected as template in MIP which can be applied as sorbent materials in solid-phase extraction (SPE). Effect of porogen on the quality of curcumin-MIP is very sensitive depends on the molecular size and polarity of the porogen. We varied three solvents as the porogen i.e. tetrahydrofuran (THF), chloroform (CHCl3) and acetonitrile (MeCN). The MIP was prepared using non-covalent approach through bulk polymerization and non-imprinted polymer (NIP) as control, also prepared using the same procedure in the absence of template. The largest imprinting factor, 1.27 was obtained from polymer P1 at ratio 1:4 of template: functional monomer. The P1 was prepared using methacrylic acid (MAA) as functional monomer and tetrahydrofuran (THF) as porogen with the highest average pore diameter i.e. 618.43 nm trough gas adsorption analysis. This will lead to better access of curcumin during batch binding analysis.


1994 ◽  
Vol 346 ◽  
Author(s):  
A.W. Reid ◽  
B. Rand ◽  
R.J.P. Emsley

ABSTRACTIt is shown that ceramics derived from polycarbosilane polymers may develop an open nanoporous network after heat treatment to a temperatures between 1300 and 1550°C in argon. The resulting SiC-based ceramics were characterised by N2 gas adsorption analysis and X-ray diffraction. The apparent surface area, and pore volume increase with increasing heat treatment temperature, reaching values of 170 m2g-1 and 0.12 cm3-1 respectively. The pore network develops as the SiC crystals grow and as carbon is ejected from the structure. It is thought that the porosity may reside within the carbon phase, but this remains to be confirmed.


2018 ◽  
Author(s):  
Jaya Prakash Madda ◽  
Pilli Govindaiah ◽  
Sushant Kumar Jena ◽  
Sabbhavat Krishna ◽  
Rupak Kishor

<p>Covalent organic Imine polymers with intrinsic meso-porosity were synthesized by condensation reaction between 4,4-diamino diphenyl methane and (para/meta/ortho)-phthaladehyde. Even though these polymers were synthesized from precursors of bis-bis covalent link mode, the bulk materials were micrometer size particles with intrinsic mesoporous enables nitrogen as well as carbon dioxide adsorption in the void spaces. These polymers were showed stability up to 260<sup>o</sup> centigrade. Nitrogen gas adsorption capacity up to 250 cc/g in the ambient pressure was observed with type III adsorption characteristic nature. Carbon dioxide adsorption experiments reveal the possible terminal amine functional group to carbamate with CO<sub>2</sub> gas molecule to the polymers. One of the imine polymers, COP-3 showed more carbon dioxide sorption capacity and isosteric heat of adsorption (Q<sub>st</sub>) than COP-1 and COP-2 at 273 K even though COP-3 had lower porosity for nitrogen gas than COP-1 and COP-2. We explained the trends in gas adsorption capacities and Qst values as a consequence of the intra molecular interactions confirmed by Density Functional Theory computational experiments on small molecular fragments.</p>


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Xinzhao Xia ◽  
Lixian Xia ◽  
Geng Zhang ◽  
Yuxuan Jiang ◽  
Fugang Sun ◽  
...  

Abstract In this work, a new type of zinc(II) coordination polymer {[Zn(HIDC)(BBM)0.5]·H2O} n (Zn-CP) was synthesized using 4,5-imidazoledicarboxylic acid (H3IDC) and 2,2-(1,4-butanediyl)bis-1,3-benzimidazole (BBM) under hydrothermal conditions. Its structure has been characterized by infrared spectroscopy, elemental analysis and single crystal X-ray diffraction analysis. The Zn(II) ion is linked by the HIDC2− ligand to form a zigzag chain by chelating and bridging, and then linked by BBM to form a layered network structure. Adjacent layers are further connected by hydrogen bond interaction to form a 3-D supramolecular framework. The solid-state fluorescence performance of Zn-CP shows that compared with free H3IDC ligand, its fluorescence intensity is significantly enhanced.


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