Synthesis and characterization of periphery-functionalized porphyrazines containing mixed pyrrolyl and pyridylmethylamino groups

2009 ◽  
Vol 13 (02) ◽  
pp. 223-234 ◽  
Author(s):  
Tomasz Goslinski ◽  
Ewa Tykarska ◽  
Wojciech Szczolko ◽  
Tomasz Osmalek ◽  
Aleksandra Smigielska ◽  
...  
Keyword(s):  
Electrochemical Properties ◽  
Chemical Sensors ◽  
Electronic Materials ◽  
Condensation Reaction ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Coordination Properties ◽  
Perpendicular Orientation ◽  
Selective Sensor

The condensation reaction of 2-amino-3-[(3-pyridylmethyl)amino]-2(Z)-butene-1,4-dinitrile with a series of diketones led to novel dinitriles, of which 2-(2,5-dimethyl-1H-pyrrol-1-yl)-3-[methyl(3-pyridylmethylene)amino]-2(Z)-butene-1,4-dinitrile, the product of the Paal-Knorr reaction, was successfully utilized in the Linstead macrocyclization towards symmetrical and unsymmetrical porphyrazines. NMR and X-ray study revealed an almost perpendicular orientation of the pyrrolyl groups in relation to the porphyrazine platform. The newly synthesized macrocycles with different peripheral groups show interesting spectroscopic and electrochemical properties. Due to selective sensor/coordination properties they are expected to find applications as chemical sensors and electronic materials.

scholarly journals Synthesis and characterization of hollow V2O5 microspheres for supercapacitor electrode with pseudocapacitance

2017 ◽  
Vol 35 (1) ◽  
pp. 188-196 ◽  
Author(s):  
Yifu Zhang
Keyword(s):  
Electrochemical Properties ◽  
Synthesis And Characterization ◽  
Carbon Spheres ◽  
Galvanostatic Charge ◽  
Supercapacitor Electrode ◽  
Promising Candidate ◽  
X Ray ◽  
Subsequent Calcination ◽  
Ft Ir

AbstractHollow V2O5 microspheres (HVOM) were fabricated using NH4VO3, ethylene glycol and carbon spheres as the starting materials by a template solvothermal approach and subsequent calcination. The morphology and composition were characterized by field emission scanning electron microscopy (FE-SEM), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and Brunauer-Emmet-Teller (BET). The results showed that the obtained HVOM were constructed from nanoparticles with rough surface. The electrochemical properties of HVOM as a supercapacitor electrode were investigated by cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD). HVOM displayed excellent pseudocapacitance property and their specific capacitances were 488 F·g–1, 455 F·g–1, 434 F·g–1 and 396 F·g–1 at the current density of 0.5 A·g–1, 1 A·g–1, 2 A·g–1 and 5 A·g–1, respectively. They also exhibited an excellent energy density of 8.784 × 105 J·kg–1 at a power density of 900 W·kg–1 . The good electrochemical properties of the as-synthesized HVOM make them a promising candidate as a cathode material for supercapacitors.

Syntheses, electrochemistry and photophysical properties of a series ofmeso-pyridylpentafluorophenylporphyrins

2010 ◽  
Vol 14 (11) ◽  
pp. 975-984 ◽  
Author(s):  
Emmanuel Z. Moreira ◽  
Alba D.Q. Ferreira ◽  
Cláudio Roberto Neri ◽  
Sumitra Mukhopadhyay ◽  
Sérgio Dovidauskas ◽  
...  
Keyword(s):  
Electrochemical Properties ◽  
Photophysical Properties ◽  
Synthesis And Characterization ◽  
Redox Potentials ◽  
Trans Isomers ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cis And Trans Isomers ◽  
Cis And Trans

This work presents the synthesis and characterization of a series of substituted pyridylpentafluroporphyrins, including the separation of the cis- and trans-isomers, the latter being characterized by X-ray crystallography. The spectroscopic and electrochemical properties of the series are dependent on the number of electron withdrawing pentafluorophenyl substituent, but they do not depend on the symmetry of the molecule. Ongoing from the monosubstituted to the more substituted pentafluorophenyl porphyrin H2(MPyTFPP) derivative, the Soret bands are slightly red-shifted and their quantum fluorescence yields range from 0.035 to 0.046, consistent with the value of 0.045 for the fully substituted 5,10,15,20-tetrapentafluorophenylporphyrin (dichloromethane solutions). The redox potentials of the reductive processes of monoanion and dianion formation are also sensitive to the number of pentafluoro substituents, shifting 180 mV to more positive values for the P0/P-1process ongoing from the monopentafluoro to the tris-pentafluorophenyl substituted derivative.

A convenient and selective route to a trans-difunctionalized macrocyclic hexadentate N4O2 ligand

2001 ◽  
Vol 79 (7) ◽  
pp. 1105-1109 ◽  
Author(s):  
Hongyan Luo ◽  
Robin D Rogers ◽  
Martin W Brechbiel
Keyword(s):  
Functional Groups ◽  
Metal Ion ◽  
Condensation Reaction ◽  
Synthesis And Characterization ◽  
Tetraaza Macrocycle ◽  
X Ray ◽  
Hexadentate Ligand

The synthesis and characterization of a novel difunctionalized tetraaza macrocycle, 1,8-bis(2-hydroxybenzyl)-1,4,8,11-tetraazacyclotetradecane (abbreviated H2bcyclamb), is described. The diprotic hexadentate ligand N4O2 was conveniently synthesized in two steps by the cyclic condensation reaction of 1,4,8,11-tetraazacyclotetradecane (abbreviated cyclam) and salicylaldehyde, followed by NaBH4 reduction of the cyclic hexahydropyrimidine condensate. The difunctionalization was selective and is the first procedure of trans-difunctionalization of a tetraazamacrocycle, without generating mono-, tri-, or tetra-functionalized products, with only 1,8-difunctionalized product being isolated, and with the convenience of the functionalization occurring as a result of deprotection. The trans-arrangement of the two functional groups in H2bcyclamb was verified by X-ray crystallographic studies of the copper(II) complex [Cu(H2bcyclamb)](OAc)2·2H2O. The crystal is monoclinic, P21/c, with a = 10.0931(2), b = 13.8820(1), c = 10.8752(1) Å, β = 106.332(1)°, V = 1462.26(3) Å3. The structure of [Cu(H2bcyclamb)](OAc)2·2H2O also shows the metal ion in an elongated octahedral geometry.Key words: 1,8-difunctionalized, cyclam, copper(II) complex.

Tetraalkyldiarsines As Potential Precursors for Electronic Materials: Synthesis and Characterization Of Various Iso-Propyl Arsenic Compounds

1993 ◽  
Vol 334 ◽  
Author(s):  
Lawrence F. Brough ◽  
Liu Gang ◽  
Matthew A. Lipkovich ◽  
Thomas J. Colacot ◽  
Virgil L. Goedken ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Lithium Salt ◽  
Electronic Materials ◽  
Synthesis And Characterization ◽  
Materials Synthesis ◽  
Arsenic Compounds ◽  
X Ray

AbstractTetrakis(iso-propyl)diarsine was synthesized by the reaction of (i-Pr)2AsLi with (i-Pr)2AsI. The lithium salt of the secondary arsine was produced following deprotonation of (i-Pr)2AsH, obtained by reduction of (i-Pr)2AsI, which was prepared by the thermolysis of (i-Pr)3Asl2. The X-ray crystal structure of \(i-Pr)3AsI]\I] has been determined on the product of the reaction of (i-Pr)3As and 12. Compounds of the general form E=As(i-Pr)3 (E = O, S, Se) have been prepared.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

scholarly journals Synthesis and characterization of Fe, Co, and Ni colloids in 2-mercaptoethanol

2020 ◽  
Vol 10 ◽  
pp. 184798042096688
Author(s):  
Galo Cárdenas-Triviño ◽  
Sergio Triviño-Matus
Keyword(s):  
Electron Microscopy ◽  
Electron Diffraction ◽  
Colloidal Dispersions ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Transmission Electron ◽  
Vis Spectroscopy ◽  
Chemical Liquid Deposition ◽  
Liquid Deposition

Metal colloids in 2-mercaptoethanol using nanoparticles (NPs) of iron (Fe), cobalt (Co), and nickel (Ni) were prepared by chemical liquid deposition method. Transmission electron microscopy, electron diffraction, UV-VIS spectroscopy, and scanning electron microscopy with electron dispersive X-ray spectroscopy characterized the resulting colloidal dispersions. The NPs exhibited sizes with ranges from 9.8 nm for Fe, 3.7 nm for Co, and 7.2 nm for Ni. The electron diffraction shows the presence of the metals in its elemental state Fe (0), Co (0), and Ni (0) and also some compounds FeO (OH), CoCo2S4, and NiNi2S4.

scholarly journals Synthesis and Characterization of Clay Polymer Nanocomposites of P(4VP-co-AAm) and Their Application for the Removal of Atrazine

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 721 ◽  
Author(s):  
Jorge A. Ramírez-Gómez ◽  
Javier Illescas ◽  
María del Carmen Díaz-Nava ◽  
Claudia Muro-Urista ◽  
Sonia Martínez-Gallegos ◽  
...  
Keyword(s):  
Polymer Nanocomposites ◽  
Nanocomposite Materials ◽  
Synthesis And Characterization ◽  
Cross Linking ◽  
X Ray Diffraction ◽  
Numerous Species ◽  
X Ray ◽  
Different Types ◽  
Synthesized Materials

Atrazine (ATZ) is an herbicide which is applied to the soil, and its mechanism of action involves the inhibition of photosynthesis. One of its main functions is to control the appearance of weeds in crops, primarily in corn, sorghum, sugar cane, and wheat; however, it is very toxic for numerous species, including humans. Therefore, this work deals with the adsorption of ATZ from aqueous solutions using nanocomposite materials, synthesized with two different types of organo-modified clays. Those were obtained by the free radical polymerization of 4-vinylpyridine (4VP) and acrylamide (AAm) in different stoichiometric ratios, using tetrabutylphosphonium persulfate (TBPPS) as a radical initiator and N,N′-methylenebisacrylamide (BIS) as cross-linking agent. The structural, morphological, and textural characteristics of clays, copolymers, and nanocomposites were determined through different analytical and instrumental techniques, i.e., X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Adsorption kinetics experiments of ATZ were determined with the modified and synthesized materials, and the effect of the ratio between 4VP and AAm moieties on the removal capacities of the obtained nanocomposites was evaluated. Finally, from these sets of experiments, it was demonstrated that the synthesized nanocomposites with higher molar fractions of 4VP obtained the highest removal percentages of ATZ.

scholarly journals High-pressure synthesis and characterization of the non-centrosymmetric scandium borate ScB6O9(OH)3

2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Structure Solution ◽  
Temperature Experiment ◽  
Pressure Synthesis

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.

scholarly journals Synthesis and characterization of an electron-deficient conjugated polymer based on pyridine-flanked diketopyrrolopyrrole

RSC Advances ◽  
2021 ◽  
Vol 11 (21) ◽  
pp. 12995-13003
Author(s):  
Jialin Yang ◽  
Li Yang ◽  
Qianqian Chen ◽  
Keke Guo ◽  
Ji-Min Han
Keyword(s):  
Conjugated Polymers ◽  
Electrochemical Properties ◽  
Conjugated Polymer ◽  
Synthesis And Characterization

We report a pyridine-flanked diketopyrrolopyrrole monomer and all-acceptor conjugated polymers synthesized therefrom. Photophysical, thermal and electrochemical properties of the polymers have been determined.

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