scholarly journals Functional Aromatic Poly(1,3,4-Oxadiazole-Ether)s with Benzimidazole Pendants: Synthesis, Thermal and Dielectric Studies

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Shimoga D. Ganesh ◽  
Vasantakumar K. Pai ◽  
Mahadevappa Y. Kariduraganavar ◽  
Madhu B. Jayanna
Keyword(s):  
Carboxylic Acid ◽  
Average Molecular Weight ◽  
Analytical Techniques ◽  
Gel Permeation Chromatography ◽  
Electrical Contacts ◽  
Dielectric Studies ◽  
Weight Average Molecular Weight ◽  
Nucleophilic Displacement ◽  
Ft Ir

Poly(1,3,4-oxadiazole-ether) with reactive carboxylic acid pendants was synthesized from solution polymerization via nucleophilic displacement polycondensation among 2,5-bis(4-fluorophenyl)-1,3,4-oxadiazole (BFPOx) and 4,4′-bis(4-hydroxyphenyl) valeric acid (BHPA). Without altering the polymeric segments, benzimidazole modified poly(1,3,4-oxadiazole-ether)s were prepared by varying stoichiometric ratios of 1,2-phenylenediamine. The molecular structural characterization of these polymers was achieved by, FT-IR, NMR, TGA, elemental analysis, and analytical techniques. The weight-average molecular weight of virgin polymer with carboxylic acid functionality was determined by gel permeation chromatography (GPC) and was found to be 22400 (Mw/Mn=2.07). All the synthesized polyethers were compressed into pellets and electrical contacts were established to perform dielectric properties.

A New Green Process for Synthesising High Quality PLLA Materials

2013 ◽  
Vol 750-752 ◽  
pp. 1377-1380 ◽  
Author(s):  
Hui Li Shao ◽  
Xian Jue Zhou ◽  
Xue Chao Hu
Keyword(s):  
Molecular Weight ◽  
Ring Opening ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Ring Opening Polymerization ◽  
Green Process ◽  
Weight Average Molecular Weight ◽  
H Nmr ◽  
Ft Ir ◽  
C Nmr

Synthesis of Poly(L-lactide) (PLLA) by the ring-opening polymerization (ROP) of L-lactides in supercritical carbon dioxide (SC-CO2) with co-solvent were studied. Effects of kinds of co-solvent on the molecular weight (MW) and the molecular weight distribution (MWD) of the resultant polymers were investigated by the gel permeation chromatography (GPC). The resultant polymers were also characterized with1H NMR,13C NMR and FT-IR. It was found that PLLA with high purity and almost without racemization could be obtained by this technology and the acetone is the best co-solvent for this kind of polymerization. By using stannous octoate as initiator and acetone as co-solvent, PLLA having a weight-average molecular weight (Mw) near to 9×104and polydispersity index (PDI) of 1.7 was successfully synthesized.

Characterization of aspen exploded wood lignin

1982 ◽  
Vol 60 (18) ◽  
pp. 2372-2382 ◽  
Author(s):  
R. H. Marchessault ◽  
Suzanne Coulombe ◽  
Hiromichi Morikawa ◽  
Danielle Robert
Keyword(s):  
Room Temperature ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Aryl Ether ◽  
Weight Average Molecular Weight ◽  
Nmr Spectrum ◽  
Typical Composition ◽  
Moist Steam ◽  
C Nmr

Exploded wood lignin (EXWL) was extracted from moist steam hydrolysed aspen (Populustremuloides) wood using methanol. The lignin was examined by elemental analysis, gel permeation chromatography, infrared spectroscopy, proton and 13C nmr. The observed nmr spectra were compared with those of aspen milled wood lignin (MWL). Typical composition of the material is C9H9.2O2.7(OCH3)1.1 Assignment of all the signals in the nmr spectrum led to the conclusion that the explosion process causes cleavage of the β-aryl-ether bond. The weight average molecular weight was found to be 1700–1900 and the polydispersity 2.6. The finely divided exploded wood was soluble in 90% methanol/water mixtures to well beyond 20% by weight at room temperature.

scholarly journals Poly(Arylene Ether Sulfone)s with HEPES Pendants: Synthesis, Thermal, and Dielectric Studies

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
S. D. Ganesh ◽  
M. N. K. Harish ◽  
B. J. Madhu ◽  
Husnasarvari Maqbool ◽  
K. V. Pai ◽  
...  
Keyword(s):  
Dielectric Properties ◽  
Carboxylic Acid ◽  
Acid Group ◽  
Electrical Contacts ◽  
Stoichiometric Ratio ◽  
Coupling Condition ◽  
Arylene Ether ◽  
Modified Polymers ◽  
Nucleophilic Displacement ◽  
Ft Ir

Polyethersulfone with active carboxylic acid pendants was prepared from solution polymerization via nucleophilic displacement polycondensation reaction among 4,4′-dichlorodiphenyl sulfone (DCDPS) and 4,4′-bis(4-hydroxyphenyl) valeric acid (BHPA). The conditions necessary to synthesize and purify the polymer were investigated in some details. The synthesized polyethersulfone comprises sulfone and ether linkages in addition to reactive carboxylic acid functionality; this reactive carboxylic acid group was exploited to hold the HEPES moiety via ester linkage and is achieved by simple DCC coupling condition at ambient temperature. Without impairing the primary polymeric backbone, three modified polymers were prepared by varying the stoichiometric ratio of HEPES. Characterization of the polymers by 1H & 13C NMR, FT-IR, and TGA demonstrated that HEPES was quantitatively incorporated into the prime polymer. All the prepared polymers were pressed into tablets, and electrical contacts were established to study the dielectric properties. Finally, the influence of the HEPES on the dielectric properties was examined.

Synthesis and Characterization of Poly(N-arylenebenzimidazole sulfone)

2012 ◽  
Vol 174-177 ◽  
pp. 473-477
Author(s):  
Ye Wei Xu ◽  
Jie Tang ◽  
Guan Jun Chang ◽  
Fang Hua Zhu ◽  
Lin Zhang
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Structure ◽  
Polyphosphoric Acid ◽  
High Resolution Mass Spectrometry ◽  
Gel Permeation Chromatography ◽  
The Novel ◽  
Good Solubility ◽  
Nucleophilic Displacement ◽  
Ft Ir

Poly(N-arylenebenzimidazole sulfone), PNABIS, has been prepared via the aromatic nucleophilic displacement reaction of 1,4-bis(2-benzimidazolyl) benzene (BBIB) with bis(4-fluorophenyl) sulfone. BBIB was synthesized by the reaction of terephthalaldehydic acid with 1,2-phenylenediamine in polyphosphoric acid. The chemical structure of BBIB was confirmed by FT-IR, high resolution mass spectrometry (HRMS) and NMR spectroscopy. The characterization of the polymer was performed with FT-IR, NMR spectroscopy, gel permeation chromatography (GPC), thermogravimetric analysis (TGA) and solubility tests. The polymer was obtained in quantitative yield with Mn value 11000 and Mw value 25300, respectively. TGA measurements show that 5% weight loss temperature is 532 °C in nitrogen and 331 °C in air, respectively. In addition, the novel polymer exhibits good solubility, which can be dissolved in common organic solvent at room temperature.

Behavior of xylans from the Eucalyptus species. Part 2. Characterization of 4-O-methylglucuronoxylans isolated from black liquors of kraft pulping of Eucalyptus grandis and E. urophylla

Holzforschung ◽  
2013 ◽  
Vol 67 (2) ◽  
pp. 123-128
Author(s):  
Andréia S. Magaton ◽  
Teresa Cristina F. Silva ◽  
Jorge Luiz Colodette ◽  
Dorila Piló-Veloso ◽  
Flaviana Reis Milagres ◽  
...  
Keyword(s):  
Average Molecular Weight ◽  
Eucalyptus Grandis ◽  
Kraft Pulping ◽  
Raw Material ◽  
Size Exclusion ◽  
Eucalyptus Species ◽  
Exclusion Chromatography ◽  
Ft Ir ◽  
Black Liquors

Abstract 4-O-methylglucuronoxylans isolated from Eucalyptus grandis and Eucalyptus urophylla kraft black liquors (KBLs) were chemically characterized by Fourier transform infrared spectroscopy (FT-IR), size exclusion chromatography (SEC), and nuclear magnetic resonance (NMR) spectroscopy. Doses of alkali charge, expressed as active alkali (AA), were 16, 17, and 18% while the sulfidity was kept at 25%. Kappa numbers of 19.1, 17.5, and 16.1 for E. grandis and 20.4, 16.8, and 15.4 for E. urophylla were obtained. At higher alkali charges, the recovery of xylans from the KBLs was lower and the degree of substitution of xylans with uronic acids decreased. The average molecular weight (Mw) of the recovered xylans was greater under conditions of mild pulping, i.e., in the case of pulps with higher kappa numbers. Mw of xylans ranged from 16.1 to 19.1 kDa for E. grandis and from 15.4 to 20.4 kDa for E. urophylla. The xylans from KBL may be useful as pulp modifying agents or as a raw material for advanced applications.

scholarly journals Characterisation of Sequential Solvent Fractionation and Base-catalysed Depolymerisation of Treated Alkali Lignin

BioResources ◽  
2015 ◽  
Vol 10 (3) ◽  
pp. 4137-4151 ◽  
Author(s):  
Aikfei Ang ◽  
Zaidon Ashaari ◽  
Edi Suhaimi Bakar ◽  
Nor Azowa Ibrahim
Keyword(s):  
Molecular Weight ◽  
Chemical Structure ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Solubility Parameters ◽  
Low Molecular Weight ◽  
Sequential Fractionation ◽  
Weight Average Molecular Weight ◽  
Solvent Fractionation ◽  
Alkali Lignin

An alkali lignin (OL) with a weight-average molecular weight (Mw) of 11646 g/mol was used to prepare low-molecular weight lignin for resin synthesis. The low-molecular weight lignin feedstock was obtained via base-catalysed depolymerisation (BCD) treatments at different combined severity factors. Sequential fractionation of the OL and BCD-treated lignins using organic solvents with different Hildebrand solubility parameters were used to alter the homogeneity of the OL. The yield and properties of OL itself and OL and BCD-treated OL dissolved in propan-1-ol (F1), ethanol (F2), and methanol (F3) were determined. Regardless of the treatment applied, a small amount of OL was dissolved in F1 and F2. The BCD treatment did not increase the yield of F1 but did increase the yields of F2 and F3. Gel permeation chromatography (GPC) showed that the repolymerization reaction occurred in F3 for all BCD-treated OL, so these lignins were not suitable for use as feedstocks for resin production. The GPC, 13Carbon-nuclear magnetic resonance, and Fourier transform infrared spectroscopy analyses confirmed that the F3 in OL exhibited the optimum yield, molecular weight distribution, and chemical structure suitable for use as feedstocks for resin synthesis.

Characterization of bi-layered magnetic nanoparticles synthesized via two-step surface-initiated ring-opening polymerization

2015 ◽  
Vol 87 (11-12) ◽  
pp. 1085-1097 ◽  
Author(s):  
Li Wang ◽  
Stefan Baudis ◽  
Karl Kratz ◽  
Andreas Lendlein
Keyword(s):  
Magnetic Nanoparticles ◽  
Ring Opening ◽  
Average Molecular Weight ◽  
Polymer Networks ◽  
Gel Permeation Chromatography ◽  
Degree Of Crystallinity ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Transmission Electron

AbstractA versatile strategy to integrate multiple functions in a polymer based material is the formation of polymer networks with defined nanostructures. Here, we present synthesis and comprehensive characterization of covalently surface functionalized magnetic nanoparticles (MNPs) comprising a bi-layer oligomeric shell, using Sn(Oct)2 as catalyst for a two-step functionalization. These hydroxy-terminated precursors for degradable magneto- and thermo-sensitive polymer networks were prepared via two subsequent surface-initiated ring-opening polymerizations (ROPs) with ω-pentadecalactone and ε-caprolactone. A two-step mass loss obtained in thermogravimetric analysis and two distinct melting transitions around 50 and 85°C observed in differential scanning calorimetry experiments, which are attributed to the melting of OPDL and OCL crystallites, confirmed a successful preparation of the modified MNPs. The oligomeric coating of the nanoparticles could be visualized by transmission electron microscopy. The investigation of degrafted oligomeric coatings by gel permeation chromatography and 1H-NMR spectroscopy showed an increase in number average molecular weight as well as the presence of signals related to both of oligo(ω-pentadecalactone) (OPDL) and oligo(ε-caprolactone) (OCL) after the second ROP. A more detailed analysis of the NMR results revealed that only a few ω-pentadecalactone repeating units are present in the degrafted oligomeric bi-layers, whereby a considerable degree of transesterification could be observed when OPDL was polymerized in the 2nd ROP step. These findings are supported by a low degree of crystallinity for OPDL in the degrafted oligomeric bi-layers obtained in wide angle X-ray scattering experiments. Based on these findings it can be concluded that Sn(Oct)2 was suitable as catalyst for the preparation of nanosized bi-layered coated MNP precursors by a two-step ROP.

Preparation and Characterization of a Novel Flame Retardant

2008 ◽  
Vol 47-50 ◽  
pp. 294-297 ◽  
Author(s):  
Xiu Wei Jia ◽  
Min Zhi Rong ◽  
Ming Qiu Zhang
Keyword(s):  
Flame Retardant ◽  
Sol Gel ◽  
Average Molecular Weight ◽  
Regular Structure ◽  
Gel Permeation Chromatography ◽  
Helical Conformation ◽  
Infrared Spectrometry ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction

A novel flame retardant polymethylsilsesquioxane (PMSQ) was successfully obtained via combination of non-hydrolytic and hydrolytic sol-gel routes. Chemical structure of the resultant PMSQ was determined by nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectrometry and powder X-ray diffraction, respectively. All the measurements demonstrated that the product possessed regular structure with chain-to-chain width of 0.87nm and chain thickness of 0.40nm. Weight average molecular weight of PMSQ was measured to be 3.5×105 using gel permeation chromatography. Numerical simulations of the molecular structure suggested that PMSQ should exhibit cis-isotactic configuration and double helical conformation at undisturbed condition.

Kinetic Studies on the Curing Reactions of Fluoroepoxy Oligomer and Cycloaliphatic Amine

2013 ◽  
Vol 747 ◽  
pp. 753-756 ◽  
Author(s):  
Thitinun Chongtum ◽  
Wunpen Chonkaew
Keyword(s):  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Kinetic Studies ◽  
Equivalent Weight ◽  
Number Average Molecular Weight ◽  
Polymeric Systems ◽  
Acid Titration ◽  
Curing Kinetic ◽  
Gel Permeation

The curing kinetic analysis is an important technique for the characterization of the curing behavior of reactive polymeric systems. In this study, fluoroepoxy oligomer was synthesized from trifluoromethyl aniline and epichlorohydrin. The epoxide equivalent weight (EEW) and the number average molecular weight (Mn) of the systhesized fluroepoxy oligomer determined from acid titration and gel permeation chromatography were found to be 312.16 g/eq and 534 g/mol, respectively. The mixtures of the fluoroepoxy oligomer were mixed with the cycloaliphatic amine in various stiochiometric ratios (1:1, 1: 1.5 and 1:2). The effects of the stiochiometric ratio on the curing behaviors were studied using both isothermal and non-isothermal DSC methods. Ozawas, Kissingers and Friedmans methods were employed to investigate the kinetic parameters. The results showed that the peak temperature (Tp) increased with the increasing heating rate. The activation energy (Ea) calculated from Ozawas and Kissingers methods were much larger than that from Friedmans method.

Synthesis, characterization and OFET property of four diaminouracil bridged novel ball-type phthalocyanines

2018 ◽  
Vol 22 (01n03) ◽  
pp. 149-156 ◽  
Author(s):  
Ayşegül Yazıcı ◽  
Ayşe Avcı ◽  
Ahmet Altındal ◽  
Bekir Salih ◽  
Özer Bekaroğlu
Keyword(s):  
Field Effect ◽  
Active Material ◽  
Text Type ◽  
H Nmr ◽  
Gate Structure ◽  
Nucleophilic Displacement ◽  
Ft Ir ◽  
Effect Transistor ◽  
Top Gate Structure

New ball-type metallobisphthalocyanines 2 (Co[Formula: see text]Pc[Formula: see text] and 3(Zn[Formula: see text]Pc[Formula: see text] were synthesized from the corresponding 4,4[Formula: see text]-[(5,6-diaminopyrimidine-2,4-diyl)bis(oxy)] diphytalonitril 1, which can be obtained by a nucleophilic displacement reaction of 4-nitrophthalonitrile with 5,6-diaminouracil sulfate. Characterization of novel compounds was performed by UV-vis, FT-IR, [Formula: see text]H-NMR, MALDI-TOF mass spectroscopy and elemental analysis. Organic field effect transistor devices (OFETs) with top gate structure were fabricated using these novel compounds as the active material. The devices were characterized by means of their output and transfer characteristics, and it was found that these OFET devices exhibit [Formula: see text]-type behavior. When compared with the 2-based device, the OFET with 3 showed higher field effect mobility and larger on/of current ratio.

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