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.

Synthesis and Characterization of Poly(N-Arylenebenzimidazole Ketone)

2012 ◽  
Vol 204-208 ◽  
pp. 4211-4214 ◽  
Author(s):  
Ye Wei Xu ◽  
Jie Tang ◽  
Guan Jun Chang ◽  
Fang Hua Zhu ◽  
Lin Zhang
Keyword(s):  
Weight Loss ◽  
Chemical Structure ◽  
Synthesis And Characterization ◽  
The Novel ◽  
Displacement Reaction ◽  
Good Solubility ◽  
Nucleophilic Displacement ◽  
Ft Ir ◽  
Good Agreement

Using 1,4-bis(2-benzimidazolyl) benzene (BBIB) and 4,4'-difluorobenzophenone as the monomers, poly(N-arylenebenzimidazole ketone) (PNABIK) has been prepared via the aromatic nucleophilic displacement reaction. The chemical structure of PNABIK was confirmed by FT-IR, elemental analysis and 1H NMR. The results show a good agreement with the proposed structures. The polymer was obtained in quantitative yields with Mn value 12500 and Mw value 28600, respectively. DSC and TGA measurements show that the glass transition temperature (Tg) is 202 °C and 5% weight loss temperature is 550°C in nitrogen and 571 °C in air, respectively. In addition, the novel polymer exhibit good solubility.

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.

Preparation and Characterization of Soybean Oil-based Flame Retardant Rigid Polyurethane Foams Containing Phosphaphenanthrene Groups

2020 ◽  
Vol 17 (10) ◽  
pp. 760-771
Author(s):  
Qirui Gong ◽  
Niangui Wang ◽  
Kaibo Zhang ◽  
Shizhao Huang ◽  
Yuhan Wang
Keyword(s):  
Soybean Oil ◽  
Flame Retardant ◽  
Chemical Structure ◽  
Cell Structure ◽  
Polyurethane Foams ◽  
Limiting Oxygen Index ◽  
Rigid Polyurethane Foams ◽  
Degradation Activation Energy ◽  
Ft Ir

A phosphaphenanthrene groups containing soybean oil based polyol (DSBP) was synthesized by epoxidized soybean oil (ESO) and 9,10-dihydro-oxa-10-phosphaphenanthrene-10-oxide (DOPO). Soybean oil based polyol (HSBP) was synthesized by ESO and H2O. The chemical structure of DSBP and HSBP were characterized with FT-IR and 1H NMR. The corresponding rigid polyurethane foams (RPUFs) were prepared by mixing DSBP with HSBP. The results revealed apparent density and compression strength of RPUFs decreased with increasing the DSBP content. The cell structure of RPUFs was examined by scanning electron microscope (SEM) which displayed the cells as spherical or polyhedral. The thermal degradation and flame retardancy of RPUFs were investigated by thermogravimetric analysis, limiting oxygen index (LOI), and UL 94 vertical burning test. The degradation activation energy (Ea) of first degradation stage reduced from 80.05 kJ/mol to 37.84 kJ/mol with 80 wt% DSBP. The RUPF with 80 wt% DSBP achieved UL94 V-0 rating and LOI 28.3. The results showed that the flame retardant effect was mainly in both gas phase and condensed phase.

scholarly journals Grape Seeds Proanthocyanidins: Advanced Technological Preparation and Analytical Characterization

Antioxidants ◽  
2021 ◽  
Vol 10 (3) ◽  
pp. 418
Author(s):  
Paolo Morazzoni ◽  
Paola Vanzani ◽  
Sandro Santinello ◽  
Antonina Gucciardi ◽  
Lucio Zennaro ◽  
...  
Keyword(s):  
High Resolution Mass Spectrometry ◽  
Industrial Process ◽  
Gel Permeation Chromatography ◽  
Grape Seed ◽  
Direct Infusion ◽  
Grape Seeds ◽  
Flow Filtration ◽  
Process Patent ◽  
Shotgun Approach

A “green” solvent-free industrial process (patent pending) is here described for a grape seed extract (GSE) preparation (Ecovitis™) obtained from selected seeds of Veneto region wineries, in the northeast of Italy, by water and selective tangential flow filtration at different porosity. Since a comprehensive, non-ambiguous characterization of GSE is still a difficult task, we resorted to using an integrated combination of gel permeation chromatography (GPC) and electrospray ionization high resolution mass spectrometry (ESI-HRMS). By calibration of retention time and spectroscopic quantification of catechin as chromophore, we succeeded in quantifying GPC polymers up to traces at n = 30. The MS analysis carried out by the ESI-HRMS method by direct-infusion allows the detection of more than 70 species, at different polymerization and galloylation, up to n = 13. This sensitivity took advantage of the nanoscale shotgun approach, although paying the limit of missed separation of stereoisomers. GPC and MS approaches were remarkably well cross-validated by overlapping results. This simple integrated analytical approach has been used for quality control of the production of Ecovitis™. The emerging feature of Ecovitis™ vs. a popular benchmark in the market, produced by a different technology, is the much lower content of species at low n and the corresponding increase of species at high n.

Synthesis and Characterization of a Novel Linear Benzoxazine-Containing Polytriazole via Metal-Free Click Reaction and its Self-Crosslinking Behavior

2012 ◽  
Vol 557-559 ◽  
pp. 973-978
Author(s):  
Zhong Yi Xu ◽  
Lei Du ◽  
Li Qiang Wan ◽  
Fa Rong Huang
Keyword(s):  
Click Reaction ◽  
Decomposition Temperature ◽  
Linear Polymer ◽  
The Novel ◽  
Metal Free ◽  
Crosslinked Polymer ◽  
Degradation Behaviors ◽  
Ft Ir ◽  
Increasing Temperature

A novel linear benzoxazine-containing polytriazole was successfully synthesized via metal-free click reaction. Benefited from the advantages of click reaction, the synthesis procedure was easily and efficiently. The linear polymer could be transformed into crosslinked structure after ring-opening polymerization of oxazine induced by the increasing temperature. The FT-IR characterization verified the structure transformation between linear and crosslinked polymer. Moreover, the thermal properties and thermal degradation behaviors of linear polymer and the corresponding crosslinked polymer were studied by DSC and TGA. The novel polytriazole was proved to be a kind of thermal stable polymers with high thermal decomposition temperature (Td5over 300°C).

Microwave-assisted solvent-free synthesis and spectral and structural characterization of cyclotriphosphazene hexakis(o-tolylamide)

2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Microwave Irradiation ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
Microwave Assisted ◽  
Ft Ir ◽  
Solvent Free Synthesis

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.

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.

Surface Grafting Modification of Silk Fibroin by Atom Transfer Radical Polymerization

2008 ◽  
Vol 373-374 ◽  
pp. 629-632 ◽  
Author(s):  
Tie Ling Xing ◽  
Hai Jiang Wang ◽  
Zhan Xiong Li ◽  
Guo Qiang Chen
Keyword(s):  
Silk Fibroin ◽  
Gel Permeation Chromatography ◽  
Catalyst System ◽  
Hydroxyl Groups ◽  
Amino Groups ◽  
Grafting Modification ◽  
Antibacterial Surface ◽  
Ft Ir ◽  
Tertiary Amino

In this work, surface modification of silk fibroin was conducted by grafting dimethylaminoethyl methacrylate (DMAEMA) via ATRP to produce well controlled grafting silk. First, the amino groups and hydroxyl groups on the side chains of the silk fibroin reacted with 2-bromoisobutyryl bromide (BriB-Br) to obtain efficient initiator for ATRP. Subsequently, the functional silk fibroin was used as macroinitiator of DMAEMA in 1,2-dichlorobenzene in conjunction with CuBr/N,N,N',N",N" -pentamethyldiethylenetriamine (PMDETA) as a catalyst system. FT-IR characterization of the modified silk substrate showed a peak corresponding to DMAEMA indicating that the polymer had been formed on the silk surface. Following the polymerization, the tertiary amino groups on the grafted silk fibroin were quaternized to produce a large concentration of quaternary ammonium groups, which endowed the silk substrate with potential antibacterial surface. The graft chains were cleaved by acid hydrolysis and analyzed by gel permeation chromatography (GPC). The GPC results indicated that the graft layer were well-controlled.

Synthesis and Characterization of Novel Degradable Responsive Polyurethane Microsphere

2013 ◽  
Vol 750-752 ◽  
pp. 1271-1275 ◽  
Author(s):  
Lian Hai Shan ◽  
Yuan Yuan Cui ◽  
Shuai Huang ◽  
Zhi Bin Zhang
Keyword(s):  
Drug Delivery ◽  
Molecular Weight ◽  
Chemical Structure ◽  
Solvent Polarity ◽  
Toluene Diisocyanate ◽  
Synthesis And Characterization ◽  
The Novel ◽  
Swelling Ratio ◽  
Swelling Properties

The present study describes degradable polyurethane (PU) microspheres fabricated using toluene diisocyanate, polycaprolactone, polyethylene glycol, 2, 2-hydroxymethyl-2-propionic acid and triethylamine for drug delivery. The novel microspheres were synthesized using self-emulsion and condensed phase separation method. Fourier-Transform Infrared Spectrum analysis (FTIR) was performed revealing the chemical structure of polyurethane microspheres with special chains changing. Swelling properties influenced by solvent polarity, PEG content, PEG molecular weight, were evaluated, suggesting that the swelling ratio (SR) of PU microspheres increased with the increase in solvent polarity, PEG content and PEG molecular weight respectively.

Synthesis and Characterization of Temperature-Sensitive TSPU/PNIPAAm Semi-IPN Polymer

2011 ◽  
Vol 399-401 ◽  
pp. 359-362 ◽  
Author(s):  
Yi Chun Wang ◽  
Zheng Wei Dai ◽  
Yuan Xue
Keyword(s):  
Chemical Structure ◽  
In Situ Polymerization ◽  
Phenyl Isocyanate ◽  
Chain Extender ◽  
Synthesis And Characterization ◽  
Temperature Sensitive ◽  
Sensitive Material ◽  
Ft Ir

Thermo-sensitive polyurethane (TSPU) was synthesized from poly(ε-caprolactone) and 4,4’-methylenebis (phenyl isocyanate) by a two-step process with 1,4-butanediol as the chain extender. Following that, a novel temperature-sensitive material was created by the strategy of IPN from TSPU and PNIPAAm in the method of in situ polymerization. The chemical structure and thermo properties of the semi-IPN were characterized with FT-IR and DSC. The results prove that intensive inter-molecular interactions exist between TSPU and PNIPAAm chains, which have significant influence on the phase transition behaviors of the material. According to these results, the transition temperature of the semi-IPN can be adjusted in the range of 30~40 °C by controlling the composition of TSPU and the semi-IPNs.

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