Synthesis,characterization, conductivity,band gap,and kinetic of thermal degradation of poly‐4‐[(2‐mercaptophenyl) imino methyl] phenol

The oxidative polycondensation reaction conditions of 4‐[(2‐mercaptophenyl) imino methyl] phenol (2‐MPIMP) were studied in an aqueous acidic medium between 40 and 90°C by using oxidants such as air, H₂O₂, and NaOCl. The structures of the synthesized monomer and polymer were confirmed by FTIR, ¹H NMR, ¹³C NMR, and elemental analysis. The characterization was made by TGA‐DTA, size exclusion chromatography (SEC) and solubility tests. At the optimum reaction conditions, the yield of poly‐4‐[(2‐mercaptophenyl) imino methyl]phenol (P‐2‐MPIMP) was found to be 92% for NaOCl oxidant, 84% for H₂O₂ oxidant 54% for air oxidant. According to the SEC analysis, the number‐average molecular weight (M_n), weight‐average molecular weight (M_w), and polydispersity index values of P‐2‐MPIMP were found to be 1700 g mol^?1, 1900 g mol^?1, and 1.118, using H₂O₂; 3100 g mol^?1, 3400 g mol^?1, and 1.097, using air; and 6750 g mol^?1, 6900 g mol^?1, and 1.022, using NaOCl, respectively. According to TG analysis, the weight losses of 2‐MPIMP and P‐2‐MPIMP were found to be 95.93% and 76.41% at 1000°C, respectively. P‐2‐MPIMP showed higher stability against thermal decomposition. Also, electrical conductivity of the P‐2‐MPIMP was measured, showing that the polymer is a typical semiconductor. The highest occupied molecular orbital, the lowest unoccupied molecular orbital, and the electrochemical energy gaps (E′_g) of 2‐MPIMP and P‐2‐MPIMP were found to be ?6.13, ?6.09; ?2.65, ?2.67; and 3.48, 3.42 eV, respectively. Kinetic and thermodynamic parameters of these compounds investigated by MacCallum‐Tanner and van Krevelen methods. The values of the apparent activation energies of thermal decomposition (E_a), the reaction order (n), pre‐exponential factor (A), the entropy change (ΔS*), enthalpy change (ΔH*), and free energy change (ΔG*) were calculated from the TGA curves of compounds. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis,characterization, thermal stability,conductivity, and band gap of a new aromatic polyether containing an azomethine as a side

In this study, the oxidative polycondensation reaction conditions of 4‐[(4‐methylphenyl)iminomethyl]phenol (4‐MPIMP) were studied by using oxidants such as air O₂, H₂O₂, and NaOCl in an aqueous alkaline medium between 50 and 90°C. The structures of the synthesized monomer and polymer were confirmed by FTIR, UV–vis, ¹H–¹³C‐NMR, and elemental analysis. The characterization was made by TGA‐DTA, size exclusion chromatography (SEC), and solubility tests. At the optimum reaction conditions, the yield of poly‐4‐[(4‐methylphenyl)iminomethyl]phenol (P‐4‐MPIMP) was found to be 28% for air O₂ oxidant, 42% for H₂O₂ oxidant, and 62% for NaOCl oxidant. According to the SEC analysis, the number–average molecular weight (M_n), weight–average molecular weight (M_w), and polydispersity index values of P‐4‐MPIMP were found to be 4400 g mol^?1, 5100 g mol^?1, and 1.159, using H₂O₂, and 4650 g mol^?1, 5200 g mol^?1, and 1.118, using air O₂, and 5100 g mol^?1, 5900 g mol^?1, and 1.157, using NaOCl, respectively. According to TG analysis, the weight losses of 4‐MPIMP and P‐4‐MPIMP were found to be 85.37% and 72.19% at 1000°C, respectively. P‐4‐MPIMP showed higher stability against thermal decomposition. Also, electrical conductivity of the P‐4‐MPIMP was measured, showing that the polymer is a typical semiconductor. The highest occupied molecular orbital and the lowest unoccupied molecular orbital energy levels and electrochemical energy gaps (E) of 4‐MPIMP and P‐4‐MPIMP were found to be ?5.76, ?5.19; ?3.00, ?3.24; 2.76 and 1.95 eV, respectively. According to UV–vis measurements, optical band gaps (E_g) of 4‐MPIMP and P‐4‐MPIMP were found to be 3.34 and 2.82 eV, respectively. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Synthesis,characterization, and thermal degradation of oligo‐2‐(morpholinoiminomethyl)phenol and its Pb(II) complex compound

The oxidative polycondensation reaction conditions of 2‐(morpholinoiminomethyl)phenol were studied with H₂O₂, air O₂, and sodium hypochloride (NaOCl) oxidants in an aqueous alkaline medium between 40 and 90°C. The structure of oligo‐2‐(morpholinoiminomethyl)phenol was characterized with ¹H‐ and ¹³C‐NMR, Fourier transform infrared, ultraviolet–visible, size exclusion chromatography, and elemental analysis techniques. Under the optimum reaction conditions, the yield of oligo‐2‐(morpholinoiminomethyl)phenol was 28% for the H₂O₂ oxidant, 12% for the air O₂ oxidant, and 58% for the NaOCl oxidant. According to the size exclusion chromatography analysis, the number‐average molecular weight, weight‐average molecular weight, and polydispersity index of oligo‐2‐(morpholinoiminomethyl)phenol were 2420 g/mol, 2740 g/mol, and 1.187 with H₂O₂, 1425 g/mol, 2060 g/mol, and 1.446 with air O₂, and 1309 g/mol, 1401 g/mol, and 1.070 with NaOCl, respectively. Thermogravimetry/dynamic thermal analysis showed that the oligo‐2‐(morpholinoiminomethyl)phenol–lead complex compound was more stable than 2‐(morpholinoiminomethyl)phenol and oligo‐2‐(morpholinoiminomethyl)phenol against thermal degradation. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102:3795–3804, 2006     

Synthesis,characterization, and thermal stability of azomethine oligomer and its metal complexes

The oxidative polycondensation reaction conditions of N,N′‐bis[(2‐hydroxy‐1‐naphthyl)methylene]urea (2‐HNMU) has been accomplished using NaOCl, H₂O₂, and air O₂ oxidants in an aqueous alkaline medium. The structures of the obtained monomer and oligomer were confirmed by FTIR, UV–vis, ¹H NMR, ¹³C NMR, and elemental analysis. The characterization was made by TG‐DTA, size exclusion chromatography (SEC), and solubility tests. At the optimum reaction conditions, the yield of oligo‐N,N′‐bis[(2‐hydroxy‐1‐naphthyl)methylene]urea (O‐2‐HNMU) was found to be 95% (for air O₂ oxidant), 51% (for H₂O₂ oxidant), 96% (for NaOCl oxidant). According to the SEC analysis, the number‐average molecular weight (M_n), weight‐average molecular weight (M_w), and polydispersity index values of O‐2‐HNMU was found to be 1036, 1225 g/mol, and 1.182, respectively, using H₂O₂, and 765, 1080 g/mol, and 1.412, respectively, using air O₂, and 857, 1105 g/mol, and 1.289, respectively, using NaOCl. TG‐DTA analyses showed that O‐2‐HNMU was more stable than 2‐HNMU. According to TG analyses, the carbonaceous residue of 2‐HNMU and O‐2‐HNMU was found to be 0.49% and 2.11% at 1000°C, respectively. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

The Oxidative Polycondensation of Benzylidene-4′-hydroxyanilene using Air O<Subscript>2</Subscript>, NaOCl and H<Subscript>2</Subscript>O<Subscript>2</Subscript>: Synthesis and Characterization

In this work, the oxidative polycondensation reaction conditions of benzylidene-4′-hydroxyanilene (B-4′-HA) were studied using oxidants such as air O₂, H₂O₂ and NaOCl in an aqueous alkaline medium between 40 and 95 ^○C. Oligo-benzylidene-4′-hydroxyanilene was characterized by ¹H-NMR, FT-IR, UV-Vis, size exclusion chromatography (SEC) and elemental analysis techniques. The solubility of oligomer using organic solvents such as DMF, THF, DMSO, methanol, ethanol, CHCl₃, CCl₄, toluene, acetonitrile, ethyl acetate was investigated. According to air O₂ oxidant (flow rate 8.5 L/h), the conversion of B-4′-HA was 82.0% in optimum conditions such as [B-4′-HA]₀=[KOH]₀=0.1015 mol/L at 50 ^○C for 25 h. According to the SEC analysis, the number-average molecular weight (M_n), weight-average molecular weight (M_w) and polydispersity index (PDI) values of O-B-4′-HA were found to be 1852 g mol⁻¹, 3101 g mol⁻¹ and 1.675; 2123 g mol⁻¹, 4073 g mol⁻¹ and 1.919; 2155 g mol⁻¹, 4164 g mol⁻¹ and 1.932, using air oxygen, NaOCl and H₂O₂ oxidants, respectively. Also, Thermo gravimetric analysis (TGA) showed oligo-benzylidene-4′-hydroxyanilene to be unstable against thermo-oxidative decomposition. The weight loss of O-B-4′-HA was found to be 95.87% at 1000 ^○C.     

Synthesis, characterization and optimum reaction conditions of oligo-2-amino-3-hydroxypyridine and its Schiff base oligomer

The oxidative polycondensation reaction conditions of 2-amino-3-hydroxypyridine (AHP) and 2-[benzilydeneimino] pyridine-3-ol (BIP) were studied by oxidants such as with air O₂, NaOCl and H₂O₂. Oligo-2-amino-3-hydroxypyridine (OAHP) was synthesized from the oxidative polycondensation of AHP with air O₂, NaOCl and H₂O₂ in an aqueous acidic and alkaline medium at 30-90 °C. BIP was synthesized from condensation of 2-amino-3-hydroxypyridine with benzaldehyde. Oligo-2-[benzilydeneimino] pyridine-3-ol (OBIP) was synthesized from the oxidative polycondensation of BIP with air O₂, NaOCl and H₂O₂ in an aqueous alkaline medium at 40-90 °C. About 95% BIP was converted to OBIP. The number average molecular weight, (M_n) weight average molecular weight (M_w) and polydispersity index (PDI) values of OAHP and OBIP (for air O₂ oxidant) were found to be 1433, 1912 g mol⁻¹, 1.33 and 2637, 5106 g mol⁻¹ and 1.94, respectively. At the optimum reaction conditions, the yield of OAHP was found to be 86.0% (for air O₂ oxidant), 43.0% (for H₂O₂ oxidant) and 85.0% (for NaOCl oxidant). At the optimum reaction conditions, the yield of OBIP was found to be 91.0% (for air O₂ oxidant), 92.0% (for H₂O₂ oxidant) and 95.0% (for NaOCl oxidant). The OHAP and OBIP were characterized by FT-IR, UV-Vis, ¹H and ¹³C-NMR elemental analysis. TG and DTA analyses were shown to be unstable of OAHP and OBIP against thermo-oxidative decomposition. According to TG analyses, the weight loss of OAHP and OBIP was found to be 97.35 and 96.60% at 520 and 685 °C, respectively.     

Synthesis,Characterization, and Thermal Degradation of Oligo-2-[(4-Chlorophenyl) Imino Methylene] Phenol and Its Oligomer-Metal Complexes

The oxidative polycondensation reaction conditions of 2-[(4-chlorophenyl) imino methylene] phenol (CPIMP) were studied by air O₂ and NaOCl oxidants at various temperatures and times. Optimum reaction conditions of air O₂ and NaOCl were determined for CPIMP. Oligo-2-[(4-chlorophenyl) imino methylene] phenol (OCPIMP) was synthesized from the oxidative polycondensation of CPIMP with air O₂ and NaOCl in alkaline medium between 50 and 90°C. The number-average molecular weight (M_n) weight-average molecular weight (M_w) and polydispersity index (PDI) values of OCPIMP were found to be 470 g mol^?1, 895 g mol^?1, and 1.90, using NaOCl, and 455 g mol^?1, 765 g mol^?1, and 1.68, using air O₂, respectively. At the optimum reaction conditions, the yield of OCPIMP was found to be 62.80% (for air O₂ oxidant) and 87.50% (for NaOCl oxidant). The OCPIMP was characterized by ¹H-NMR, FT-IR, UV-Vis and elemental analysis. The thermogravimetric (TGA)-DTA analyses were shown to be stable of OCPIMP and its oligomer metal complexes (such as Co⁺², Ni⁺², and Cu⁺²) against thermo-oxidative decomposition. The weight loss of OCPIMP and its oligomer metal complexes (such as Co⁺², Ni⁺², and Cu⁺²) were found to be 98%, 85%, 80%, and 82%, respectively, at 1000°C.     

Synthesis,Crystal Structure,and Thermal Behavior of 3‐(4‐Aminofurazan‐3‐yl)‐4‐(4‐nitrofurazan‐3‐yl)furazan (ANTF)

The energetic material 3‐(4‐aminofurazan‐3‐yl)‐4‐(4‐nitrofurazan‐3‐yl)furazan (ANTF) with low melting‐point was synthesized by means of an improved oxidation reaction from 3,4‐bis(4′‐aminofurazano‐3′‐yl)furazan. The structure of ANTF was confirmed by ¹³C NMR spectroscopy, mass spectrometry, and the crystal structure was determined by X‐ray diffraction. ANTF crystallized in monoclinic system P2₁/c, with a crystal density of 1.785 g cm⁻³ and crystal parameters a=6.6226(9) Å, b=26.294(2) Å, c=6.5394(8) Å, β=119.545(17)°, V=0.9907(2) nm³, Z=4, μ=0.157 mm⁻¹, F(000)=536. The thermal stability and non‐isothermal kinetics of ANTF were studied by differential scanning calorimetry (DSC) with heating rates of 2.5, 5, 10, and 20 K min⁻¹. The apparent activation energy (E_a) of ANTF calculated by Kissinger's equation and Ozawa's equation were 115.9 kJ mol⁻¹ and 112.6 kJ mol⁻¹, respectively, with the pre‐exponential factor lnA=21.7 s⁻¹. ANTF is a potential candidate for the melt‐cast explosive with good thermal stability and detonation performance.     

Influence of technological parameters on the epoxidation of 1‐butene‐3‐ol over titanium silicalite TS‐2 catalyst

BACKGROUND: The influence of technological parameters on the epoxidation of 1‐butene‐3‐ol (1B3O) over titanium silicalite TS‐2 catalyst has been investigated. Epoxidations were carried out using 30%(w/w) hydrogen peroxide at atmospheric pressure. The major product from the epoxidation of B3O was 1,2‐epoxybutane‐3‐ol, with many potential applications. RESULTS: The influence of temperature (20–60 °C), 1B3O/H₂O₂ molar ratio (1:1–5:1), methanol concentration (5–90%(w/w)), TS‐2 catalyst concentration (0.1–6.0%(w/w)) and reaction time (0.5–5.0 h) have been studied. CONCLUSION: The epoxidation process is most effective if conducted at a temperature of 20 °C, 1B3O/H₂O₂ molar ratio 1:1, methanol concentration (used as the solvent) 80%(w/w), catalyst concentration 5%(w/w) and reaction time 5 h. Copyright © 2009 Society of Chemical Industry     

Poly‐2‐[(4‐methylbenzylidene)amino]phenol: Investigation of thermal degradation and antimicrobial properties

A new polyphenol (poly‐2‐[(4‐methylbenzylidene)amino]phenol) (P(2‐MBAP)) containing an azomethine group was synthesized by oxidative polycondensation reaction of 2‐[(4‐methylbenzylidene)amino]phenol (2‐MBAP) with NaOCl, H₂O₂, and O₂ oxidants in an aqueous alkaline medium. The structures of 2‐MBAP and P(2‐MBAP) were characterized by UV‐vis, FT‐IR, and ¹H NMR spectra. While the monomer decomposed completely up to 350°C and 57.2% of the polymer decomposed up to 1000°C. The thermal degradation of P(2‐MBAP) was also supported by the Thermo‐IR spectra recorded in the temperature range of 25–800°C. Electrical conductivity of the polymer was observed to increase 10⁸ fold after doping with I₂. Antimicrobial activities of the P(2‐MBAP) and 2‐MBAP against Sarcina lutea, Enterobacter aerogenes, Escherichia coli, Enterococcus feacalis, Klebsiella pneumoniae, Bacillus subtilis, Candida albicans, and Saccharomyces cerevisiae were also investigated. The number average molecular weight (M_n), weight average molecular weight (M_w) and polydispersity index (PDI) of the polymers were determined by gel permeation chromatography (GPC). © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41758.     

Structural and Preliminary Explosive Property Characterizations of New 3,4,5‐Triamino‐1,2,4‐triazolium (Guanazinium) Salts

Two new highly stable energetic salts were synthesized in reasonable yield by using the high nitrogen‐content heterocycle 3,4,5‐triamino‐1,2,4‐triazole and resulting in its picrate and azotetrazolate salts. 3,4,5‐Triamino‐1,2,4‐triazolium picrate (1) and bis(3,4,5‐triamino‐1,2,4‐triazolium) 5,5′‐azotetrazolate (2) were characterized analytically and spectroscopically. X‐ray diffraction studies revealed that protonation takes place on the nitrogen N1 (crystallographically labelled as N2). The sensitivity of the compounds to shock and friction was also determined by standard BAM tests revealing a low sensitivity for both. B3LYP/6–31G(d, p) density functional (DFT) calculations were carried out to determine the enthalpy of combustion (Δ_cH (1) =−3737.8 kJ mol⁻¹, Δ_cH (2) =−4577.8 kJ mol⁻¹) and the standard enthalpy of formation (Δ_fH° (1) =−498.3 kJ mol⁻¹, (Δ_fH° (2) =+524.2 kJ mol⁻¹). The detonation pressures (P (1) =189×10⁸ Pa, P (2) =199×10⁸ Pa) and detonation velocities (D (1) =7015 m s⁻¹, D (2) =7683 m s⁻¹) were calculated using the program EXPLO5.     

The synthesis and characterization of oligo-N-4-aminopyridine, oligo-2-[(pyridine-4-yl-imino) methyl] phenol and its some oligomer-metal complexes

The product and the oxidative polycondensation reaction conditions of oligo-4-aminopyridine were studied by using NaOCl as oxidant. Oligo-4-aminopyridine (4-OAP) was synthesized from the oxidative polycondensation of 4-aminopyridine (4-AP) in an aqueous solution medium acidic and neutral between 25 and 60 °C by using NaOCl as oxidant. About 85% of 4-AP was converted to 4-OAP. The number average molecular weight, (M_n) mass average molecular weight (M_w) and polydispersity index (PDI) values of 4-OAP synthesized were found to be 270, 850 g mol⁻¹ and 3.15, respectively, using NaOCl. The respective values of the Schiff base were 1721, 2256 g mol⁻¹ and 1.31, respectively, using air oxygen and 2173, 2372 g mol⁻¹ and 1.09, respectively, using NaOCl and 2749, 6432 g mol⁻¹ and 2.33, respectively, using H₂O₂. At the optimum reaction conditions, the yield of oligo-2-[(pyridine-4-yl-imino) methyl] phenol (OPMP) were found to be 86% (H₂O₂) and 89% (NaOCl) and 95% (air oxygen). The 4-OAP and OPMP were characterized by ¹H NMR, FT-IR, UV-Vis and elemental analysis. TG analysis showed to be stable of 4-OAP against thermo-oxidative decomposition. The weight loss of 4-OAP and its Schiff base oligomer was found to be 50, 86.39 and 71.78% at 525, 625 and 1000 °C, respectively. Also, new oligomeric Schiff base was synthesized from condensation of 4-AP with salicylaldehyde and their structures and properties were determined. During polycondensation reaction, a part of the azomethine (-CHN-) groups oxidized to carboxylic (-COOH) group. Thus, soluble fraction in water of oligo-2-[(pyridine-4-yl-imino) methyl] phenol involved in carboxylic (-COOH) (11%) group. Besides, the structure and properties of oligomer-metal complexes of oligo-2-[(pyridine-4-yl-imino) methyl] phenol (OPMP) with Cu(II), Ni(II) and Co(II) were studied.     

Synthesis,Characterization and Conductivity Properties of Novel Oligomer Schiff Bases Derived from 4-Amino-3-hydrazino-5-mercapto-1, 2, 4-triazole and Their Reactions with VO(IV), Cu(II) Ions

A new Schiff base, 4-(4-hydroxysalicylidenamino)-3-hydrazino-5-mercapto-1,2,4-triazole (4HSAHMT), and novel Schiff base oligomers of 4-salicylidenamino-3-hydrazino-5-mercapto-1,2,4-triazole (SAHMT), 4-(2-hydroxynaphthylidenamino)-3-hydrazino-5-mercapto-1,2,4-triazole (2HNAHMT), 4-(4-hydroxysalicylidenamino)-3-hydrazino-5-mercapto-1,2,4-triazole (4HSAHMT) and 4-(5-bromosalicylidenamino)-3-hydrazino-5-mercapto-1,2,4-triazole (BrSAHMT) were synthesized via oxidative polymerization using NaOCl as the oxidant. The structures of the oligomers were supported by FT-IR, UV–Vis, ¹H-NMR, and ¹³C-NMR techniques. The compounds were further characterized by solubility tests, TG–DTA, and elemental analysis. The molecular weight distribution parameters of the compounds were determined by the size exclusion chromatography (SEC). According to SEC, the number average molecular weight (M _n ) values of O-SAHMT, O-BrSAHMT, O-4HSAHMT and O-2HNAHMT were 2,700, 2,100, 2,700 and 1,000 g mol^?1, respectively. The weight losses of O-SAHMT, O-BrSAHMT, O-4HSAHMT and O-2HNAHMT were 73, 76, 80 and 54 %, respectively, at 1,000 °C. TG analyses showed that the synthesized oligomers were stable toward thermal decomposition. The synthesized oligomers were converted to metal complexes with salts of VO(IV) and Cu(II). The doped and undoped electrical properties of oligomers and oligomer–metal complexes were determined by the four-point probe technique at room temperature and atmospheric pressure.     

Synthesis and spectroelectrochemistry of dithieno(3,2‐b:2′,3′‐d)pyrrole derivatives

New π‐conjugated polymers containing dithieno(3,2‐b:2′,3′‐d)pyrrole (DTP) were successfully synthesized via electropolymerization. The effect of structural differences on the electrochemical and optoelectronic properties of the 4‐[4H‐dithieno(3,2‐b:2′,3′‐d)pyrrol‐4‐yl]aniline (DTP–aryl–NH₂), 10‐[4H‐dithiyeno(3,2‐b:2′,3′‐d)pirol‐4‐il]dekan‐1‐amine (DTP–alkyl–NH₂), and 1,10‐bis[4H‐dithieno(3,2‐b:2′,3′‐d)pyrrol‐4‐yl] decane (DTP–alkyl–DTP) were investigated. The corresponding polymers were characterized by cyclic voltammetry, NMR (¹H‐NMR and ¹³C‐NMR), and ultraviolet–visible spectroscopy. Changes in the electronic nature of the functional groups led to variations in the electrochemical properties of the π‐conjugated systems. The electroactive polymer films revealed redox couples and exhibited electrochromic behavior. The replacement of the DTP–alkyl–DTP unit with DTP–aryl–NH₂ and DTP–alkyl–NH₂ resulted in a lower oxidation potential. Both the poly(10‐(4H‐Dithiyeno[3,2‐b:2′,3′‐d]pirol‐4‐il)dekan‐1‐amin) (poly(DTP–alkyl–NH₂)) and poly(1,10‐bis(4H‐dithieno[3,2‐b:2′,3′‐d]pyrrol‐4‐yl) decane) (poly(DTP–alkyl–DTP)) films showed multicolor electrochromism and also fast switching times (<1 s) in the visible and near infrared regions. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40701.     

Polymerization of cyclic monomers. VII. Synthesis and radical polymerization of 1,3‐bis[(1‐alkoxycarbonyl‐2‐vinylcyclopropane‐1‐yl)carboxy]benzenes

1,3‐Bis[(1‐alkoxycarbonyl‐2‐vinylcyclopropane‐1‐yl)carboxy]benzenes 1 [RO: CH₃O (a), C₂H₅O (b)] were synthesized by the esterification of the corresponding 1‐alkoxycarbonyl‐2‐vinylcyclopropane‐1‐carboxylic acids with resorcinol. The structure of the new vinylcyclopropanes was confirmed by elemental analysis and infrared (IR), ¹H nuclear magnetic resonance (¹H‐NMR), and ¹³C nuclear magnetic resonance (¹³C‐NMR) spectroscopy. The radical polymerization of difunctional 2‐vinyl‐cyclopropanes in bulk with 2,2′‐azoisobutyronitrile (AIBN) results in hard, transparent, crosslinked polymers. During the bulk polymerization of the crystalline bis[(1‐methoxycarbonyl‐2‐vinylcyclopropane‐1‐yl)carboxy]benzene 1a, an expansion in volume of about 1% took place. The radical solution polymerization of 1a resulted in a soluble polymer with pendant 2‐vinylcyclopropane groups. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 1775–1782, 1999     

Fabrication of BaZr0.1Ce0.7Y0.2O3 – δ ‐Based Proton‐Conducting Solid Oxide Fuel Cells Co‐Fired at 1,150 °C

Dense proton‐conducting BaZr_0.1Ce_0.7Y_0.2O_{3 – δ} (BZCY) electrolyte membranes were successfully fabricated on NiO–BZCY anode substrates at a low temperature of 1,150 °C via a combined co‐press and co‐firing process. To fabricate full cells, the LaSr₃Co_1.5Fe_1.5O_{10 – δ}–BZCY composite cathode layer was fixed to the electrolyte membrane by two means of one‐step co‐firing and two‐step co‐firing, respectively. The SEM results revealed that the cathode layer bonded more closely to the electrolyte membrane via the one‐step co‐firing process. Correspondingly, determined from the electrochemical impedance spectroscopy measured under open current conditions, the electrode polarisation and Ohmic resistances of the one‐step co‐fired cell were dramatically lower than the other one for its excellent interface adhesion. With humidified hydrogen (2% H₂O) as the fuel and static air as the oxidant, the maximum power density of the one‐step co‐fired single cell achieved 328 mW cm^–2 at 700 °C, showing a much better performance than that of the two‐step co‐fired single cell, which was 264 mW cm^–2 at 700 °C.     

Efficient synthesis of organic carbonates and poly(1,4‐butylene carbonate‐co‐terephthalate)s

Dimethyl carbonate (DMC) is an environmentally benign chemical currently produced using CO₂. Using the conventional Dean–Stark apparatus, a method was developed for the effective and selective removal of the methanol generated in the transesterification of DMC with alcohol. Using this device, various diols (HO‐A‐OH; A = (CH₂)₄, (CH₂)₂O(CH₂)₂, CH₂C₆H₁₀CH₂, and CH₂C₆H₄CH₂) were converted to mixtures of the corresponding MeOC(O)[O‐A‐OC(O)]OMe and MeOC(O)[O‐A‐OC(O)]₂OMe. Dialkyl carbonates such as dibutyl carbonate, dibenzyl carbonate, and diallyl carbonate were also efficiently prepared from the corresponding alcohols using this device. The compound prepared from 1,4‐butanediol, MeOC(O)[O(CH₂)₄OC(O)]_1.5OMe, was subjected to polycondensation with HO(CH₂)₄[O₂CC₆H₄CO₂(CH₂)₄]_1.5OH or HO(CH₂)₄[O₂CC₆H₄CO₂(CH₂)₄]_1.8OH, which directly was prepared from terephthalic acid and 1,4‐butanediol. The polycondensation afforded high‐molecular‐weight poly(1,4‐butylene carbonate‐co‐terephthalate)s (PBCTs) with M_w of 80–270 kDa and 0.40–0.46 terephthalate mole fractions. PBCTs are attractive materials with potential biodegradability and LDPE‐like thermal properties. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44951.     

Synthesis,characterization, and kinetic of thermal degradation of oligo‐2‐[(4‐bromophenylimino)methyl]phenol and oligomer‐metal complexes

Oligo‐2‐[(4‐bromophenylimino)methyl]phenol (OBPIMP) was synthesized from the oxidative polycondensation reaction of 2‐[(4‐bromophenylimino)methyl]phenol (BPIMP) with air and NaOCl oxidants in an aqueous alkaline medium between 50 and 90°C. The yield of OBPIMP was found to be 67 and 88% for air and NaOCl oxidants, respectively. Their structures were confirmed by elemental and spectral such as IR, ultraviolet–visible spectrophotometer (UV–vis), ¹H‐NMR, and ¹³C‐NMR analyses. The characterization was made by TG‐DTA, size exclusion chromatography, and solubility tests. The resulting complexes were characterized by electronic and IR spectral measurements, elemental analysis, AAS, and thermal studies. According to TG analyses, the weight losses of OBPIMP, and oligomer‐metal complexes with Co⁺², Ni⁺², and Cu⁺² ions were found to be 93.04%, 59.80%, 74.23%, and 59.30%, respectively, at 1000°C. Kinetic and thermodynamic parameters of these compounds investigated by Coats‐Redfern, MacCallum‐Tanner, and van Krevelen methods. The values of the apparent activation energies of thermal decomposition (E_a), the reaction order (n), preexponential factor (A), the entropy change (ΔS*), enthalpy change (ΔH*), and free energy change (ΔG*) obtained by earlier‐mentioned methods were all good in agreement with each other. It was found that the thermal stabilities of the complexes follow the order Cu(II) > Co(II) > Ni(II). © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Kinetic study of the thermal decomposition of (2‐phenyl‐1,3‐dioxolane‐4‐yl) methyl methacrylate and 2‐hydroxyethyl methacrylate copolymers

The kinetics of nonisothermal decomposition of (2‐phenyl‐1,3‐dioxolane‐4‐yl) methyl methacrylate (PDMMA), 2‐hydroxyethyl methacrylate (HEMA), and vinyl‐pyrrolidone (VPy) copolymers were investigated by thermogravimetry (TG) and differential thermal analysis (DTA). The data indicated that the major weight loss occurs in the range of 270 to 450°C. The decomposition characteristics showed essentially two regimes and varied depending on the temperature and the copolymer composition. The apparent kinetic parameters of the decompositions were estimated from both TG and DTA data by using the alternative calculation methods. The results suggest that the weight loss rates may be represented, depending on the type of sample, by a reaction model of overall order 1.0 to 1.6, with an activation energy of approximately 65–95 kJ mol^?1. The DTA data estimated considerably higher values for the overall activation energies, around 198–240 kJ mol^?1. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 1500–1508, 2005     

Synthesis of oligo‐ortho‐azomethinephenol and its oligomer–metal complexes: Characterization and application as anti‐microbial agents

The oxidative polycondensation reaction conditions and optimum parameters of o‐phenylazomethinephenol (PAP) with oxygen (air) and NaOCl were determined in an aqueous alkaline solution at 60–98°C. The properties of oligo‐o‐phenylazomethinephenol (OPAP) were studied by chemical and spectra analyses. PAP was converted to dimers and trimers (25–60%) by oxidation in an aqueous alkaline medium. The number average molecular weight (M_n), mass average molecular weight (M_w), and polydispersity index (PDI) values were 1180 g mol^?1, 1930 g mol^?1, and 1.64, respectively. According to these values, 20–33% of PAP turned into OPAP. During the polycondensation reaction, a part of the azomethine (? CH?N? ) groups oxidized to carboxylic (? COOH) group. Thus, a water‐soluble fraction of OPAP was incorporated in the carboxylic (? COOH); (2–20%) group. Also, the structure and properties of oligomer–metal complexes of OPAP with Cu(II), Ni(II), Zn(II), and Co(II) were studied. Antimicrobial activites of the oligomer and its oligomer–metal complexes were tested against B. cereus, L. monocytogenes, B. megaterium, B. subtilis, E. coli, Str. thermophilus, M. smegmatis, B. brevis, E. aeroginesa, P. vulgaris, M. luteus, S. aureus, and B. jeoreseens. Also, according to differential thermal analysis and thermogravimetric analysis, OPAP and its oligomer–metal complexes were stable throughout to temperature and thermo‐oxidative decomposition. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2004–2013, 2002