Studies on the curing kinetics of epoxy resins using mixture of nadic/or maleic anhydride and 4,4′-diaminodiphenyl sulfone

Curing kinetics of diglycidyl ether of bisphenol-A (DGEBA) in the presence of maleic anhydride (MA)/or nadic anhydride (NA) or mixture of MA/NA: 4,4′-diaminodiphenyl sulfone (DDS) in varying molar ratios were investigated using differential scanning calorimetry. Curing behaviour of DGEBA in the presence of varying amounts of DDS:MA/NA was evaluated by recording DSC scans at heating rates of 5, 10, 15 and 20°C min⁻¹. The peak exotherm temperature depends on the heating rate, structure of the anhydride as well as on the ratio of anhydride: DDS. Thermal stability of the isothermally cured resins was evaluated by thermogravimetry. The char yield was highest in case of resins cured using mixture of DDS:MA (0.75:0.25; sample EM-1) and DDS:NA (0.75:0.25, sample EN-1).     

Some compounds of iron(III) with bidentate bases

Summary The iron(III) compound, FeCl(OH)(MeCO₂) · MeCO₂H · 0.5 H₂O, (1), interacts with the sample bidentate ligand, 2,2-bipyridyl (bipy), to form an aduct, Fe₂Cl₂(OH)₂(MeCO₂)₂ · (bipy). By the loss of protons, anthranilic (anthH) and salicylic (salH₂) acids behave as uninegative charged ligands to give FeCl(anth)₂ · H₂O and FcCl(salH)₂ · H₂O, respectively. The former decomposes on heatingin vacuo to form Fe₂O(anth)₄ while the latter yields Fe₂O(sal)₂. Acetylacetone (acacH) and 8-hydroxyquinoline (quinH) give FeCl(acac)₂ and FeCl(quin)₂ · (quinH). The latter desolvates at 140°/10^–4 torr to form FeCl(quin)₂. l.r. spectra, thermal decomposition, molar conductance and magnetic susceptibility studies at room temperature have been used to characterize these compounds.     

Binuclear iron(III) acetates

Summary The binuclear iron(III) compound, Fe₂Cl(OH)₂(MeCO₂)₃ 2 AcOH combines with pyridine, -picoline and 2,2-bipyridyl (B) to form Fe₂Cl(OH)₂(AcO)₃·B adducts. The secondary bases, pyrrolidine and diethylamine (RNH), on the other hand, combine with the complete elimination of chlorine to form, Fe₂(NR)(OH)₂(AcO)₃. These products have been characterised by molecular weight, i.r. spectra, magnetic susceptibility and Mössbauer measurements.     

1,1,1,1-Tetrakis(o-fluorophenylamino)silane tris[titanium(IV) chloride]. Evidence for a new titanium cation [Ti2Cl7]+

Si(NHC₆H₄F-o)₄ · 3TiCl₄ (1) has been obtained from the disproportionation of (CF₃CH₂O)₃SiNHC₆H₄F-o and TiCl₄ in petroleum ether (40–60 °C) at –10 °C. The analytical (elemental analysis, molar conductance) and spectral (i.r., ¹H- and ¹⁹F-n.m.r.) data suggested that (1) behaves as [Si(NHC₆H₄F-o)₄ · Ti₂Cl₇]⁺ [TiCl₅]^–. The presence of these ions has been confirmed by characterising the products of metathetical reactions of (1) with R₄NX (R = Bu and Et; X = I and Br) and with AgNO₃. The data suggest the presence of a new titanium cation [Ti₂Cl₇]⁺.     

Convenient Microwave-Assisted Chlorosulfonic Acid-Catalyzed Synthesis of Some Quinazolinones from 2-Phenylindole

Russian Journal of Organic Chemistry - A new convenient method has been developed for the synthesis of quinazolinones from 2-phenyl-1H-indole and substituted amines under catalysis by...     

Curing and thermal behaviour of a flame retardant cycloaliphatic epoxy resin based on phosphorus containing poly(amide–imide)s

The curing behaviour of 3,4-epoxycyclohexylmethyl 3,4-epoxycyclohexane carboxylate was investigated by the dynamic differential scanning calorimetry (DSC) using phosphorus-containing poly(amide–imide)s (PAIs) having free amine groups, 4,4′-diaminodiphenylmethane (PM) and p-phenylenediamine (PA), in the ratio of 1:1. The PAIs were prepared by co-polymerization of diimide–diacid (DIDA) and phosphorus-containing triamines having phenylene moiety. l-Tryptophan and pyromellitic anhydride were used to synthesize DIDA. Triamines used in the synthesis PAIs were tris(3-aminophenyl) phosphine (TAP), tris(3-aminophenyl) phosphine oxide (TAPO) and bis(3-aminophenyl) aminotolyl phosphine (BAP). TAP-, TAPO- and BAP-containing PAIs were designated as PTAP, PTAPO and PBAP, respectively. These PAIs with free amine groups were characterized by FTIR, ¹H NMR, ¹³C NMR spectroscopic techniques and elemental analysis. The mixture of PAIs and PM or/and PA in the ratios of 0:1, 1:0 and 0.5:0.5 was used for investigation. DSC was used to study the curing of epoxy by recording the DSC scans at heating rates of 10 °C min^?1. Thermal stability of epoxy resin cured isothermally was evaluated by recording thermo gravimetric traces in nitrogen atmosphere at the heating rate of 20 °C min^?1. All samples are highly stable, and the 10 % mass loss found was in the range of 335–520 °C. The percent char yield was highest in case of resin sample E/PM/PTAPO. The flame-retardant properties of cured epoxy resins were investigated by the limiting oxygen index test (LOI) and UL94 test. When phosphorus was incorporated in epoxy resin, the epoxy resin system met the UL94 V-0 classification and the LOI reached at 37.8, because of nitrogen–phosphorus synergistic effect.     

Binuclear iron(III) compounds with bidentate bases

Summary Binuclear iron(III) derivatives, Fe₂Cl(anth)₅, Fe₂Cl(salH)₅, Fe₂Cl(acac)₅ and Fe₂Cl(quin)₅ · quinH have been prepared by reacting Fe₂Cl(OH)₂(AcO)₃ · 2AcOH with anthranilic acid (anthH), salicylic acid (salH₂), acetylacetone (acacH) and 8-hydroxyquinoline (quinH), respectively. These compounds have been characterised by molecular weight, conductance, i.r. spectral, magnetic susceptibility and Mössbauer measurements.     

Studies on the curing and thermal behaviour of diglycidyl ether of bisphenol-A (DGEBA) in the presence of aromatic diimide–diacids

This paper describes the synthesis and characterization of aromatic diimide–diacids (DIDAS) obtained by reacting pyromellitic dianhydride (PMDA), 4,4′-oxo diphthalic anhydride (ODA), 1,4,5,8-naphthalene tetra carboxylic dianhydride (NTDA) with excess of 4-aminobutyric acid (B) or 6-aminohexanoic acid (H) using N,N-dimethyl formamide (DMF) as solvent. The synthesized compounds were used as curing agents to investigate the effect of structure on the curing and thermal behaviour of diglycidyl ether of bisphenol-A (DGEBA). Structural characterization of DIDAS was done by using FTIR, ¹H-NMR, ¹³C-NMR spectroscopy and elemental analysis. Curing behaviour of DGEBA in the presence of aromatic DIDAS was investigated by differential scanning calorimetry (DSC). The peak exotherm temperature (T _P) was low in the case of DIDAS synthesized from ODA and high in the case of DIDAS synthesized from NTDA. Thermal stability of the isothermally cured DGEBA with DIDAS was investigated using dynamic thermogravimetry in nitrogen atmosphere. The char yield was highest for resin cured with DIDAS containing NTDA.     

Cardiac magnetic resonance imaging: infarct size is an independent predictor of mortality in patients with coronary artery disease

Background

Cardiac magnetic resonance imaging (CMR) can accurately determine infarct size. Prior studies using indirect methods to assess infarct size have shown that patients with larger myocardial infarctions have a worse prognosis than those with smaller myocardial infarctions.

Objectives

This study assessed the prognostic significance of infarct size determined by CMR.

Methods

Cine and contrast CMR were performed in 100 patients with coronary artery disease (CAD) undergoing routine cardiac evaluation. Infarct size was determined by planimetry. We used Cox proportional hazards regression analyses (stepwise forward selection approach) to evaluate the risk of all-cause death associated with traditional cardiovascular risk factors, symptoms of heart failure, medication use, left ventricular ejection fraction, left ventricular mass, angiographic severity of CAD and extent of infarct size determined by CMR.

Results

Ninety-one patients had evidence of myocardial infarction by CMR. Mean follow-up was 4.8±1.6 years after CMR, during which time 30 patients died. The significant multivariable predictors of all-cause mortality were extent of myocardial infarction by CMR, extent of left ventricular systolic dysfunction, symptoms of heart failure, and diabetes mellitus (P<.05). The presence of infarct greater than or equal to 24% of left ventricular mass and left ventricular ejection fraction less than or equal to 30% were the most optimal cut-off points for the prediction of death with bivariate adjusted hazard ratios of 2.11 (95% confidence interval 1.02-4.38) and 4.06 (95% confidence interval 1.73-9.54), respectively.

Conclusions

The extent of myocardial infarction determined by CMR is an independent predictor of death in patients with CAD.     

Imprinted silica nanoparticles coated with N‐propylsilylmorpholine‐4‐carboxamide for the determination of m‐cresol in synthetic and real samples

m‐Cresol‐imprinted silica nanoparticles coated with N‐propylsilylmorpholine‐4‐carboxamide have been developed that contain specific pockets for the selective uptake of m‐cresol. Silica nanoparticles were synthesized by a sol–gel process followed by functionalization of their surface with N‐propylsilylmorpholine‐4‐carboxamide. The formation of m‐cresol‐imprinted silica nanoparticles was confirmed by UV‐Vis spectrophotometry, infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy and transmission electron microscopy. Electron microscopic studies revealed the formation of monodispersed imprinted silica nanoparticles with spherical shape and an average size of 83 nm. The developed nanoparticles were filled in a syringe and used for the extraction of m‐cresol from aqueous samples followed by quantification using high‐performance liquid chromatography with diode array detection. Various adsorption experiments showed that developed m‐cresol‐imprinted silica nanoparticles exhibited a high adsorption capacity and selectivity and offered a fast kinetics for rebinding m‐cresol. The chromatographic quantification was achieved using mobile phase consisting of acetonitrile/water (70:30 v/v) at an isocratic flow rate of 1.0 mL/min using a reversed‐phase C₁₈ column and detection at λ_max = 275 nm. The limits of detection and quantification were 1.86 and 22.32 ng/mL, respectively, for the developed method. The percent recoveries ranged from 96.66–103.33% in the spiked samples. This combination of this nanotechnique with molecular imprinting was proved as a reliable, sensitive and selective method for determining the target from synthetic and real samples.