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- Author or Editor: X. Sheng x
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Isothermal cure characterization of dicyclopentadiene
The glass transition temperature and conversion
Abstract
Conversion (α) and the glass transition temperature (T g) were investigated during the isothermal cure of endo-dicyclopentadiene (DCPD) with a Grubbs catalyst for different temperatures using differential scanning calorimetry. Conversion vs. In (time) data at an arbitrary reference temperature were superposed by horizontal shift and the shift factors were used to calculate an Arrhenius activation energy. Glass transition temperature vs. conversion data fell on a single curve independent of cure temperature, implying that reaction of the norbornene and cyclopentene ring of DCPD proceeds in a sequential fashion. Implications of the isothermal reaction kinetics for self-healing composites are discussed.
Abstract
The addition of suitable cross-linking agents with norbornene-based monomers has significant effects on the thermal properties of the resulting polymers formed by olefin metathesis. Ethylidene norbornene (ENB) and endo-dicyclopentadiene (endo-DCPD) were mixed separately with various loadings of three different cross-linking agents and then polymerized with the addition of Grubbs’ catalyst. The polymerization kinetics and resulting glass transition temperature (T g) of the systems were evaluated by differential scanning calorimetry (DSC). The addition of the first cross-linking agent, norbornadiene (CL-1), to both endo-DCPD and ENB resulted in decreasing glass transition temperatures with increasing concentrations. In contrast, the addition of the other two cross-linking agents (CL-2 and CL-3), which were both custom synthesized bifunctional norbornyl systems, to both endo-DCPD and ENB resulted in a monotonic increases in T g with cross-linker concentration. By tailoring the loading of these custom cross-linking agents, the properties of these polymer systems can be controlled for various applications, including self-healing composites.
Abstract
Resin injection repair is a common method to repair delamination damage in polymer matrix composites (PMCs). To repair high-temperature PMCs, the resin should have a very low viscosity, yet cure into a compatible adhesive with high temperature stability. Normally, thermosetting polymers with high glass transition temperatures (T g) are made from monomers with high room temperature viscosities. Among the high temperature resins, bisphenol E cyanate ester (BECy, 1,1’-bis(4-cyanatophenyl)ethane), is unique because it has an extremely low viscosity of 0.09–0.12 Pa s at room temperature yet polymerizes as a cross-linked thermoset with a high T g of 274°C. BECy monomer is cured via a trimerization reaction, without volatile products, to form the high T g amorphous network. In this study, the cure kinetics of BECy is investigated by differential scanning calorimetry (DSC). Both dynamic and isothermal experiments were carried out to obtain the kinetic parameters. An autocatalytic model was successfully used to model isothermal curing. The activation energy from the autocatalytic model is 60.3 kJ mol−1 and the total reaction order is about 2.4. The empirical DiBenedetto equation was used to evaluate the relationship between T g and conversion. The activation energy of BECy from the dynamic experiments is 66.7 kJ mol−1 based on Kissinger’s method, while isoconversional analysis shows the activation energy changes as the reaction progresses.
Abstract
A radioactive multitracer solution obtained from the nuclear reaction of selenium with 25 MeV/nucleon40Ar ions was applied to the investigation of the trace elements behavior in feces and urine of mouse. The excretion rates of 23 elements, Na, K, Rb, Mg, Ca, Sr, Ga, As, Sc, V, Cr, Mn, Co, Fe, Zn, Y, Zr, Mo, Nb, Tc, Ru, Ag and In were simultaneously detected under strictly identical experimental conditions, in order to clarify the excretion behavior of the elements in mice. Fecal and urinary excretion rates of the elements in mice reached the highest value separately at 48 and 24 hours. The total excretion of Mo, Tc and Co within 96 hours were all larger, more than 60%. Accumulative excretion rates of Ca, Nb, Mg, Sr, V, Sc, Na, Cr, Fe, Ag, Mn and Zr were 60-30%. The total rates of Ru, K, As, Zn, Rb, Y, Ga and In were less than 30%, and low excretion. The main excretion pathway of Mo, Co, Mg, Fe and Ag was through urine, and Na, K, As and Rb were eliminated from the body also in urine. But fecal excretion of Tc, Nb, Sr, Y, Ru, and In were larger than urinary excretion, and Ca, Sc, Mn, Zr, Zn were eliminated from the body in feces.
Abstract
The complex from reaction of neodymium chloride six-hydrate with salicylic acid and 8-hydroxyquinoline, Nd(C7H5O3)2·(C9H6NO), was synthesized and characterized by IR, elemental analysis, molar conductance, and thermogravimatric analysis. The standard
molar enthalpies of solution of [NdCl3·6H2O(s)], [2C7H6O3(s)], [C9H7NO(s)] and [Nd(C7H5O3)2·(C9H6NO)(s)] in a mixed solvent of anhydrous ethanol, dimethyl formamide (DMF) and perchloric acid were determined by calorimetry at
298.15 K. Based on Hess’ law, a new chemical cycle was designed, and the enthalpy change of the reaction
((1))
A new, sensitive, and selective high-performance liquid chromatography-tandem mass spectrometric method (HPLC-MS/MS) has been developed for the quantification of six flavonoids (sophoricoside, genistin, genistein, rutin, quercetin, and kaempferol) in rat bile and urine. The sample pretreatment was simple by liquid-liquid extraction. Sulfamethalazole was used as internal standard (IS). During method development, the effect of extraction volume, mobile phase composition, column temperature, and injection volume were varied to optimize sensitivity and achieve a run time as short as possible. Chromatographic separation was accomplished on a C18 column with a simple linear gradient elution within 9 min. Full validation of the assay was in accordance with the requirement of the validation of the method in vivo and implemented including specificity, linearity, accuracy, precision, recovery, and matrix effect. This is the first report on determination of the major flavones in rat bile and urine after oral administration of Fructus Sophorae extract. The method has been used successfully in excretion studies of six major flavonoids in rat bile and urine.