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Abstract  

Differential scanning calorimetry was used to study the influence of an epoxy reactive diluent, vinylcyclohexane dioxide, on the curing reaction of a polymeric system composed of diglycidyl ether of bisphenol A (n=0) and 1,2-diaminecyclohexane (DCH). Heat evolution and glass transition temperature, were measured in terms of the added diluent percentage. Experimental results show that both the curing degree and the glass transition temperature of the polymeric system decrease with an increase in the diluent percentage. Dynamic mechanical analysis of several samples also showed that T g decreases with the increase of diluent percentage, thus corroborating DSC measurements.

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Abstract  

Thermal behaviour of blends based on N,N'-bis(4-itaconimidophenyl) ether (IE) and 4,4'-bis(4-allyl-2-methoxyphenoxy) benzophenone (R1) or 4,4'-bis(2-allylphenoxy) benzophenone (R2) are described in this paper. The reactive diluent content was varied from 5-50% (mass/mass) in these blends. A decrease in the melting point and exothermic peak temperature was observed with increasing mass percent of reactive diluent. Thermal stability of blends was affected at high mass percentage of reactive diluents.

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Different formulations, composed of the diglycidyl ether of bisphenol-A, diepoxidized cardanol as reactive diluent, an anhydride as curing agent, and a tertiary amine as curing catalyst, with/without the use of an epoxy fortifier, were analysed. The effect of the fortifier on the diluent was also observed. The overall kinetics of curing was observed to follow a simple Arrhenius-type temperaturedependence, with an activation energy in the range 54–120 kJ/mol, with first-order kinetics up to 85% conversion. An increase in activation energy was observed with an increase of diluent content. The curing reaction was found to follow a three-step mechanism, involving a nucleophilic bimolecular displacement reaction, for which an explanation was offered. Incorporation of the fortifier lowers the curing temperature, but does not alter the final degree of reaction.

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Abstract  

The rheological behaviour of the materials diglycidil ether of bisphenol A (n = 0), 1, 2 diamine-cyclohexane and the epoxy reactive diluent vinylcyclohexane dioxide have been studied both separately and mixed before the beginning of the curing reaction. Different kinds of tests such as: preshear and time sweep, flow curve and stress sweep experiments were carried out. From these experiments, interesting information about: viscosity-shear stress and viscosity-shear rate dependences, storage modulus and the linear viscoelastic region were found out. Relationships between concentration of diluent and the final viscosity of the mixed sample and also between percentage of diluent and storage modulus were studied.

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Abstract  

Structural relaxation in different epoxy-anhydride and epoxy-diamine resins has been investigated by differential scanning calorimetry using annealing and cooling rate experiments. The annealing experiments lead to the determination of enthalpy loss,δH, at an equivalent annealing temperatureT a=T g-20, and for periods of annealing time, ta, between 1 h and 4 months. The variation ofδH with logta, defines a relaxation rate per decade,rrpd, which is very sensitive to changes of the epoxy network. The cooling rate experiments allow the determination of the apparent activation energy,δh *. The effect of the degree of crosslinking, the addition of a reactive diluent, which acts as flexibilizer, and the length of cross-link onrrpd and δh* was studied.

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Abstract  

The thermal degradation of the epoxy system diglycidyl ether of bisphenol A (BADGE n=0)/1,2-diamine cyclohexane (DCH) containing different concentrations of an epoxy reactive diluent was studied by thermogravimetric analysis in order to determine the reaction mechanism of the degradation process and to compare it with the results for the same system without diluent. The value of the activation energy, necessary for this study, was calculated using various integral and differential methods. Values obtained using the different methods were compared to the value obtained by the Flynn-Wall-Ozawa"s method (between 193-240 kJ mol-1 depending on the diluent concentration) with does not require a knowledge of the nth order reaction mechanism. All the experimental results were compared to master curves in the range of Doyle"s approximation (20-35% of conversion). Analysis of the results suggests that the reaction mechanism could be F2, F3, or A2 type.

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Journal of Thermal Analysis and Calorimetry
Authors: Bimlesh Lochab, Indra Varma, and Jayashree Bijwe

Abstract  

A novel benzoxazine monomer (Bz-C) based on agrochemical renewable resource—cardanol (by-product of cashew nut tree, Anacardium occidentale) was synthesized. Bz-C, a liquid monomer, was used as reactive diluent for the solventless synthesis of bisphenol-A benzoxazine monomer (Bz-A). Benzoxazine monomer based on cardanol and bisphenol-A in 3:1, 1:1 and 1:3 blend ratio were prepared by this method. The resins had Brookfield viscosity at 316 K in the range of 145–81,533 mPa s. The resins were characterized by 1H-NMR, FTIR and elemental analysis. Curing characteristics were studied by DSC analysis. Thermal stability of cured resins was found to improve with increase in Bz-C content in the blends.

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The curing behaviour of bismethacryloxy derivative of diglycidyl ether of bisphenol A (vinyl ester resin) containing styrene as the reactive diluent (40% w/w) was studied using gel point determination method and DSC. Seven samples of styrene/α-methylstyrene in the ratio 40∶0, 35∶5, 30∶10, 25∶15, 20∶20, 15∶25 and 0∶40 were studied. Delayed curing was observed in samples containing increasing proportions of α-methylstyrene. The energy of activation decreased from 869 kJ mol−1 to 333 kJ mol−1 as the concentration of α-methylstyrene increased in the formulations. However, no difference in thermal stability was observed by replacement of styrene by α-methylstyrene. It was concluded that in vinyl ester resin samples 10–15% α-methylstyrene and 30-25% styrene can be used as reactive diluent.

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TG, DTG, DTA and DSC methods were used to study the curing reaction of diglycidyl ether of bisphenol A and nadic methyl anhydride in the presence of a reactive diluent. DTG plots were used to identify the various stages of weight loss arising from volatilization of components from the resin formulation and pyrolysis of cured resin. DTA and DSC results established the temperatures at which catalysed and thermally activated cure occurred.

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