Kinetics of the Curing Reaction of a Diglycidyl Ether of Bisphenol with a Methanol Etherified Amino Resin

2011 ◽  
Vol 380 ◽  
pp. 60-63 ◽  
Author(s):  
Yong Lv ◽  
Zhu Long ◽  
Shi Yong Luo ◽  
Lei Dai

Subscript text Subscript textEpoxy resins have been widely used for inner coating in food can and other chemical products storage containers. Differential scanning calorimetry (DSC) was used at different heating rates to study the cure kinetics of the diglycidyl ether of bisphenol A (DGEBA) with a methanol etherified amino resin (MEAR). The apparent activation energy derived from Kissinger and Ozawa methods is 35.67KJ/mol and 40.27kJ/mol, respectively. The reaction order evaluated by Crane equation is 0. 95 and the frequency factor is 1.12×104s-1. Reaction mechanism was monitored by FTIR spectra of the reaction mixtures before and after curing. The curing reaction below 200°C is between alkoxylmethyl (>NCH2OCH3) and epoxide group, not between alkoxylmethyl and hydroxyls.

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Ali Kuliaei ◽  
Iraj Amiri Amraei ◽  
Seyed Rasoul Mousavi

Abstract The purpose behind this research was to determine the optimum formulation and investigate the cure kinetics of a diglycidyl ether of bisphenol-A (DGEBA)-based epoxy resin cured by dicyandiamide and diuron for use in prepregs. First, all formulations were examined by the tensile test, and then, the specimens with higher mechanical properties were further investigated by viscometry and tack tests. The cure kinetics of the best formulation (based on tack test) in nonisothermal mode was investigated using differential scanning calorimetry at different heating rates. Kissinger and Ozawa method was used for determining the kinetic parameters of the curing process. The activation energy obtained by this method was 71.43 kJ/mol. The heating rate had no significant effect on the reaction order and the total reaction order was approximately constant ( m + n ≅ 2.1 $m+n\cong 2.1$ ). By comparing the experimental data and the theoretical data obtained by Kissinger and Ozawa method, a good agreement was seen between them. By increasing the degree of conversion, the viscosity decreased; as the degree of conversion increased, so did the slope of viscosity. The results of the tack test also indicated that the highest tack could be obtained with 25% progress of curing.


2010 ◽  
Vol 123-125 ◽  
pp. 667-670 ◽  
Author(s):  
Jae Young Lee ◽  
Bum Choul Choi ◽  
Hong Ki Lee

Polymer nanocomposite was synthesized through the intercalation and exfoliation of organoclay in an epoxy matrix. The epoxy matrix was composed of diglycidyl ether of bisphenol A (DGEBA, epoxy base resin), 4,4'-methylene dianiline (MDA, curing agent) and malononitrile (MN, chain extender) and organoclay was prepared by treating the montmorillonite with octadecyltrimethylammonium bromide (ODTMA). The intercalation of the organoclay was estimated by wide angle X-ray diffraction (WAXD) and transmission electron microscope (TEM) analyses. In order to measure the cure rate of DGEBA/MDA (30 phr)/MN (5 phr)/Organoclay (5 phr), differential scanning calorimetry (DSC) analysis were performed at the heating rates of 5, 10, 15 and 20 oC/min, and the data was interpreted by Kissinger equation. Thermal degradation kinetics of the epoxy nanocomposite was also studied by thermogravimetric analysis (TGA). The epoxy sample was decomposed in the TGA furnace at the heating rates of 5, 10, 15 and 20 oC/min with nitrogen atmosphere of 50 ml/min. The TGA data was introduced to the Ozawa equation and the degradation activation energy was calculated according to the degradation ratio. The activation energy for cure kinetics was 43.3 kJ/mol and that for thermal degradation was 171.5 kJ/mol.


2021 ◽  
pp. 002199832110015
Author(s):  
Alexander Vedernikov ◽  
Yaroslav Nasonov ◽  
Roman Korotkov ◽  
Sergey Gusev ◽  
Iskander Akhatov ◽  
...  

Pultrusion is a highly efficient composite manufacturing process. To accurately describe pultrusion, an appropriate model of resin cure kinetics is required. In this study, we investigated cure kinetics modeling of a vinyl ester pultrusion resin (Atlac 430) in the presence of aluminum hydroxide (Al(OH)3) and zinc stearate (Zn(C18H35O2)2) as processing additives. Herein, four different resin compositions were studied: neat resin composition, composition with Al(OH)3, composition comprising Zn(C18H35O2)2, and composition containing both Al(OH)3 and Zn(C18H35O2)2. To analyze each composition, we performed differential scanning calorimetry at the heating rates of 5, 7.5, and 10 K/min. To characterize the cure kinetics of Atlac 430, 16 kinetic models were tested, and their performances were compared. The model based on the [Formula: see text]th-order autocatalytic reaction demonstrated the best results, with a 4.5% mean squared error (MSE) between the experimental and predicted data. This study proposes a method to reduce the MSE resulting from the simultaneous melting of Zn(C18H35O2)2. We were able to reduce the MSE by approximately 34%. Numerical simulations conducted at different temperatures and pulling speeds demonstrated a significant influence of resin composition on the pultrusion of a flat laminate profile. Simulation results obtained for the 600 mm long die block at different die temperatures (115, 120, 125, and 130 °C) showed that for a resin with a final degree of cure exceeding 95% at the die exit, the maximum difference between the predicted values of pulling speed for a specified set of compositions may exceed 1.7 times.


2020 ◽  
Vol 4 (3) ◽  
pp. 111
Author(s):  
Zohre Karami ◽  
Seyed Mohammad Reza Paran ◽  
Poornima Vijayan P. ◽  
Mohammad Reza Ganjali ◽  
Maryam Jouyandeh ◽  
...  

Layered double hydroxide (LDH) minerals are promising candidates for developing polymer nanocomposites and the exchange of intercalating anions and metal ions in the LDH structure considerably affects their ultimate properties. Despite the fact that the synthesis of various kinds of LDHs has been the subject of numerous studies, the cure kinetics of LDH-based thermoset polymer composites has rarely been investigated. Herein, binary and ternary structures, including [Mg0.75 Al0.25 (OH)2]0.25+ [(CO32−)0.25/2∙m H2O]0.25−, [Mg0.75 Al0.25 (OH)2]0.25+ [(NO3−)0.25∙m H2O]0.25− and [Mg0.64 Zn0.11 Al0.25 (OH)2]0.25+ [(CO32−)0.25/2∙m H2O]0.25−, have been incorporated into epoxy to study the cure kinetics of the resulting nanocomposites by differential scanning calorimetry (DSC). Both integral and differential isoconversional methods serve to study the non-isothermal curing reactions of epoxy nanocomposites. The effects of carbonate and nitrate ions as intercalating agents on the cure kinetics are also discussed. The activation energy of cure (Eα) was calculated based on the Friedman and Kissinger–Akahira–Sunose (KAS) methods for epoxy/LDH nanocomposites. The order of autocatalytic reaction (m) for the epoxy/Mg-Al-NO3 (0.30 and 0.254 calculated by the Friedman and KAS methods, respectively) was smaller than that of the neat epoxy, which suggested a shift of the curing mechanism from an autocatalytic to noncatalytic reaction. Moreover, a higher frequency factor for the aforementioned nanocomposite suggests that the incorporation of Mg-Al-NO3 in the epoxy composite improved the curability of the epoxy. The results elucidate that the intercalating anions and the metal constituent of LDH significantly govern the cure kinetics of epoxy by the participation of nitrate anions in the epoxide ring-opening reaction.


2020 ◽  
Vol 2020 ◽  
pp. 1-10 ◽  
Author(s):  
Haleh Nowruzi Varzeghani ◽  
Iraj Amiri Amraei ◽  
Seyed Rasoul Mousavi

This study investigated the effect of polyethylene glycol (PEG) and nanosilica (NS) on the physical-mechanical properties and cure kinetics of diglycidyl ether of bisphenol-A-based epoxy (DGEBA-based EP) resin. For this purpose, tensile and viscometry tests, dynamic mechanical thermal analysis (DMTA), and differential scanning calorimetry (DSC) were carried out under dynamic conditions. The results showed that adding NS and PEG enhances the maximum cure temperature as well as the heat of cure reaction (ΔH) in EP-NS, while it decreases in EP-PEG and EP-PEG-NS. The cure kinetic parameters of EP-PEG-NS were calculated by Kissinger, Ozawa, and KSA methods and compared with each other. The Ea calculated from the Kissinger method (96.82 kJ/mol) was found to be lower than that of the Ozawa method (98.69 kJ/mol). Also, according to the KAS method, the apparent Ea was approximately constant within the 10-90% conversion range. Tensile strength and modulus increased by adding NS, while tensile strength diminished slightly by adding PEG to EP-NS. The glass transition temperature (Tg) was calculated using DMTA which was increased and decreased by the addition of NS and PEG, respectively. The results of the viscometry test showed that the viscosity increased with the presence of both PEG and NS and it prevented the deposition of solid particles.


2012 ◽  
Vol 463-464 ◽  
pp. 181-184
Author(s):  
Ya Juan Xu ◽  
Qin Cun Cao ◽  
Xi Gao Jian

A series of blends have been prepared by adding a novel thermoplastic poly (phthalazinone ether sulfone ketone) (PPESK) in varying proportions to diglycidyl ether of bisphenol A epoxy resin (DGEBA) cured with p-diaminodiphenylsulfone. The kinetics of curing reaction and glass transition temperature (Tg) of PPESK/DGEBA blends were performed using differential scanning calorimetry (DSC) technique. It is proved that the addition of PPESK accelerated curing reaction and resulted in great enhancement of thermal properties of the blends. There was moderate increase in the fracture toughness as estimated by the critical stress intensity factor (KIc). Compared to that of unmodified epoxy, the maximum toughness of the modified blends had increased 32% by addition of 15 phr PPESK. Fracture mechanisms such as crack deflection and branches, ductile microcracks, ductile tearing of the thermoplastic of the matrix were responsible for the increase in the fracture toughness of the blends


2011 ◽  
Vol 236-238 ◽  
pp. 2058-2062
Author(s):  
Hong Jun Zhou ◽  
Guo Qiang Yin ◽  
Miao Hong Zhuang ◽  
Jian Fang Ge ◽  
Xuan Lin

The cure kinetics of epoxy/epoxy-grafted nano-aluminum oxide using 4, 4'-diaminodiphenylsulphone (DDS) as the curing agent was studied by nonisothermal differential scanning calorimetry (DSC) at different heating rates. The activation energy (Ea) was determined by Flynn-Wall-Ozawa method, and kinetic model was predicted by Málek method. TheEa values of epoxy/nano-aluminum oxide/DDS systems are generally higher than those of epoxy /DDS. These imply that the addition of nano-aluminum oxide would inhibit the chain mobility of the epoxy resins. Furthermore, autocatalytic model was found to be appropriate to describe the kinetics of above mentioned reactions. The predicted curves fit well with the experimentally obtained curves.


2010 ◽  
Vol 123-125 ◽  
pp. 955-958
Author(s):  
De Wen Zhou ◽  
Li Yan Liang ◽  
Man Geng Lu

A series of dimeric liquid crystalline (LC) epoxy monomers containing azo groups with different length of central spacers were synthesized. The mesogenic behavior of these monomers was characterized by differential scanning calorimetry(DSC), polarized optical microscopy (POM) and wide-angle X-Ray diffraction(WAXS). Like other dimeric LC epoxy monomers, the melting points, clear points and mesophase of these compounds were influenced by the carbon numbers of the central spacers. Cure kinetics of these monomers with anhydride was studied by non-isothermal DSC at different heating rates. With the increasing of conversion, the values of activation energy show a tendency to decrease. The formation and development of LC phase during curing were also studied by POM. Finally LC thermosets with nematic phase were obtained.


2012 ◽  
Vol 706-709 ◽  
pp. 1311-1317 ◽  
Author(s):  
S.A. Hasheminezhad ◽  
M. Haddad-Sabzevar ◽  
S. Sahebian

Non-isothermal crystallization kinetics of Co67Fe4Cr7Si8B14amorphous ribbons was studied by differential scanning calorimetry (DSC) technique under 10, 20, 30, 40 and 80 °Cmin-1heating rates. It is found that Co67Fe4Cr7Si8B14amorphous alloy exhibits two-stage crystallization on heating. The two crystallization peaks shift to higher temperatures with increasing heating rate. The apparent activation energies (EC) for the first stage of crystallization were determined as 443.44 and 434.47 kJmol-1by using the Kissinger and Ozawa equations, respectively. Frequency factor (A) estimated to be 1.084×1026s-1using Kissinger equation. Kinetics parameters such as Crystallization exponent (n) and dimensionality of growth (Ndim) were determined using JMA (Johnson-Mehl-Avrami) method. Details of the nucleation and growth behaviours during the non-isothermal crystallization were studied in terms of local activation energy EC(x) by the OFW (Ozawa, Flynn and Wall) method. Also the activation energy for nucleation (En) and growth (Eg) separately estimated.


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