scholarly journals Kinetics of Cross-Linking Reaction of Epoxy Resin with Hydroxyapatite-Functionalized Layered Double Hydroxides

Polymers ◽  
2020 ◽  
Vol 12 (5) ◽  
pp. 1157 ◽  
Author(s):  
Zohre Karami ◽  
Mohammad Reza Ganjali ◽  
Maryam Zarghami Dehaghani ◽  
Mustafa Aghazadeh ◽  
Maryam Jouyandeh ◽  
...  
Keyword(s):  
Epoxy Resin ◽  
Curing Kinetics ◽  
Frequency Factor ◽  
Isoconversional Methods ◽  
Divalent Metal Ions ◽  
Interlayer Water ◽  
Scanning Calorimetry ◽  
Kinetics Parameters ◽  
Bending Vibration ◽  
Weak Band

The cure kinetics analysis of thermoset polymer composites gives useful information about their properties. In this work, two types of layered double hydroxide (LDH) consisting of Mg2+ and Zn2+ as divalent metal ions and CO32− as an anion intercalating agent were synthesized and functionalized with hydroxyapatite (HA) to make a potential thermal resistant nanocomposite. The curing potential of the synthesized nanoplatelets in the epoxy resin was then studied, both qualitatively and quantitatively, in terms of the Cure Index as well as using isoconversional methods, working on the basis of nonisothermal differential scanning calorimetry (DSC) data. Fourier transform infrared spectroscopy (FTIR) was used along with X-ray diffraction (XRD) and thermogravimetric analysis (TGA) to characterize the obtained LDH structures. The FTIR band at 3542 cm−1 corresponded to the O–H stretching vibration of the interlayer water molecules, while the weak band observed at 1640 cm−1 was attributed to the bending vibration of the H–O of the interlayer water. The characteristic band of carbonated hydroxyapatite was observed at 1456 cm−1. In the XRD patterns, the well-defined (00l) reflections, i.e., (003), (006), and (110), supported LDH basal reflections. Nanocomposites prepared at 0.1 wt % were examined for curing potential by the Cure Index as a qualitative criterion that elucidated a Poor cure state for epoxy/LDH nanocomposites. Moreover, the curing kinetics parameters including the activation energy (Eα), reaction order, and the frequency factor were computed using the Friedman and Kissinger–Akahira–Sunose (KAS) isoconversional methods. The evolution of Eα confirmed the inhibitory role of the LDH in the crosslinking reactions. The average value of Eα for the neat epoxy was 54.37 kJ/mol based on the KAS method, whereas the average values were 59.94 and 59.05 kJ/mol for the epoxy containing Zn-Al-CO3-HA and Mg Zn-Al-CO3-HA, respectively. Overall, it was concluded that the developed LDH structures hindered the epoxy curing reactions.

scholarly journals A Comparative Study on Cure Kinetics of Layered Double Hydroxide (LDH)/Epoxy Nanocomposites

2020 ◽  
Vol 4 (3) ◽  
pp. 111
Author(s):  
Zohre Karami ◽  
Seyed Mohammad Reza Paran ◽  
Poornima Vijayan P. ◽  
Mohammad Reza Ganjali ◽  
Maryam Jouyandeh ◽  
...  
Keyword(s):  
Layered Double Hydroxide ◽  
Cure Kinetics ◽  
Frequency Factor ◽  
Isoconversional Methods ◽  
Epoxide Ring ◽  
Epoxy Nanocomposites ◽  
Scanning Calorimetry ◽  
Noncatalytic Reaction ◽  
Double Hydroxide ◽  
Kinetics Of

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.

Curing Kinetics and Rheology of Diglycidyiether of Bisphenol-A Modified by Poly(ethylene glycol) Flexible Chains

2010 ◽  
Vol 123-125 ◽  
pp. 411-414 ◽  
Author(s):  
Da Hu Yao ◽  
Kyung Bok Sun ◽  
Peng Li ◽  
Joong Hee Lee
Keyword(s):  
Ethylene Glycol ◽  
Bisphenol A ◽  
Epoxy Resin ◽  
Kinetic Parameters ◽  
Curing Kinetics ◽  
Poly Ethylene Glycol ◽  
Scanning Calorimetry ◽  
Exponential Factor ◽  
Curing Reaction ◽  
Poly Ethylene

The curing reaction of the system bisphenol-A glycidol ether epoxy resin modified by poly (ethylene glycol) (PEO) and flexible amine (D-230) as curing agent has been studied by means of differential scanning calorimetry (DSC) and thermal scanning rheometry. The curing kinetic parameters have been calculated from the non-thermal DSC curve. The kinetic analysis suggests that the two-parameter autocatalytic model is more appropriate to describe the kinetics of the curing reaction of the system. Increasing the PU content leads to an increase in the heat of curing and has a little effect on the kinetic parameters apparent activation energy (Ea), pre-exponential factor (A), and order of the reaction (m and n). The rheological properties were measured by isothermal curing evolution. Introduction of PEO flexible chains delayed the polymerization. It has been confirmed that the introduction of PEO chains in the structure of the epoxy resin increases the mobility of the molecular segment of the epoxy networks and results in the decrease in glass transition temperature.

An improved simplified approach for curing kinetics of epoxy resins by nonisothermal differential scanning calorimetry

2017 ◽  
Vol 30 (3) ◽  
pp. 303-311 ◽  
Author(s):  
Chao Chen ◽  
Yanxia Li ◽  
Yizhuo Gu ◽  
Min Li ◽  
Zuoguang Zhang
Keyword(s):  
Differential Scanning Calorimetry ◽  
Epoxy Resin ◽  
Kinetic Parameters ◽  
Epoxy Resins ◽  
Curing Kinetics ◽  
Scanning Calorimetry ◽  
Simplified Approach ◽  
Curing Kinetic ◽  
Autocatalytic Curing ◽  
Kinetics Of

The curing kinetics of two different types of commercial epoxy resins were investigated by means of nonisothermal differential scanning calorimetry (DSC) in this work. The complex curve of measured heat flow of CYCOM 970 epoxy resin was simplified with the method of resolution of peak. Two typical autocatalytic curing reaction curves were gained and the kinetic parameters of the curing process were demonstrated by combination of those two reactions. The Kissinger method was adopted to obtain the values of the activation energy. The parameters of curing kinetic model were acquired according to the fitting of Kamal model. Isothermal DSC curve of CYCOM 970 epoxy resin obtained using the experimental data shows a good agreement with that theoretically calculated. Then, 603 epoxy resin was investigated by the simplified method and the kinetic parameters were received through the same procedure. The nonisothermal DSC curve tested according to the recommended cure cycle of 603 epoxy resin is also consistent with the calculated results. This improved simplified approach provides an effective method to analyze the curing kinetics of the epoxy resins with complex DSC curves as similar to this study.

scholarly journals The Curing Kinetics of E-Glass Fiber/Epoxy Resin Prepreg and the Bending Properties of Its Products

Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4673
Author(s):  
Lvtao Zhu ◽  
Zhenxing Wang ◽  
Mahfuz Bin Rahman ◽  
Wei Shen ◽  
Chengyan Zhu
Keyword(s):  
Glass Fiber ◽  
Epoxy Resin ◽  
Composite Laminates ◽  
Curing Kinetics ◽  
Curing Temperature ◽  
Scanning Calorimetry ◽  
Three Point Bending ◽  
Reinforced Composite ◽  
Curing Kinetic ◽  
Kinetics Of

The curing kinetics can influence the final macroscopic properties, particularly the three-point bending of the fiber-reinforced composite materials. In this research, the curing kinetics of commercially available glass fiber/epoxy resin prepregs were studied by non-isothermal differential scanning calorimetry (DSC). The curing kinetic parameters were obtained by fitting and the apparent activation energy Ea of the prepreg, the pre-exponent factor, and the reaction order value obtained. A phenomenological nth-order curing reaction kinetic model was established according to Kissinger equation and Crane equation. Furthermore, the optimal curing temperature of the prepregs was obtained by the T-β extrapolation method. A vacuum hot pressing technique was applied to prepare composite laminates. The pre-curing, curing, and post-curing temperatures were 116, 130, and 153 °C respectively. In addition, three-point bending was used to test the specimens’ fracture behavior, and the surface morphology was analyzed. The results show that the differences in the mechanical properties of the samples are relatively small, indicating that the process settings are reasonable.

scholarly journals Curing Kinetics and Mechanism Research of E44/T31 Insulation Paint

2019 ◽  
Vol 25 (4) ◽  
pp. 478-484
Author(s):  
Haoqing XU ◽  
Yuan FANG ◽  
Aizhao ZHOU ◽  
Pengming JIANG ◽  
Shi SHU ◽  
...  
Keyword(s):  
Epoxy Resin ◽  
Epoxy Group ◽  
Curing Kinetics ◽  
Curing Temperature ◽  
Scanning Calorimetry ◽  
Curing Reaction ◽  
Rate Versus ◽  
Reaction Orders ◽  
Dsc Method ◽  
Kinetics Of

Epoxy resin insulation paint was prepared with epoxy resin (E44) as binder and with proper inorganic fillers and curing agent (T31) as additives. The isothermal curing reaction process of paint was studied by the differential scanning calorimetry method (DSC), and the curves of curing reaction rate versus time of paint were obtained. The curing reaction kinetics was investigated by using the phenomenological method, and the corresponding parameters of the n-order model, autocatalytic model and Kamal model were determined by fitting the experimental data, respectively. According to the values of R2 and the sum of square due to error (SSE), a suitable curing reaction kinetic model was determined. The curing reaction mechanism of paint was ascertained by the dynamic temperature DSC method and IR spectroscopy (FTIR) method. The results show that the Kamal model can be used to describe the curing kinetics of epoxy resin paint, and the total reaction orders increase from 1.30 to 2.14. The two rate constants increase with the increase of the curing temperature. The activation energy is 90.5832 kJ/mol and 68.3733 kJ/mol respectively, and the pre-exponential factors are 6.521 × 1015 s-1 and 6.3807 × 109 s-1. The curing reaction of paint consists of two steps: the first step is the addition reaction of epoxy group and primary amine or secondary amine; the second step is the etherification reaction of epoxy group and phenolic hydroxyl or alcoholic hydroxyl. Epoxy resin insulation paint was prepared with epoxy resin (E44) as binders and with proper inorganic fillers and curing agent (T31) as additives. The isothermal curing reaction process of paint was studied by differential scanning calorimetry method (DSC), and the curves of curing reaction rate versus time of paint were obtained. The curing reaction kinetics was studied by using the phenomenological method, the corresponding parameters of the n-order model, autocatalytic model and Kamal model were determined by fitting the experimental data, respectively. According to the values of R2 and the sum of square due to error (SSE), a suitable curing reaction kinetic model was determind. The curing reaction mechanism of paint was ascertained by dynamic temperature DSC method and IR spectrogram (FTIR) method. The results show that the kamal model can be used to describe the curing kinetics of epoxy resin paint, the total reaction orders increase from 1.30 to 2.14. The results also show that the two rate constants increase with increasing curing temperature, The activation energies are 90.5832 kJ/mol and 68.3733 kJ/mol, and the pre-exponential factor are 6.521×1015 s-1 and 6.3807×109 s-1. The curing reaction of paint in two steps, the first step is the addition reaction of epoxy group and primary amine or secondary amine. The second step is the etherification reaction of epoxy group and phenolic hydroxyl or alcoholic hydroxyl.

scholarly journals Thermo-kinetics of Forest Waste Using Model-Free Methods

2019 ◽  
Vol 24 (1) ◽  
pp. 1-31 ◽  
Author(s):  
Alok Dhaundiyal ◽  
Abdulrahman Th Mohammad ◽  
Toth Laszlo
Keyword(s):  
Thermal Decomposition ◽  
Kinetic Parameters ◽  
Frequency Factor ◽  
Isoconversional Methods ◽  
Pine Needles ◽  
Kissinger Method ◽  
Heating Rates ◽  
Pinus Roxburghii ◽  
Kinetics Parameters ◽  
Model Free

Thermal behaviour of pine needles (Pinus Roxburghii) is examined through a thermogravimetry technique. The dried samples of pine needles undergo the non isothermal decomposition at temperature range of 308 - 1173 K. The heating rates used for experimental purposes are: 5 °C min-1, 10 °C min-1 and 15 °C min-1. Kinetic parameters of thermal decomposition reactions of pine needles are obtained through the model-free schemes. The estimated values of activation energy and frequency factor derived from Kissinger method are 132.77 kJ mol-1 and 13.15 x107 min-1, respectively. Furthermore, the averaged values of the same kinetics parameters retrieved from the isoconversional methods are 82.38 kJ mol-1 and 74.833 kJ mol-1, 25.42 x1013 min-1 and 13.449 x1010 min-1, respectively. Instead of the Flynn-Wall-Ozawa (FWO) and Kissinger-Akahira Sunrose (KAS) schemes, the kinetic parameters derived from the Kissinger method are relatively promising for the thermal decomposition process, since the kinetic parameters are highly affected by intermediate stages and overlapping of the concurrent reaction occurred during pyrolysis.

scholarly journals Studies on Curing Kinetics and Tensile Properties of Silica-Filled Phenolic Amine/Epoxy Resin Nanocomposite

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 680 ◽  
Author(s):  
Ting Zheng ◽  
Xiaodong Wang ◽  
Chunrui Lu ◽  
Xiaohong Zhang ◽  
Yi Ji ◽  
...  
Keyword(s):  
Epoxy Resin ◽  
Tensile Properties ◽  
Curing Kinetics ◽  
Tensile Fracture ◽  
Resin System ◽  
Scanning Calorimetry ◽  
Nano Sio2 ◽  
Model Free ◽  
Uniform Dispersion ◽  
Epoxy Resin System

In this study, the curing kinetics of the phenolic amine/epoxy resin system were investigated by nonisothermal differential scanning calorimetry (DSC). The model-free isoconversional method of Ozawa–Flynn–Wall reveals a dependence of Eα (activation energy) on conversion (α), which interprets the autocatalytic curing reaction mechanism of the phenolic amine/epoxy resin system. Studies on the effects of nano-SiO2 particles on the tensile properties and tensile fracture face morphology of nanocomposites show that the uniform dispersion of SiO2 nanoparticles plays an important role in promoting the tensile performance of nanocomposites. Additionally, increases of 184.1% and 217.2% were achieved by adding 1.5% weight parts of nano-SiO2 in composites for the tensile strength and tensile modulus, respectively.

Curing kinetics study of epoxy resin/hyperbranched poly(amideamine)s system by non-isothermal and isothermal DSC

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Li Zhang ◽  
Hui Kang Yang ◽  
Guang Shi
Keyword(s):  
Kinetic Model ◽  
Epoxy Resin ◽  
Kinetic Parameters ◽  
Curing Kinetics ◽  
Scanning Calorimetry ◽  
Fitting Procedure ◽  
Hyperbranched Poly ◽  
Numerical Process ◽  
Isothermal Kinetic ◽  
Dsc Method

AbstractCuring kinetics of epoxy resin/hyperbranched poly(amide amine)s (HPAMAM) system was studied by non-isothermal and isothermal differential scanning calorimetry (DSC). Non-isothermal DSC scans indicated that H-PAMAM was an effective curing agent of epoxy resin. The apparent activation energy (E) was 54.3 kJ/mol calculated through Kissinger method, and the kinetic parameters were determined by Málek method for the kinetic analysis of the thermal treatment obtained by DSC measurement. A two-parameter (m, n) autocatalytic model (Sěsták-Berggren equation) was found to be the most adequate selected kinetic model. In addition, the predicted curves from the kinetic model fit well with the nonisothermal DSC thermogram. The isothermal DSC method was used to investigate the curing process for resin at 60, 65, 70, 75 and 80 °С, respectively. Isothermal kinetic parameters, including k1, k2, m and n, were determined based on an autocatalytic mechanism proposed by Kamal. Both models were validated for a fitting to the experimental data by the Levenberg-Marquardt method. A process to determine the initial values for the fitting procedure was also proposed. The predictions of the validated models were in good agreement with the measured data, and were therefore applicable for numerical process optimization

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