Kinetic analysis of the curing of branched phthalonitrile resin based on dynamic differential scanning calorimetry

Zu, Yuan Gang; Zong, Lishuai; Wang, Jinyan; Jian, Xigao

doi:10.1016/j.polymertesting.2021.107062

Cited by 17 publications

(13 citation statements)

References 45 publications

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“…This phenomenon may be related to the generally accepted knowledge that for thermosetting resin, the curing reaction will approach diffusion control during post-curing stage, leading to un-crosslinking components such as linear polymers, branched polymers. 61–63 Thus, the storage modulus gradually approached the minimums at temperatures lower than the maximum post-curing temperatures. In other words, the T g was lower than the maximum post-curing temperature.…”

Section: Resultsmentioning

confidence: 99%

Synthesis of oligomeric phthalonitrile resins containing imide units and study of the methylene-cyano thermal synergistic polymerization effect

Xie

et al. 2022

High Performance Polymers

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The meta- and para-catenated methylene-containing phthalonitrile oligomers were prepared from the reaction of an excess amount of 4,4′-(4,4′-isopropylidenediphenoxy) bis-(phthalic anhydride) (BPADA) with 4,4′-Methylenedianiline (MDA) in a N, N-dimethylformamide/ toluene solvent mixture, followed by end-capping agent with 4-nitrophthalonitrile or 4-phenoxyaniline in a two-step, one-pot reaction. Differential scanning calorimetry (DSC) showed that both PN oligomers exhibited low softening points. The self-catalyzed curing reactivity of the PN oligomers was confirmed by the isothermal rheological measurements. Fourier transform infrared spectroscopy (FTIR) and ultraviolet and visible spectrophotometry (UV–Vis) data of the pre-curing resins were employed to investigate the chemical structure of the pre-cured resins, suggesting that oligomers generated crosslinking sites, including triazine, isoindoline, and phthalocyanine. The results further confirmed the self-catalyzed curing reactivity of the oligomers. Thermal properties were investigated by dynamic mechanical analysis (DMA) and thermal gravimetric analysis (TGA), demonstrating good thermal properties of the cured resins. The glass transition temperatures (Tgs) of PIPN-1-325, PIPN-1-350, PIPN-1-375 were in the range of 285–345°C, the 5% weight loss temperature (T5%) was observed at 482°C. The PIPN-2-325, PIPN-2-350, PIPN-2-375 showed Tgs ranging from 293 to 370°C, and T5% of the resins were in the range of 481–501°C. Then the isothermal rheological results of model compound and PN oligomers implied that the curing process of PN oligomers was closely related to the methylene-cyano radical thermal synergistic polymerization (TSP) effect proposed in our previous research, and then a revised curing mechanism (radical TSP mechanism) was proposed.

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Section: Resultsmentioning

confidence: 99%

Synthesis of oligomeric phthalonitrile resins containing imide units and study of the methylene-cyano thermal synergistic polymerization effect

Xie

et al. 2022

High Performance Polymers

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“…Among phenomenological models, the n ‐order reaction model is the simplest to interpret the curing behavior, which is used extensively as well as the autocatalytic model. Málek and least squares regression (LSR) methods can be used in the autocatalytic reaction model 3,13–20 . There exist Kamal and Kamal–Chern models in which nonlinear regression or data fitting methods are used to calculate the kinetic parameters 2,16,21 .…”

Section: Introductionmentioning

confidence: 99%

“…M alek and least squares regression (LSR) methods can be used in the autocatalytic reaction model. 3,[13][14][15][16][17][18][19][20] There exist Kamal and Kamal-Chern models in which nonlinear regression or data fitting methods are used to calculate the kinetic parameters. 2,16,21 Additionally, the Coats-Redfern method combined with different kinetic models from four major solid-state reaction mechanisms is a kind of way to characterize the kinetic behavior as well.…”

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confidence: 99%

“…[27][28][29] There are indeed quite a few works related to the simulation of curing kinetics including calculations of kinetic parameters and establishments of fitting models. It is well known that the evaluation of cuing kinetic parameters depends on the curing degree, the initial value of which is generally 0.1 3,[13][14][15]18,19,[29][30][31][32] or 0.2 33,34 or minimum value increment. 12,16 Due to the incapacity of Kamal-Sourour kinetic model for predicting cure behavior at the beginning stages of reaction, although the influence of different initial curing degrees on the accuracy of predicted values of the curing degree and time has been discussed, the initial curing degree is assumed as a very small nonzero initial value to be considered as the curing degree at the end of induction time, the maximum of which is 0.01.…”

mentioning

confidence: 99%

“…To investigate the curing kinetics of resin, several experimental techniques have been used such as thermogravimetry analysis (TGA), [22][23][24]32,34 rheology, 2,19,29,35 differential scanning calorimetry (DSC). 3,[11][12][13][14][15][16][17][18][19][20][21]24,25,30,31 Among the techniques for determining the degree of conversion, TGA is performed by analyzing biomass decomposition. The data obtained from registering weight loss can be used to estimate the degree of conversion of biomass from solid to volatile state.…”

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confidence: 99%

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Reliability evaluation of a new method developed for DSC curing kinetic model of epoxy resin

Jia

Zhu

Yan

et al. 2023

J of Applied Polymer Sci

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The curing kinetic model of epoxy resin is crucial for understanding reaction mechanism and accurately describing curing behavior of fiber reinforced polymer composites. In the investigations related to kinetic models of epoxy, much attention is payed to the curing characterizations of modified or mixed materials for the desired field of application in the case that the initial curing degree for calculating kinetic parameters is generally constant. In this paper, a new method by specifying the initial curing degree for kinetic parameters is developed to improve the accuracy of fitting models based on the resin systems and methods for activation energy. The curing kinetics of resin systems including Epoxy 4330, Epoxy 5212, and diglycidyl ether pentaerythritol vanillin diacetalbisphenol-A epoxy resin-4,4 0 -diaminodiphenyl sulfone (DEPVD-E51-DDS) are examined utilizing differential scanning calorimetric technique at five different heating rates. Additionally, Kissinger, Starink, and Friedman methods, and piecewise models are adopted to fit the experimental data. The predictions from fitting models using different initial curing degrees are subsequently compared with experimental data. It is concluded that the utilization of initial curing degree promotes the accuracy of fitting models.activation energy, curing kinetics, epoxy resin, fitting model | INTRODUCTIONEpoxy resin can be applied separately and also be taken as the matrix of fiber reinforced polymer (FRP) composites or particles reinforced epoxy hybrid composites 1 due to the superior properties such as easy processing, high chemical, and good adhesive properties, 2,3 which can be fabricated by various composite manufacturing

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Synthesis, Curing Kinetics, and Properties of a Novel Phthalazine‐Based Phthalonitrile Resin

Jia,

Rong,

et al. 2023

ChemistrySelect

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A novel phthalazine‐based phthalonitrile resin was prepared by two different curing procedures. The phthalonitrile monomer, namely, 4,4′‐(((phthalazine‐1,4‐diylbis(oxy))bis(3,1‐phenylene))bis(oxy))diphthalonitrile (PDOP), was synthesized from the reaction of 1, 4‐dichloropthalazine, resorcinol, and 4‐nitrophthalonitrile. Its curing behavior and curing kinetics with 4‐(4‐aminophenoxy)phthalonitrile (APPH) were investigated by Differential Scanning Calorimetric (DSC). Isoconversional method based on Starink was applied to analyze the curing process of PDOP/APPH. The PDOP monomer exhibits a low melting point (89 °C) and a wide processing window (146 °C). The PDOP polymer mainly forms triazine, isoindoline, and phthalocyanine structure, as revealed by Fourier Transform Infrared (FTIR) spectroscopy, and its properties improved with the increase of post‐curing temperature and curing time. After post‐curing at 350 °C, the polymer has high storage modulus (3313 MPa), high glass‐transition temperature (380 °C), and outstanding thermal stability and thermal oxidation stability.

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Kinetic analysis of the curing of branched phthalonitrile resin based on dynamic differential scanning calorimetry

Cited by 17 publications

References 45 publications

Synthesis of oligomeric phthalonitrile resins containing imide units and study of the methylene-cyano thermal synergistic polymerization effect

Synthesis of oligomeric phthalonitrile resins containing imide units and study of the methylene-cyano thermal synergistic polymerization effect

Reliability evaluation of a new method developed for DSC curing kinetic model of epoxy resin

Synthesis, Curing Kinetics, and Properties of a Novel Phthalazine‐Based Phthalonitrile Resin

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