Kinetics and curing mechanism of epoxy and boron trifluoride monoethyl amine complex system

Li, Ye‐Shiu; Li, Ming-Shiu; Chang, Feng‐Chih

doi:10.1002/(sici)1099-0518(19990915)37:18<3614::aid-pola9>3.3.co;2-q

Cited by 11 publications

(13 citation statements)

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“…The kinetics of epoxy–amine reactions has been well established in the literature 17–21. In the DSC curve of dynamic curing for the DGEBA/MP system, at a heating rate of 10°C/min as shown in Figure 2, T i (199.2°C) is the initial temperature of the curing reaction, T p (244.8°C) is the peak maximum temperature, and T f (276.4°C) is the final temperature, respectively.…”

Section: Resultsmentioning

confidence: 91%

Study on curing kinetics and curing mechanism of epoxy resin based on diglycidyl ether of bisphenol a and melamine phosphate

Chen

Wang

Chang

2004

J of Applied Polymer Sci

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ABSTRACT:The curing kinetics of the diglycidyl ether of bisphenol A/melamine phosphate (DGEBA/MP) was analyzed by the DSC technique. The Kissinger and Flynn-WallOzawa methods were applied to determine the dynamic kinetics of the DGEBA/MP system. The activation energies obtained by these two methods were 83.9 and 85.6 kJ/mol, respectively. An autocatalytic equation was applied to determine the isothermal curing kinetics of the DGEBA/MP system. The DGEBA/MP system exhibits autocatalytic behavior in the isothermal curing procedure, whose kinetics fits well with the autocatalytic mechanism. The obtained isothermal curing activation energy of the DGEBA/MP system was 110.0 kJ/mol. The curing mechanism of DGEBA with melamine phosphate was investigated using FTIR, 13 C solid-state NMR, and 31 P solid-state NMR. It involved an epoxide-amine reaction, etherification of phosphoric acid and epoxy, dehydration, and thermal oxidation of the hydroxyl group of the DGEBA/MP system. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: [892][893][894][895][896][897][898][899][900] 2004

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Section: Resultsmentioning

confidence: 91%

Study on curing kinetics and curing mechanism of epoxy resin based on diglycidyl ether of bisphenol a and melamine phosphate

Chen

Wang

Chang

2004

J of Applied Polymer Sci

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“…DCPD are 11,000-14,000 cP and 1 cP, respectively, at room temperature. (63)(64) Even at low DCPD conversions, the system may be diffusion-limited at high concentrations of the epoxy resin components.…”

Section: Effect Of Dilution On the Dcpd Curing Kineticsmentioning

confidence: 99%

Concurrent curing kinetics of an anhydride-cured epoxy resin and polydicyclopentadiene

Rohde

Robertson

Krishnamoorti

2015

Polymer

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The development of interpenetrating polymer networks provides a route to create tough materials that maintain high strength and stiffness, suitable for meeting the demands of an offshore wind turbine environment. This work has focused on a system composed of diglycidyl ether of bisphenol A (DGEBA)-based epoxy resin, contributing high tensile strength and modulus, and polydicyclopentadiene (polyDCPD), which has a higher toughness and impact strength as compared to other thermoset polymers. In situ Fourier transform infrared spectroscopy was used to explore the reaction kinetics in neat, diluted and sequentially cured mixtures of epoxy resin and polyDCPD. There were significant differences in the rate of network formation in the two neat systems, as the rate of anhydride curing of the epoxy was extremely slow at the temperatures required for reasonably measurable dicyclopentadiene (DCPD) ring-opening metathesis polymerization. The dissimilar kinetics of these two systems were leveraged in the design of a sequential curing protocol in which the DCPD was first cured in the presence of the epoxy resin components, followed by curing of the epoxy resin at an elevated temperature. The curing kinetics of the macroscopically phase separated domains of the epoxy resin components in the presence of the polyDCPD network behaved as expected for a diluted epoxy resin. These results provide the kinetic basis for future studies to prepare interpenetrating polymer networks which employ thermodynamic control of phase separation such as through the addition of compatibilizing molecules.

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“…However, the reaction between epoxy and secondary hydroxyl functionalities is controversial. Whereas Tackie and Martin and others22, 23 claimed that the secondary hydroxyl functionalities on the epoxy chain are less reactive than the epoxy functionalities and do not react below 230 to 270°C, Li et al and other authors24–26 found hydroxyl functionality no less reactive than the epoxy functionality and so did not neglect its participation in the homopolymerization reaction. If the participation of the secondary hydroxyl groups is negligible, the homopolymerization must result in essentially linear polymerization of the epoxy oligomers.…”

Section: Discussionmentioning

confidence: 97%

“…Simplified representations of epoxy resin and MDSA molecules are used. (Note: In homopolymerization, reaction between epoxy and secondary hydroxyl group is also possible but its occurrence is controversial 22–26…”

Section: Discussionmentioning

confidence: 99%

Wrinkling of epoxy powder coatings

Basu

Scriven

Francis

et al. 2005

J of Applied Polymer Sci

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Differential scanning calorimetry (DSC) and mechanical profilometry were used to study wrinkle formation in curing epoxy powder coatings. Powder coating formulations were studied that contained solid epoxy resins, methylene disalicylic acid (MDSA) crosslinker, and an amine-blocked Lewis acid catalyst. Both the crosslinker (MDSA) and the amine-blocked catalyst are required for wrinkle formation. Evaporation of the blocking amine from the free surface of the coating generated a depthwise gradient in the extent of polymerization and crosslinking, and hence in the degree of solidification, as evidenced by the formation of a mechanical skin prior to wrinkling. It is hypothesized that compressive elastic stress develops in the still swellable skin when unreacted low-molecular-weight material from beneath diffuses up into the monomer-or oligomer-depleted crosslinking skin and swells it. This compressive stress, if above a critical value, buckles the skin to produce wrinkles. Experimentally observed compositional requirements for wrinkle formation were consistent with the proposed mechanism. The size of the wrinkles can be controlled by varying formulation parameters such as the amount of catalyst or crosslinker. Increasing the amount of catalyst decreased both the wavelength and the amplitude of the wrinkle pattern. Increasing the amount of crosslinker initially increased the amplitude of the wrinkles; after reaching a maximum level, the wrinkle amplitude decreased. DSC was a useful tool to understand the critical reactions responsible for wrinkling in this system. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 116 -129, 2005

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Kinetics and curing mechanism of epoxy and boron trifluoride monoethyl amine complex system

Cited by 11 publications

References 0 publications

Study on curing kinetics and curing mechanism of epoxy resin based on diglycidyl ether of bisphenol a and melamine phosphate

Study on curing kinetics and curing mechanism of epoxy resin based on diglycidyl ether of bisphenol a and melamine phosphate

Concurrent curing kinetics of an anhydride-cured epoxy resin and polydicyclopentadiene

Wrinkling of epoxy powder coatings

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