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Synthesis and Thermal Properties of Resorcinol-Furfural Thermosetting Resin.

ABSTRACT: A mild and effective synthesis of resorcinol-furfural (RF) thermosetting resin was proposed with ethanol as a distinctive solvent, which, as a usually neglected factor, was shown to not only help form a homogeneous reaction system but also observably reduce the energy barriers between the early intermediates and transition states in addition reactions by explicit solvent effects, drawn from theoretical calculation conclusions. Besides, the para-additions on aromatic rings were more dominant than ortho-additions with the same reactants, which affected the final link types of monomers verified by Fourier transform infrared spectroscopy and two-dimensional nuclear magnetic resonance tests. The prepared resin can be assigned to a relatively fast gel speed and a high residual mass (65.25%) after pyrolysis in a N2 atmosphere by adjusting the molar ratios of F to R, and the curing of that was a complex reaction, with a curing temperature around 149 °C and an activation energy of about 49.11 kJ mol-1 obtained by the Kissinger method.

SUBMITTER: Liu J

PROVIDER: S-EPMC7203984 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:A novel organic-inorganic hybrid containing allyl benzoxazine and polyhedral oligomeric silsesquioxane (POSS) was synthesized by the thiol-ene (click) reaction. The benzoxazine (BOZ)-containing POSS (SPOSS-BOZ) copolymerized with benzoxazine/epoxy resin was used to prepare composites of SPOSS-PBZ-E nanocomposites(NPs). The polymerization behavior was monitored by FTIR and non-isothermal differential scanning calorimetry (DSC), which showed that the composites had completely cured with multiple polymerization mechanisms according to the oxazine ring-opening and epoxy resin (EP) polymerization. The thermal properties of the organic-inorganic polybenzoxazine (PBZ) nanocomposites were analyzed by DSC and thermogravimetric analysis (TGA). Furthermore, the X-ray diffraction analysis and the scanning electron microscopy (SEM) micrographs of the SPOSS-PBZ-E nanocomposites indicated that SPOSS was chemically incorporated into the hybrid nanocomposites in the size range of 80-200 nm. The flame retardancy of the benzoxazine epoxy resin composites was investigated by limiting oxygen index (LOI), UL 94 vertical burn test, and cone calorimeter tests. When the amount of SPOSS reached 10% or more, the vertical burning rating of the curing system arrived at V-1, and when the SPOSS-BOZ content reached 20 wt %, the thermal stability and flame retardancy of the material were both improved. Moreover, in the cone calorimeter testing, the addition of SPOSS-BOZ hindered the decomposition of the composites and led to a reduction in the peak heat release rate (pHRR), the average heat release rate (aHRR), and the total heat release (THR) values by about 20%, 25%, and 25%, respectively. The morphologies of the chars were also studied by SEM and energy dispersive X-ray spectroscopy (EDX), and the flame-retardant mechanism of POSS was mainly a condensed-phase flame retardant. The ceramic layer was formed by the enrichment of silicon on the char surface. When there are enough POSS nanoparticles, it can effectively protect the combustion of internal polymers.

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Synthesis and Thermal Properties of Resorcinol-Furfural Thermosetting Resin.

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