Low viscosity and low temperature curing reactive POSS/epoxy hybrid resin with enhanced toughness and comprehensive thermal performance† † Electronic supplementary information (ESI) available. See DOI: https://doi.org/10.1039/d3ra08390j
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ABSTRACT:
SUBMITTER: Han R
PROVIDER: S-EPMC10905323 | biostudies-literature | 2024 Mar
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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Project description:The curing of a mixture of glycidyl phenyl ether (GPE) and hexahydro-4-methylphthalic anhydride (MHHPA) with zeolitic imidazolate frameworks (ZIFs)-ZIF-7, ZIF-8, ZIF-11, and ZIF-14-as latent thermal initiators has been critically evaluated. For ZIF-8 and ZIF-14, the % conversion values for GPE were 92 and 93%, respectively, for curing at 100 °C and for 1 h. With regard to the stability of ZIF-8 and ZIF-14 in the GPE-MHHPA mixture, the % conversion values for GPE were 11 and 12% for storage over 8 days at 25 °C. The ZIF-8 and ZIF-14 initiators exhibited excellent thermal latency for heating at 100 °C and showed good stability for storage at 25 °C. To evaluate the practicality of the resin curing system, the reactions of 2,2-bis(4-glycidyloxyphenyl)propane (DGEBA) and MHHPA with ZIFs were studied by differential scanning calorimetry. Prominent exothermic peaks for ZIF-8 and ZIF-14 were observed at 157 and 162 °C, respectively; by comparison, for the commercially available microencapsulated latent thermal initiators HX-3088 and HX-3722, the respective peak maxima were 177 and 181 °C, respectively. The exothermic peak maxima for ZIF-8 and ZIF-14 were lower than those for HX-3088 and HX-3722. The ZIF-8 and ZIF-14 initiators can be stored in precured epoxy resin at 25 °C and cured by lower temperatures compared with commercially-available initiators HX-3088 and HX-3722.
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