Novel heat resistant methyl-tri(phenylethynyl)silane resin: Synthesis, characterization and thermal properties

摘要

Methyl-tri(phenylethynyl)silane (MTPES) was successfully synthesized by the reaction of lithium phenylacetylide with methyltrichlorosilane. The structure was characterized by HRMS, FTIR, H-1-NMR, C-13-NMR Si-29-NMR, and elementary analysis. Thermal cure process was monitored by DSC, DMA, and FTIR. MTPES was heated to free flowing liquid around 130 degrees C and thermally polymerized at 327-377 degrees C to form thermoset. Thermal and oxidative properties were evaluated by TGA analysis. Thermoset exhibits extremely high heat-resistance and TGA curve in nitrogen shows the temperature of 5% weight loss (Td(5)) of 695 degrees C and total weight loss at 800 degrees C of 7.1%. TGA shows a high Td5 of 565 degrees C even in air, although the total weight loss at 800 degrees C was 56.1% of the initial weight, much higher than that in nitrogen. The high heat resistance of MTPES was ascribed to crosslinking reaction concerning ethynyl groups. Aging studies performed at elevated temperatures in air on a thermoset showed that MTPES is oxidatively stable to 300 degrees C. (c) 2006 Wiley Periodicals, Inc.