Preparation and Characterization of Degradable Poly(silyl ester) and the Self-Crosslinking Reaction of Poly(silyl ester) without Solvent
The new poly(silyl ester) has been prepared by the polycondensation reaction of 1,5-dichloro-1,1,5,5-tetramethyl-3,3-diphenyl-trisi1oxane with di-tert-butyl fumarate by the elimination of tert-butyl chloride as a driving force. To investigate the self-crosslinking reaction of the unsaturated poly(silyl ester), poly(1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane) was self- crosslinked in the presence of 2, 2'-azobis(isobutyronitri1e) (AIBN) as a radical initiator without solvent. After the self-crosslinking, the unsaturated poly(silyl ester), which was viscous liquids, turned into solid product. The characterization of the poly(silyl ester) and the self-crosslinked product included 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Comparisons were made between the linear poly(silyl ester) and the self-crosslinked products. It was found that after crosslinking, the important resonance signal for ethenylene (C=C) of the poly(silyl ester) reduced, which show that the crosslinking reaction is carried out. The self-crosslinked product exist the structures of linear isomer and four-membered ring isomer. The glass-transition temperatures of the self-crosslinked poly(silyl ester) was higher than that of the uncrosslinked poly(silyl ester), and the thermal stability of the self-crosslinked poly(silyl ester) was better than that of uncrosslinked poly(silyl ester).
Xie Yi and Li Mi
D. J. Zhou et al., "Preparation and Characterization of Degradable Poly(silyl ester) and the Self-Crosslinking Reaction of Poly(silyl ester) without Solvent", Advanced Materials Research, Vols. 129-131, pp. 862-866, 2010