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Series of Polymethylphenylsiloxane (PMPS)/Polydiphenylsiloxane (PDPS) statistical random copolymers with different PDPS content were synthesized through a living anionic copolymerization from hexaphenylcyclotrisiloxane (P3) and 1,3,5-trimethyl-1,3,5-triphenylcyclotrisiloxaiie (D3Ph) in various solvent system, using n-butyllithium as initiator, and diphenylmediylchlorosilane as terminator. These copolymers were characterized by GPC and 1H-NMR. The monomer reactivity ratios of the D3Ph/P3 copolyinerization in various solvent system were estimated from Fineman-Ross equation. The monomer sequence of the copolymers was confirmed by the 1H-NMR and the glass transition temperature (Tg) of the synthesized copolymers. The Tg and mesophase transition temperature (Tm) of these copolymers were determined by Differential Scanning Calorimeter (DSC). The isotropic temperature (Ti) of the copolyiners were measured by the Polarized Optical Microscopy (POM). Basing upon DSC and POM results, the phase diagrams of these copolymers were established. The thermal stability (T10) of these copolymers were measured by Thermogravimetry Analysis (TGA).
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