Heat-Treatment Effects on Polyorganosiloxane Spherical Particles Prepared in W/O Emulsion

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Monodispersed micro polyorganosiloxane spherical particles synthesized from methyltrimethoxysilane in W/O emulsion consisting of sorbitantrioleate (SPAN85), n-octane, and H2O were heat treated from 100 to 600°C in the air, and examined from SEM, NMR, FT-IR, and specific surface area measurements. The heating process is characterized as follows. Before the formation of the Si-O-Si linkage by oxidation of CH3 in Si-CH3 near 410°C, silica network in the particles consists of only T2 and T3 units and the transformation of T2 into T3 and the shrinkage of the particles were observed up to 400°C, specific surface area showing the maximum value (18 m2 g-1) for the particles heat treated at 300°C. We concluded that the origin of the change in thespecific surface area was related to the changes in both the degree of polymerization and the shrinkage. On the other hand, after the formation of the new Si-O-Si linkage by the oxidation, silica network consists of only Q units and the particles were thermally stable with almost constant diameter and specific surface area.
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