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We report the first sol−gel
polymerization of alkoxysilane monomers in supercritical carbon dioxide
(SCCD) as the polymerization solvent. Monolithic silica and
silsesquioxane gels were formed in SCCD by the nonaqueous
polymerization of tetramethoxysilane and
1,4-bis(triethoxysilyl)benzene, respectively, with formic
acid (99%). The gels were dried to give high surface area,
mesoporous aerogels by simply venting carbon dioxide from the
autoclave.
New highly cross-linked polysiloxanes were prepared by sol−gel
polymerization of 1,6-bis(diethoxymethylsilyl)hexane (1) and
1,4-bis(diethoxymethylsilyl)benzene (2).
Hydrolysis
and condensation of 1 and 2 under acidic and
basic conditions with 4 equiv of water led to
the rapid formation of hexylene- and phenylene-bridged polysiloxane
gels. The dry gels
(xerogels) were intractable, insoluble materials that were noticeably
hydrophobic, exhibiting
no swelling in organic solvents or water. Most of the xerogels
were high surface area,
mesoporous materials. Hexylene-bridged polysiloxanes prepared
under acidic conditions
were always nonporous regardless of whether they were
processed to afford xerogels or
supercritically dried as aerogels. Hexylene-bridged polysiloxanes
prepared under basic
conditions and all of the phenylene-bridged polysiloxanes were
mesoporous with surface
areas as high as 1025 m2/g.
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