R. Takahashi et al., Preparation of microporous silica gel by sol-gel process in the presence of ethylene glycol oligomers, B CHEM S J, 73(3), 2000, pp. 765-774
A microporous silica gel was prepared by a sol-gel process in the presence
of ethylene glycol (EG) and its oligomers (oligoEG), and the pore formation
process was investigated by using NMR and TG-DTA. The micropore volume cha
nged with the polymerization degree of oligoEG, and showed a minimum at the
trimer of EG. An attractive interaction between silanol and organic additi
ves plays a key role in micropore formation: the interaction inhibits the b
ond formation of Si-O-Si during drying and heating, and heterogeneous domai
ns which convert into micropore are formed after the combustion of additive
s. There are two kinds of interaction: one is eater (Si-OR) bond formation
of a silanol with an end hydroxy group of additives; the other is hydrogen
bonding between a silanol and an ether oxygen of additives. The former inte
raction is significant for EG. With increasing length of oligoEG, however,
the former interaction rapidly disappears, while the latter becomes stronge
r. Because of a minimum in the combination of these interactions, the minim
al volume of the micropore is observed.