J. Rathousky et al., THE EFFECTS OF PROCESSING PARAMETERS ON THE SYNTHESIS OF SILICEOUS MCM-41 FROM COLLOIDAL SILICAS, Collection of Czechoslovak Chemical Communications, 63(2), 1998, pp. 271-282
Well-ordered as-synthesized siliceous MCM-41 mesoporous molecular siev
es can be prepared from the sol of colloidal silica (Ludox HS-40 and A
S-40) only under optimized conditions. Two processing parameters have
a significant effect on the structure. First, the period of stirring t
he mixture of Ludox AS-40 or HS-40 and tetraethylammonium hydroxide sh
ould be extended to 22 h. Second, the following temperature regime sho
uld be used: the reaction mixture consisting of colloidal silica, tetr
aethylammonium hydroxide, hexadecyltrimethylammonium chloride and wate
r is being first aged at ambient temperature for 20 h, then the temper
ature is gradually increased and finally the mixture is kept at 100 de
grees C for 40 h. As-made MCM-41 prepared even by an optimized procedu
re contains after calcination some proportion of an amorphous phase. E
xtraction with water of the as-made material is a suitable procedure f
or the improvement of the phase purity as less well-ordered and amorph
ous particles are preferentially dissolved and thus removed. In this w
ay, a substantial improvement in the quality of MCM-41 molecular sieve
s can be achieved.