P. Vandervoort et al., SYNTHESIS OF HIGH-QUALITY MCM-48 AND MCM-41 BY MEANS OF THE GEMINI SURFACTANT METHOD, JOURNAL OF PHYSICAL CHEMISTRY B, 102(44), 1998, pp. 8847-8851
Pure silica MCM-48 and MCM-41 materials were prepared using GEMINI sur
factants, with the general formula 2n+1N+(CH3)(2)-(CH2)(s)-N+(CH3)(2)C
mH2m+1].2Br(-), abbreviated as GEM n-s-m. The alkyl chain length (n,m)
determines the pore size, whereas the length of the spacer (s) influe
nces the crystallographic phase formed. A spacer length of 10-12 C yie
lds the cubic MCM-48; smaller spacers favor the hexagonal MCM-41 phase
. A hydrothermal treatment is introduced as an intermediate synthesis
step, which strongly improves the quality and stability of the calcine
d materials. The hydrothermal treatment reduces the synthesis time of
high-quality MCM-48 to only 2 days. Both GEM 18-12-18 and GEM 16-12-16
yield excellent MCM-48, with a surface area in the range 1200-1600 m(
2)/g and pore volumes exceeding 1.2 mL/g. The maxima of the very narro
w pore size distributions are found at r(p) = 13.1 and 12.2 Angstrom,
respectively. The GEM 16-10-16 and GEM 18-10-18 surfactants also yield
MCM-48, but the quality of these materials is Fewer. The GEM 16-8-16
finally yields MCM-41.