TY - JOUR
T1 - Periodic mesoporous benzene- and thiophene-silicas prepared using aluminum chloride as an acid catalyst
T2 - Effect of aluminum salt/organosilane ratio and stirring time
AU - Cho, Eun Bum
AU - Kim, Dukjoon
AU - Górka, Joanna
AU - Jaroniec, Mietek
PY - 2009/4/2
Y1 - 2009/4/2
N2 - Periodic mesoporous benzene-silica and thiophene-silica with two dimensional (2D) p6mm symmetry were synthesized in the presence of a nonionic poly(ethylene oxide)-poly(DL-lactic acid-co-glycolic acid)- poly(ethylene oxide) (PEO-PLGA-PEO) block copolymer template using aluminum chloride hexahydrate (AlCl 3 ·6H 2O) as an acid catalyst instead of the proton-containing hydrochloric acid (HCl). 1,4-Bis(triethoxysilyl) benzene (BTEB) and 2,5-bis(triethoxysilyl)thiophene (BTET) were used as organosilica precursors. The effect of the AlCl 3 ·6H 2O/ organosilane ratio and the stirring time was investigated to find the optimum experimental conditions. It was shown that the highly ordered 2D hexagonal mesostructures of aromaticsilicas were formed using relatively small amounts of AlCl 3 ([AlCl 3 ·6H 2O]/[BTEB] and [AlCl 3 ·6H 2O]/[BTET] ≥ 1) and a stirring time of about 20 h. The BET surface areas, pore volumes, and pore diameters of the benzene- and thiophene-silicas studied varied from 505 to 1215 m 2 g -1, from 0.55 to 1.62 cm 3 g -1, and from 7.55 to 9.23 nm, respectively, depending on the aluminum salt concentration and the stirring time. In the case of thiophene-silica, the optimum experimental conditions for the formation of ordered mesostructure were [AlCl 3 ·6H 2O]/[BTET] ) 1 and a stirring time of 20 h. Also, the chemistry and crystallinity of aromaticsilicas were investigated using solid-state 13C-, 29Si-, and 27Al-NMR and wide-angle X-ray scattering methods.
AB - Periodic mesoporous benzene-silica and thiophene-silica with two dimensional (2D) p6mm symmetry were synthesized in the presence of a nonionic poly(ethylene oxide)-poly(DL-lactic acid-co-glycolic acid)- poly(ethylene oxide) (PEO-PLGA-PEO) block copolymer template using aluminum chloride hexahydrate (AlCl 3 ·6H 2O) as an acid catalyst instead of the proton-containing hydrochloric acid (HCl). 1,4-Bis(triethoxysilyl) benzene (BTEB) and 2,5-bis(triethoxysilyl)thiophene (BTET) were used as organosilica precursors. The effect of the AlCl 3 ·6H 2O/ organosilane ratio and the stirring time was investigated to find the optimum experimental conditions. It was shown that the highly ordered 2D hexagonal mesostructures of aromaticsilicas were formed using relatively small amounts of AlCl 3 ([AlCl 3 ·6H 2O]/[BTEB] and [AlCl 3 ·6H 2O]/[BTET] ≥ 1) and a stirring time of about 20 h. The BET surface areas, pore volumes, and pore diameters of the benzene- and thiophene-silicas studied varied from 505 to 1215 m 2 g -1, from 0.55 to 1.62 cm 3 g -1, and from 7.55 to 9.23 nm, respectively, depending on the aluminum salt concentration and the stirring time. In the case of thiophene-silica, the optimum experimental conditions for the formation of ordered mesostructure were [AlCl 3 ·6H 2O]/[BTET] ) 1 and a stirring time of 20 h. Also, the chemistry and crystallinity of aromaticsilicas were investigated using solid-state 13C-, 29Si-, and 27Al-NMR and wide-angle X-ray scattering methods.
UR - https://www.scopus.com/pages/publications/65249148482
U2 - 10.1021/jp810179g
DO - 10.1021/jp810179g
M3 - Article
AN - SCOPUS:65249148482
SN - 1932-7447
VL - 113
SP - 5111
EP - 5119
JO - Journal of Physical Chemistry C
JF - Journal of Physical Chemistry C
IS - 13
ER -