J. Am. Chem. Soc., 1998, 120(24), , DOI: /ja974025i

Transcription

1 J. Am. Chem. Soc., 1998, 120(24), , DOI: /ja974025i Terms & Conditions Electronic Supporting Information files are available without a subscription to ACS Web Editions. The American Chemical Society holds a copyright ownership interest in any copyrightable Supporting Information. Files available from the ACS website may be downloaded for personal use only. Users are not otherwise permitted to reproduce, republish, redistribute, or sell any Supporting Information from the ACS website, either in whole or in part, in either machinereadable form or any other form without permission from the American Chemical Society. For permission to reproduce, republish and redistribute this material, requesters must process their own requests via the RightsLink permission system. Information about how to use the RightsLink permission system can be found at Copyright 1998 American Chemical Society

2 '- U~rIYuYO %M111r11LcU1 '.~11c1 d 3UUdrLY J. LXIH. a ulu. v 1/-V r-dgruuv/9. LAdU 31tPPIUMUIiLcdi ragr, I b a Chemical Shift (ppm) Figu L 2Si MAS NMR spectra of (a) SBA- 11 prepared using C 16 E0O surfactant species at room temperature; (b) SBA-15 prepared using polyoxyalkylene block copolymer EOfPO 7 E4On surfactant species at 35 OC.

3 '"UHrIlluall %-111r,111lual 13UUIr'Ly J. '"un. auu. V 1/V r-dgrukj/--t Z HdU OUPPIUMUIlLdl Fdgr, / 600 Cl) 45. Pore size 31 A F BET Surface area 1150 m 2 Ig o' Pore Volume = 0.83 cm 3 /g E T E C) S < E > Pore Diameter, (A) Relative Pressure, (P/Po) Figue I Nitrogen adsorption-desorption isotherm plots and pore size distribution curve from the adsorption branch of calcined SBA-12 prepared using C 18 EO 1 surfactant species at room temperature. SI.1

4 as-synthesized calcined 1 C Figure III. Powder X-ray diffraction (XRD) patterns of (A) as-synthesized and (B) calcined mesoporous silica prepared using Tween 60 surfactant species with different concentrations at room temperature.

5 V1998 American Lhemical Society J. Am. Uliem. soc. V 12U Fageou24 Lnao supplemental Fage 4 Cf) 101i I IIII (IY) CO C) OL Figure IV. Powder X-ray diffraction (XRD) patterns of lamellar mesostructured silica prepared using Tween 60 surfactant species in higher concentration (16 wt %) at room temperature. Si

6 Saouan I Y M area 150 BET Surface Area 570 m 2 /g BET Surface area 610 m 2 /g Pore Volum 0.52 cm3/ g C E U100 d < L e <0, Relative Pressure, (P/P 1 ) Relative Pressure, (P/P 0 ) FiueV Nitrogen adsorption/desorption isotherm plots and pore-size 0C0 distribution s 160cn cocetato curve from the Poe Dmer, A)ur0 adsorption branch of (a) calcined mesoporous silica 0 ~ 0. ~ ~ (54 at8 room A SBA prepared. using C 12 EO 4 surfactant eltv rssr,(/ species (2 wt %) at room temperature; (b) calcined mesophase, probably L 3, prepared using C C12EO4 ssurfactant species at 60 "C (c) calcined L silica mesostructure prepared using a higher

7 4C0 *1-.' C', U) Figure VI. Powder X-ray diffraction (XRD) patterns of as-synthesized and calcined SBA- 15 prepared using polyoxyalkylene block copolymer EO 20 PO 70 EO 20 surfactant species, (a) without addition of organic swelling agent; (b) with addition of cosolvent orzanic molecules 1,3,5-trimethylbenzene (TMB). The chemical composition of the reaction mixture was 4 g copolymer: 3 g TMB : mole TEOS: 0.24 mole HCl: 6.67 mole HO

8 vt'6 American onemicai 3ociety J. Am. k-nem. 3oc. v izu rageouz, Lnao 3uppiementai rage / 10 nm Figure VI. Transmission electron micrographs (TEM) with different orientations of calcined hexagonal SBA-15 prepared using E0OP07O block copolymer species.

9 a b M E -0c 1125 E c 12 pore size 260 A.2- E C' Pr pore volume 2.2 cm 3 /g.9 Pore size 47 A O 100 BET Surface area 690 m/g 200 < - 2 /g BET Surface Area m Pore Volume = 0.56 cm 3 /g 0 I > BET Surface Area ,8 1 0 > 910 m 2 /g ~~ Relative Pressure, (P/P 0 ) Relative Pressure, (P/P ) E 3 - C 8 2E pore size 89 A 2 6 pore volume 1.17 cm'/g 6 -~ I- >4- w O> 2- w 2 o Pore Diameter (A) (- 0 Pore Diameter (A) Pore Diameter (A) 1-0 C EigureYII Nitrogen adsorption-desorption isotherm plots andpo sz dstributioni! fix=' the adsorption branch of calcined SBA-15 prepared using EO 2 0 POIOEQn block copolymer species, (a) at room temperature; (b) at 100 *C; (c) in the presence of 1,3,5-trimethylbenzene cosolvent species at 100 *C.

10 vt'6 American onemicai 3ociety J. Am. Linem. 3oc. v izu rageouz, Lnao 3uppiementai rage! O09 14 og -90 -I C 70-1 DTA 50 TGA -6 I II Temperature ( OC) Figure I. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) traces for as-synthesized SBA-15 prepared using the block copolymer EOWPO 7 0O20 NI

11 v1 6 American onemicai 3ociety J. Am. k-nem. 3oc. v izu rageouz, Lfnao 3uppiementai rage iu Figure X. Transmission electron micrographs (TEM) with different orientations (top, [110]; bottom, [1111) of calcined hexagonal mesoporous silica SBA-16 prepared by using EO 1 PO 7 0 EO 10 6 block copolymer species. Ci.2

12 ' 1:;,:; 011L1 r~lal ' %I11r111Rdl1.. 3UU~r'LY J. I-un. a ulu. V 1/-V radgrukj/9. LAHdU 31tPIUMIfl~Ldi rcgr, I1I 300 Pore size 54 A BET Surface area 740 m 2 /g 225 Pore Volume = 0.45 cm 3 /g CL E~ o Pore Diameter, (A) Relative Pressure, (P/Po) Figure XI. Nitrogen adsorption-desorption isotherm plots and pore size distribution curve from the adsorption branch of calcined mesoporous silica SBA-16 prepared by using EO 1 PO 70 EO 1 0 block copolymer species.

13 C o O0 - o x8 401 ITx8 d 000 I\ I IM igur XI Powder X-ray diffraction (XRD) patterns of (a) as-synthesized and (b) calcined MCM-41 silica prepared using the cationic surfactant C 16 H 33 N(CH 3 ) 3 Br; (c) calcined MCM-41 after heating in boiling water for 6 h; and (d, e) Calcined SBA-15 prepared by using the block copolymer EO 20 P0 70 E0 20 after heating in boiling water for (d) 6 h, (e) 24 h. ST