2007
DOI: 10.1021/ja067987a
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Use of p-Toluenesulfonic Acid for the Controlled Grafting of Alkoxysilanes onto Silanol Containing Surfaces:  Preparation of Tunable Hydrophilic, Hydrophobic, and Super-Hydrophobic Silica

Abstract: The modification of Aerosil 200 has been carried out using methoxysilanes in toluene reflux, with p-toluenesulfonic acid as the catalyst. Both trimethoxyalkyl silanes (methyl, ethyl, propyl, butyl, hexyl, octyl, and octadecyl) and trialkylmethoxy silanes (trimethyl and dimethyloctyl) have been used. The surface has been studied by 29Si NMR, 13C NMR, elemental analysis, thermogravimetry, water contact angle, and BET analysis. When incorporating trimethoxysilanes, a plateau of modification was achieved after 1 h… Show more

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Cited by 103 publications
(106 citation statements)
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“…The 29 Si MAS NMR spectrum of the yolk-shell mesoporous hybrid spheres shows six signals at -93, -102, and -110 ppm, corresponding to Q 2 ( Si (OSi) 2 (OX) 2 , X = H or Et), Q 3 ( Si (OSi) 3 (OX)), and Q 4 ( Si (OSi) 4 ) species, and at -47, -58, and, -66 ppm, corresponding to T 1 (C-Si (OSi) 1 (OX) 2 , X = H or Et), T 2 (C-Si (OSi) 2 (OX)), and T 3 (C-Si (OSi) 3 ) species (Figure 2 b, curve i). [ 46,47 ] The observation of these T sites in the spectrum further indicates the condensation of BTSE into the spheres. Quantitative analysis shows that 33% of the silicon atoms in the yolk-shell mesoporous hybrid spheres are at the Q sites and that 67% of the silicon atoms are at the T sites.…”
Section: Communicationmentioning
confidence: 84%
“…The 29 Si MAS NMR spectrum of the yolk-shell mesoporous hybrid spheres shows six signals at -93, -102, and -110 ppm, corresponding to Q 2 ( Si (OSi) 2 (OX) 2 , X = H or Et), Q 3 ( Si (OSi) 3 (OX)), and Q 4 ( Si (OSi) 4 ) species, and at -47, -58, and, -66 ppm, corresponding to T 1 (C-Si (OSi) 1 (OX) 2 , X = H or Et), T 2 (C-Si (OSi) 2 (OX)), and T 3 (C-Si (OSi) 3 ) species (Figure 2 b, curve i). [ 46,47 ] The observation of these T sites in the spectrum further indicates the condensation of BTSE into the spheres. Quantitative analysis shows that 33% of the silicon atoms in the yolk-shell mesoporous hybrid spheres are at the Q sites and that 67% of the silicon atoms are at the T sites.…”
Section: Communicationmentioning
confidence: 84%
“…Based on their silane chemistry, only the outer surfaces of hollow SNP shells could be modifi ed by the hydrophobic OTMS. [18][19][20] The ultimate results are the formation of SHSMs with hydrophilic cores (due to the PAH) and amphiprotic shells (due to the PAH and OTMS) because the interpenetrating PAH coexists with the OTMS on the outer shell. Figure 1 b-d shows scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images of each step of the formation of the SHSMs.…”
Section: Resultsmentioning
confidence: 99%
“…[4][5][6][7][8] They mostly involve the reaction of organosilanes with the silanol group of the silica matrix. [9] The nature of the resulting material depends heavily on the experimental conditions used during the grafting and parameters such as the temperature, the dilution, or the polarity of the solvent often lead to products having different properties. [10,11] Equally important are titania matrices onto which organic moieties bearing generally carboxylic acid functions have been grafted, almost exclusively by adsorption phenomena, and thoroughly studied by various spectroscopic techniques.…”
Section: Introductionmentioning
confidence: 99%