Characterization of the reactivity of a silica derived from acid activation of sepiolite with silane by 29Si and 13C solid-state NMR

被引:34
作者
Valentin, J. L. [1 ]
Lopez-Manchado, M. A. [1 ]
Posadas, P. [1 ]
Rodriguez, A. [1 ]
Marcos-Fernandez, A. [1 ]
Ibarra, L. [1 ]
机构
[1] Inst Sci & Technol Policy, Madrid 28006, Spain
关键词
surface modification; silanization; organosilane; bis(triethoxysilylpropyl)tetrasulfane (TESPT); silica; sepiolite; acid treatment; solid state NMR spectroscopy; environmental scanning electron microscopy (ESEM); rubber;
D O I
10.1016/j.jcis.2005.12.056
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
The mechanism of the reaction between a silica sample coming from acid treatment of sepiolite (denominated Silsep) and an organosilane, namely bis(triethoxysilylpropyl)tetrasulfane (TESPT), has been evaluated by solid state NMR spectroscopy, being compared with the silanization reaction of a commercial silica. The effect of the silane concentration and temperature on the course of the reaction was considered. Experimental results indicate that the silanization reaction is more effective in the case of Silsep, favoring both the reaction of silane molecules with the filler surface and the reaction between neighboring silane molecules. This different behavior is attributed to structural factors, moisture, and number of acid centers on silica surface. Environmental scanning electron microscopy (ESEM) was used to deposit micrometric water drops on the surface of these samples and to evaluate the proportion and distribution of the organophylization process. (c) 2006 Elsevier Inc. All rights reserved.
引用
收藏
页码:794 / 804
页数:11
相关论文
共 44 条
[1]   Characterization of Spanish sepiolites by high-resolution solid-state NMR [J].
Aramendia, MA ;
Borau, V ;
Jimenez, C ;
Marinas, JM ;
Ruiz, JR .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 1997, 8 (04) :251-256
[2]   Silica from sepiolite: Preparation, textural properties, and use as support to catalysts [J].
Aznar, AJ ;
Gutierrez, E ;
Diaz, P ;
Alvarez, A ;
Poncelet, G .
MICROPOROUS MATERIALS, 1996, 6 (02) :105-114
[3]   SOLID-STATE SI-29 SPIN-LATTICE RELAXATION IN SEVERAL 2-1 PHYLLOSILICATE MINERALS [J].
BARRON, PF ;
SLADE, P ;
FROST, RL .
JOURNAL OF PHYSICAL CHEMISTRY, 1985, 89 (15) :3305-3310
[4]  
BARRON PF, 1985, AM MINERAL, V70, P758
[5]  
Blume A, 2000, KAUT GUMMI KUNSTST, V53, P338
[6]   ACTIVATION OF A SEPIOLITE WITH DILUTE-SOLUTIONS OF HNO3 AND SUBSEQUENT HEAT-TREATMENTS .2. DETERMINATION OF SURFACE ACID CENTERS [J].
BONILLA, JL ;
LOPEZGONZALEZ, JDD ;
RAMIREZSAENZ, A ;
RODRIGUEZREINOSO, F ;
VALENZUELACALAHORRO, C .
CLAY MINERALS, 1981, 16 (02) :173-179
[7]   Fillers for balancing passenger tire tread properties [J].
Byers, JT .
RUBBER CHEMISTRY AND TECHNOLOGY, 2002, 75 (03) :527-547
[8]   The structure of acid treated sepiolites:: small-angle X-ray scattering and multi MAS-NMR investigations [J].
Dékány, I ;
Turi, L ;
Fonseca, A ;
Nagy, JB .
APPLIED CLAY SCIENCE, 1999, 14 (1-3) :141-160
[9]   AL MODIFIED SEPIOLITE AS CATALYST OR CATALYST SUPPORT [J].
DELACAILLERIE, JBD ;
FRIPIAT, JJ .
CATALYSIS TODAY, 1992, 14 (02) :125-140
[10]  
DELACAILLERIE JBD, 1994, CLAY MINER, V29, P313