Synthesis of ordered mesostructured polymer–organosilica composites by the triconstituent co-assembly method
Introduction
Recently, highly ordered mesoporous polymers have been reported through organic–organic assembly between block polymers and phenolic resins [1], [2], [3]. Incorporation of rigid constituents, for example silica, into the polymer networks can not only trigger co-assembly to form ordered mesostructures with designed functionalities, but also effectively reduce shrinkage during thermal treatment [4]. With such a co-assembly pathway, two or more components can be combined together to produce composites with high homogeneity that previously have been shown to be phase separable or even incompatible [5]. Periodic mesoporous organosilicas (PMOs) have received considerable attention in materials science in the last decade [6], [7]. In this regard, the full potential of organosilica/surfactant mesophases as ‘precursors’ for the formation of mesostructured composites with phenolic resins has not been fully explored. Inspired by such one-pot fabrication of ordered mesoporous polymer–silica composites, it would be worthwhile to devote much effort to the synthesis of organic polymer frameworks combined with mesoporous organosilica/surfactant mesophases by manipulating polymerization [8]. Here, we report a triconstituent co-assembly approach to synthesize ordered hexagonal mesoporous polymer–organosilica composites. The adsorption properties of these hybrid composites for benzene were also investigated.
Section snippets
Material and methods
The composites were prepared by triconstituent co-assembly of resols [1], oligomer silicates from 1,2-bis(triethoxysilyl)ethane (96%) (BTSE), and triblock copolymer Pluronic F127 (EO106PO70EO106) template. Typically, 0.40 g of F127 was dissolved in a mixture of 2.0 g of ethanol and 0.037 g of 0.2 M HCl and stirred for 1 h at 40 °C to afford a clear solution. Then, 0.44 g of BTSE and 1.25 g of resol solution (20 wt.% in ethanol) [1] were added. After stirring for 2 h, the mixture was transferred into
Mesostructure
XRD pattern of the as-made composite MP–COS–0.44BTSE (Fig. 1a) shows one sharp diffraction peak, which is difficult to index. However, after calcination, the product yields three well-resolved diffraction peaks (Fig. 1b), associated with the 10, 11, and 20 reflections of two-dimensional (2-D) hexagonal symmetry with the space group of p6m [10]. The unit cell parameter (a0) decreases from 15.4 to 13.4 nm upon calcination (Table 1), indicating only a 13.0% framework shrinkage. This phenomenon
Conclusions
Ordered 2-D hexagonal (p6m) mesoporous polymer–organosilica composites have been synthesized by a triconstituent co-assembly strategy. The composites have homogeneous interpenetrating frameworks, in which both polymer and organosilica synergistically support the ordered mesostructure. The presence of phenyl- and ethylene-bridging groups in the framework endows these materials with the adsorption capacity of benzene up to 2.0 mmol g−1, which suggests that they are potential candidates for
Acknowledgments
This work was supported by Discovery Grants from the Australian Research Council (DP0773160 and 0879769).
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