Issue 5, 2015

Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica

Abstract

Hexagonal mesostructured templated silicas were produced in less than 10 minutes using an ultra-fast microwave assisted hydrothermal synthesis. Typically, 10 g can be prepared at once in a commercial microwave device usually devoted to analytical digestion. Undesired alcohol side-products were avoided using inexpensive water colloidal silica instead of silicon alkoxides as the silicon source. In comparison with classical heating activation, the absence of pore expansion and pore wall thickening even for synthesis temperatures as high as 190 °C evidenced that heat transfer and diffusion of matter had no time to take place. Comparison between the chemically extracted and calcined samples shows that the structure was better stabilized for autoclaving above 150 °C. However, a fast temperature ramping and final temperatures above 180 °C were required to sear structures of the highest quality comparable to that of the best conventional methods. This is rationalized by assuming a sequential flake-by-flake assembly of the pore-wall at the micelle palisade. Notably, tosylate counterions yielded better structural characteristics than bromide counterions and allowed better opportunities for surfactant recycling.

Graphical abstract: Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica

Supplementary files

Article information

Article type
Paper
Submitted
07 Jan 2015
Accepted
01 Apr 2015
First published
07 Apr 2015

Green Chem., 2015,17, 3130-3140

Author version available

Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica

J. Chaignon, Y. Bouizi, L. Davin, N. Calin, B. Albela and L. Bonneviot, Green Chem., 2015, 17, 3130 DOI: 10.1039/C5GC00038F

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