Synthesis of Silica Nanoparticles for the Manufacture of Porous Carbon Membrane and Particle Size Analysis by Sedimentation Field‐Flow Fractionation

Abstract

Silica nanoparticles were synthesized by emulsion polymerization by mixing ethanol, ammonium hydroxide, water, and tetraethyl orthosilicate. An apparatus was designed and assembled for a large‐scale synthesis of silica nanospheres, which was aimed for uniform mixing of the reactants. Then sedimentation field‐flow fractionation (SdFFF) was used to determin the size distribution of the silica nanoparticles. SdFFF provided mass‐based separation where the retention time increased with the particle size, thus the size distribution of silica nanoparticles obtained from SdFFF appeared more accurate than that from dynamic light scattering, particularly for those having broad and multimodal size distributions. A disk‐shaped porous carbon membrane (PCM) was manufactured for application as an adsorbent by pressurizing the silica particles, followed by calcination. Results showed that PCM manufactured in this study has relatively high surface area and temperature stability. The PCM surface was modified by attaching a carboxyl group (PCM‐COOH) and then by incorporating silver (PCM‐COOH‐Ag). The amount of COOH group on PCM was measured electrochemically by cyclic voltammetry, and the surface area, pore size, pore volume of PCM‐COOH‐Ag by Brunauer–Emmet–Teller measurement. The surface area was 40.65 and reduced to 13.02 after loading a COOH group then increased up to 30.37 after incorporating Ag.