Morphology control of microporous silica particles obtained by gradual injection of reactants

Abstract

Industrial-scale synthesis of fine-tuned monodisperse microporous silica is a central concern on fillers and optical applications. We recently reported that the efficient synthesis of monodisperse microporous silica particles can be achieved by the gradual injection of reactants. In the present study, we investigated the influence of the injection kinetics, the template, and catalyst contents on the morphology of the resulting silica particles. Their specific surface area (SSA) could be tuned from 100 to 500 m 2 /g by the amount of templating molecule, ndodecylamine, without changing the particle size and dispersibility. The most important parameters for controlling the particle size were found to be the amounts of catalyst. The resultant microporous and monodisperse silica particles exhibit diameter ranging from 20 to 200 nm and SSA from 50 to 1000 m 2 /g. These results show that the gradual injection of the reactants in a controlled manner is effective to the industrial-scale synthesis of the silica nanoparticles with expected morphologies. Graphical Abstract

Large-scale preparation of morphology-controlled microporous silica particles via gradual injection of reactants with different surfactants

“…We have reported previously that the aggregation of particles is more frequent with higher concentrations of DDA [34]. Samples 12 and 13 were prepared to obtain monodispersed and microporous silica particles with higher SSA using DA as a template molecule, which exhibits a better solubility in reaction solution than DDA.…”

“…The obtained silica particles show a narrow distribution of particulate diameter. Using dodecylamine (DDA) as a template molecule, the monodisperse, microporous silica particles with diameters ranging from 20 to 200 nm and specific surface area (SSA) from 50 to 1000 m 2 /g can be obtained by adjusting the synthetic parameters [34].…”

Single-process fabrication of antireflective acrylic hard coating via surface segregation of porous silica nanoparticles

“…29,30 Methanol (852.8 g), distilled water (245.2 g), and 28% NH 3 (109.6 g) were mixed in a 2-L four-neck ask at 20 C. Methanol (180.4 g), DA (127.6 g), and TMOS (137.2 g) were mixed in a PE container and were then injected into the rst ask with a tube pump for 120 min under vigorous stirring. Mesoporous silica particles were prepared using a previously reported procedure.…”

“…29,30 Commercial hollow silica particles 50 to 60 nm in diameter (Nano Balloon XL100) were used for a comparison. 29,30 Commercial hollow silica particles 50 to 60 nm in diameter (Nano Balloon XL100) were used for a comparison.…”

“…Mesoporous silica particles were prepared using a previously reported procedure. 29,30 Methanol (852.8 g), distilled water (245.2 g), and 28% NH 3 (109.6 g) were mixed in a 2-L four-neck ask at 20 C. Methanol (180.4 g), DA (127.6 g), and TMOS (137.2 g) were mixed in a PE container and were then injected into the rst ask with a tube pump for 120 min under vigorous stirring. The molar ratio of the reaction solution was TMOS/DA/NH 3 /H 2 O ¼ 0.5/0.4/1/10.…”