Herein, we introduce an innovative experimental assembly based on a high-speed disperser and a water recirculator connected to a double-wall stainless steel container as a new and effective pathway for an eco-friendly and controlled synthesis of mesoporous silica particles (MSPs). With the setup, we demonstrated a one-pot encapsulation of the particles with an inhibitor benzotriazole (BTA) to produce a smart nano/microcontainer for potential use in anticorrosive coatings. One advantage of the experimental setup is the high volume of reactant solution that can be used, yet with good control of solution temperature and stirring conditions, which increases the yield and saves laboratory time. The results obtained from the modified Stöber method show the successful preparation of near-spherical and "bean-shaped" nanometer-size (∼310 nm) MSPs with high benzotriazole encapsulation capacity (46 wt %). More so, the one-pot BTA encapsulated mesoporous silica approach revealed monodispersed spherical particles at optimal temperature and stirring conditions with a mean diameter of ∼1.1 μm and a BTA encapsulation of 23 wt %. The synthesized particles show pH responsiveness and can be further optimized and applied as nanocarriers in smart anticorrosive coatings. The experimental assembly adopted in this work represents a new, scalable approach for the synthesis of mesoporous silica particles.