Effect and mechanism of ultrasound on acid loading in the preparation of silicon-based sulfonic solid acids

Silicon-based sulfonic solid acids have the advantages of high catalytic activity and selectivity, easy separation from products, low equipment corrosion, and environmental protection, and sulfuric acid loading is the key to their preparation. To overcome the shortcomings of low acid loading and uneven distribution in the existing preparation methods of micron-sized silicon-based sulfonic solid acids, a method was proposed to prepare micron-sized silicon-based sulfonic solid acids using ultrasonic enhanced technology. The effect of different reaction parameters, such as time, power, and temperature of ultrasonication, sulfonation temperature and time, and sulfuric acid concentration, on acid loading in solid acid was investigated in this work. The results showed that a micron-sized mesoporous silica-based solid acid was successfully synthesized with a high acid content of 0.8633 mmol/g, uniform acid distribution, high specific surface area of 269.332 m2/g, and large average particle size of 172.142 μm in this work. The introduction of ultrasound was found to expand the carrier's pore volume and increase the carrier's specific surface area and the number of hydroxyl groups, thereby increasing the acid loading capacity and the specific surface area of the solid acid sample by 66.6 % and 10.97 % respectively, compared with the case without ultrasound.