Today, the principles of green chemistry are being fundamentally applied in the chemical industry, such as the nitrobenzene industry, which is an essential intermediate for various commercial products. Research on the application of response surface methodology (RSM) to optimize nitrobenzene synthesis was conducted using a sulfated silica (SO4/SiO2) catalyst and batch microwave reactor. The nitrobenzene synthesis process was carried out according to RSM using a central composite design (CCD) design for three independent variables, consisting of sulfuric acid concentration on the silica (%), stirring time (min), and reaction temperature (°C), and the response variable of nitrobenzene yield (%). The results showed that a three-factorial design using the response surface method could determine the optimum conditions for obtaining nitrobenzene products in a batch microwave reactor. The optimum condition for a nitrobenzene yield of 63.38 % can be obtained at a sulfuric acid concentration on the silica of 91.20 %, stirring time of 140.45 min, and reaction temperature of 58.14 °C. From the 20 experiments conducted, the SO4/SiO2 catalyst showed a selectivity of 100 %, which means that this solid acid catalyst can potentially work well in converting benzene to nitrobenzene.
In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H2SO4/SiO2 as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO2 was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 °C. SiO2 with a 200-mesh size was impregnated with 98 % H2SO4 by mixing for 1 h. The resulting 33 % (w/w) H2SO4/SiO2 catalyst was separated by centrifugation, dried, and calcined at 600 °C. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 °C for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H2SO4/SiO2 could generate an average benzene conversion of 40.33 %.