Optimization of catalytic activity of sulfated titania for efficient synthesis of isoamyl acetate by response surface methodology

Abstract

TiO 2 nanoparticles were synthesized by sol-gel method using titanium tetraisopropoxide. Sulfate ions were introduced on the titania by impregnation method using sulfuric acid as precursor of sulfate ions. Fourier transform infrared and energy-dispersive X-ray spectroscopy, X-ray fluorescence as well as X-ray diffraction, scanning electron microscopy, and BET methods were used for the characterization of the obtained nanoparticles. The esterification of isoamyl alcohol with acetic acid was investigated to prove the catalytic activity of the TiO 2 nanoparticles under solvent-free conditions. Response surface methodology was applied to optimize the effect of some parameters such as the molar ratio of acetic acid to alcohol, catalyst loading, reaction temperature, and reaction time on the yield of the isoamyl acetate. The TiO 2 nanoparticles were proved to be an excellent heterogeneous catalyst for isoamyl acetate synthesis under solvent-free conditions affording a high yield of 94 % under the following optimal conditions: molar ratio of acetic acid to alcohol (1:7), catalyst loading (3.2 wt% with respect to the acetic acid), the reaction temperature (130°C), and the reaction time (300 min). Graphical abstract

Optimization of green and environmentally-benign synthesis of isoamyl acetate in the presence of ball-milled seashells by response surface methodology

“…9) illustrate the in uence of interaction between the reaction temperature (A) and molar ratio of acid: alcohol (D) on values of time (B) and catalyst loading (C) were set to 165 min and 25.5 mg, respectively. These results clearly show that at temperature of 56.5 °C, enhancing the molar ratio of reactants had no notable effect on the yield of isoamyl acetate (4) whereas at 98 °C lower yields were obtained when high molar ratio of reactants are used 11,54 . Moreover, (Fig.…”

“…The p values from Table 1 were used to check the signi cance of each of the factors and interaction between the factors. The value of prob F less then 0.05 for a variable implies that its effect is signi cant at the 95% of con dence interval 11,48,49 . Values greater than 0.1 display that the variable is not signi cant.…”

Sulfated Titania (TiO2‐SO42−) as an Efficient Catalyst for Organic Synthesis: Overarching Review from 2000 to 2021

“…Dekamin et al [74] have investigated the esterification of isoamyl alcohol with acetic acid in the existence of TiO 2 -SO 4 2À as a catalyst to afford isoamyl acetate using response surface Scheme 17. Microwave irradiated organic transformation using TiO 2 -P25-SO 4…”

“…Jin et al [75] developed acetalization of various aldehydes and cyclic ketones with triethylorthoformate in presence of TiO 2À . [74] Scheme 21. Acetalization of carbonyl compounds using TiO 2 -SO 4 2À catalyst.…”

Processo enzimático para produção de acetato de isoamila livre de solvente orgânico

“…Economizando consequentemente energia e evitando a toxicidade indesejável da reação. Esses resultados enfatizam a relevância de nosso estudo, pois foram obtidas conversões mais altas no sistema livre de solventes orgânicos (AFSHAR et al, 2015;KHAN E RATHOD, 2015;DOS SANTOS et al, 2017).…”