Abstract
TiO2 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 TiO2 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 TiO2 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).
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Ropero-Vega JL, Aldana-Perez A, Gomez R, Nino-Gomez ME (2010) Appl Catal A 379:24
Guvenc A, Kapucu N, Kapucu H, Aydogan O, Mehmetglu U (2007) Enzyme Microb Technol 40:778
Marchetti JM, Errazu AF (2008) Biomass Bioenerg 32:892
Casas A, Ramos MJ, Rodríguez JF, Pérez Á (2013) Fuel Process Technol 106:321
Li KT, Wang CK, Wang I, Wang CM (2011) Appl Catal A 392:180
Koo HM, Lee JH, Chang TS, Suh YW, Lee DH, Bae JW (2014) React Kinet Mech Catal 112:499
Alizadeh MH, Kermani T, Tayebee R (2007) Monatsh Chem 138:165
Hajra B, Pathak AK, Guria C (2014) Int J Ind Chem 5:95
Mitran G, Pavel OD (2015) React Kinet Mech Catal 114:197
Mitran G, Yuzhakova T, Popescu I, Marcu IC (2015) J Mol Catal A 396:275
Zhao H, Jiang P, Dong Y, Huang M, Liu B (2014) React Kinet Mech Catal 113:445
Dai X, Wu C (2013) Adv Mater Res 634:632
Safary E (2011) J Sulfur Chem 32:463
Shi W (2013) Catal Lett 143:732
Hosseini-Sarvari M, Sodagar E (2013) C R Chim 16:229
Sunajadevi KR, Sugunan S (2005) Catal Lett 99:263
Lu Q, Xiong WM, Li WZ, Guo QX, Zhu XF (2009) Bioresour Technol 100:4871
Teo HTR, Saha B (2004) J Catal 228:174
Pizzio L, Vázquez P, Cáceres C, Blanco M (2001) Catal Lett 77:233
Liu CS, Luo GX (2004) China Surfact Det Cosmet 34:403
Azudin NY, Mashitah MD, Abd-Shukor SR (2013) J Food Qual 36:441
Bezerra MA, Santelli RA, Oliveira EP, Villar LS, Escaleira LA (2008) Talanta 76:965
Zhang DH, Bai S, Dong XY, Sun Y (2007) J Agric Food Chem 55:4526
Soo EL, Salleh AB, Basri M, Rahman RNZA, Kamaruddin K (2004) Process Biochem 39:1511
Yan M, Chen F, Zhang J, Anpo M (2005) J Phys Chem B 109:8673
Lin J, Lin Y, Liu P, Meziani MJ, Allard LF, Sun Y (2002) J Am Chem Soc 124:11514
Iwuchukwu IJ, Iwuchukwu E, Le R, Paquet C, Sawhney R, Bruce B, Frymier P (2011) Int J Hydrogen Energy 36:11684
Cam M, Aaby K (2010) J Agric Food Chem 58:9103
Kutner MH, Nachtsheim CJ, Neter J (1996) Applied linear regression models, 4th edn. McGraw-Hill/Irwin, New York
Noda LK, Almeida RMD, Probst LFD, Gonçalves NS (2005) J Mol Catal A 225:39
Hu C, Tang Y, Jiang Z, Hao Z, Tang H, Wong PK (2003) Appl Catal A 253:389
Heravi MJ, Parastar H, Najafabadi HE (2009) J Chromatogr A 1216:6088
Furnis BS, Hannaford AJ, Rogers V, Smith PWG, Tatohal AR (1987) Text book of practical organic chemistry including qualitative organic analysis, 4th edn. Longman, New York
Das R, Sarkar S, Bhattacharjee C (2014) J Water Process Eng 2:79
Nandiwale KY, Galande ND, Bokade VV (2015) RSC Adv 5:17109
Tan KT, Lee KT, Mohamed ARA (2010) Bioresour Technol 101:965
Montgomery DC (2012) Design and analysis of experiments, 8th edn. John Wiley and Sons, New York
Pang XY, Lv P, Yang YS, Ren HL, Gong F (2008) E J Chem 5:149
Nagaraju N, Peeran M, Prasad D (1997) React Kinet Catal Lett 61:155
Yang Z, Zhou C, Zhang W, Li H, Chen M (2010) Colloids Surf A 365:134
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We are grateful for the financial support from the Research Council of Iran University of Science and Technology (IUST), Tehran, Iran. Furthermore, we are thankful to Dr. R. Zare Dorabei for useful discussions concerning RSM.
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Afshar, S., Sadehvand, M., Azad, A. et al. Optimization of catalytic activity of sulfated titania for efficient synthesis of isoamyl acetate by response surface methodology. Monatsh Chem 146, 1949–1957 (2015). https://doi.org/10.1007/s00706-015-1533-5
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DOI: https://doi.org/10.1007/s00706-015-1533-5