Mechanochemical synthesis of CaO·ZnO.K2CO3 catalyst: Characterization and activity for methanolysis of sunflower oil
Mehanohemijska sinteza CaO·ZnO.K2CO3, katalizatora - karakterizacija i aktivnost u metanolizi suncokretovog ulja
Abstract
The goal of this study was to prepare a CaO·ZnO catalyst containing a small amount of K2CO3 and analyze its activity for biodiesel synthesis. The catalyst was prepared using the following procedure: CaO and ZnO (mole ratio of 1:2), water and K2CO3 (in various amounts) were mechanochemically treated and after milling heated at 700°C in air atmosphere for obtaining mixed CaO·ZnO/xK2CO3 oxides (x = 0, 1, 2 and 4 mol of K2CO3 per 10 mol of CaO). All the samples were characterized by X-ray diffraction (XRD), inductively coupled plasma (ICP), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), infrared spectroscopy (FTIR), scanning electron microscopy/ energy-dispersive spectroscopy (SEM/EDS), particle size laser diffraction (PSLD) distribution, solubility measurement of Ca, Zn and K ions in methanol as well as by determination of their alkalinity (Hammett indicator method). Prepared CaO·ZnO/xK2CO3 composite powders were tested as catalysts for methanolysis of sunflower... oil at 70 °C using mole ratio of sunflower oil to methanol of 1:10 and with 2 mass% of catalyst based on oil weight. The presence of K2CO3 in prepared samples was found to increase the activity of catalyst, and that such effect is caused by homogeneous-heterogeneous catalysis of biodiesel synthesis.
Cilj ovih istraživanja bio je da se pripremi CaO·ZnO katalizator koji sadrži malu količinu K2CO3 i analizira njegova aktivnost u sintezi biodizela. Katalizator je pripremljen prema sledećoj proceduri: CaO i ZnO (molski odnos 1:2), voda i K2CO3 (u različitoj količini) su tretirani mehanohemijski i nakon mlevenja zagrevani na 700 °C u atmosferi vazduha da bi se dobila smeša oksida CaO·ZnO/xK2CO3 (x = 0, 1, 2 i 4 mol K2CO3 na 10 mol CaO). Karakterizacija pripremljenih katalizatora izvršena je metodama rendgenske difrakcije (XRD), indukovane kuplovane plazme (ICP), spektroskopije fotoelektrona dobijenih X-zracima (XPS), termogravimetrijske analize (TGA), infracrvene spektroskopije (FTIR), skenirajuće elektronske mikroskopije i energetske disperzione spektroskopije (SEM/EDS), raspodele veličine čestica (PSLD), merenjem rastvorljivosti katalizatora odnosno Ca, Zn i K jona u metanolu, kao i određivanjem njihove baznosti (metodom Hametovih indikatora). Pripremljeni CaO·ZnO/xK2CO3 kompozitni pr...ahovi testirani su kao katalizatori u reakciji metanolize suncokretovog ulja na 70 °C, pri molarnom odnosu suncokretovog ulja i metanola od 1:10 i sa 2 mas.% katalizatora u odnosu na masu ulja. Pokazano je da prisustvo K2CO3 u pripremljenim uzorcima povećava aktivnost katalizatora i da je takav efekat posledica homogeno-heterogene katalize u sintezi biodizela.
Keywords:
mechanochemical synthesis / CaO / ZnO / K2CO3 / mixed oxides / biodiesel synthesis / mehanohemijska sinteza / CaO / ZnO / K2CO3 / mešani oksidi / sinteza biodizelaSource:
Chemical Industry & Chemical Engineering Quarterly, 2015, 21, 1-1, 1-12Publisher:
- Association of the Chemical Engineers of Serbia
Funding / projects:
- Nanostructured Functional and Composite Materials in Catalytic and Sorption Processes (RS-MESTD-Integrated and Interdisciplinary Research (IIR or III)-45001)
DOI: 10.2298/CICEQ131026041K
ISSN: 1451-9372
WoS: 000354755400001
Scopus: 2-s2.0-84946185788
Institution/Community
Tehnološko-metalurški fakultetTY - JOUR AU - Kesić, Željka AU - Lukić, Ivana AU - Zdujić, Miodrag AU - Jovalekić, Čedomir AU - Liu, Hui AU - Skala, Dejan PY - 2015 UR - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/2921 AB - The goal of this study was to prepare a CaO·ZnO catalyst containing a small amount of K2CO3 and analyze its activity for biodiesel synthesis. The catalyst was prepared using the following procedure: CaO and ZnO (mole ratio of 1:2), water and K2CO3 (in various amounts) were mechanochemically treated and after milling heated at 700°C in air atmosphere for obtaining mixed CaO·ZnO/xK2CO3 oxides (x = 0, 1, 2 and 4 mol of K2CO3 per 10 mol of CaO). All the samples were characterized by X-ray diffraction (XRD), inductively coupled plasma (ICP), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), infrared spectroscopy (FTIR), scanning electron microscopy/ energy-dispersive spectroscopy (SEM/EDS), particle size laser diffraction (PSLD) distribution, solubility measurement of Ca, Zn and K ions in methanol as well as by determination of their alkalinity (Hammett indicator method). Prepared CaO·ZnO/xK2CO3 composite powders were tested as catalysts for methanolysis of sunflower oil at 70 °C using mole ratio of sunflower oil to methanol of 1:10 and with 2 mass% of catalyst based on oil weight. The presence of K2CO3 in prepared samples was found to increase the activity of catalyst, and that such effect is caused by homogeneous-heterogeneous catalysis of biodiesel synthesis. AB - Cilj ovih istraživanja bio je da se pripremi CaO·ZnO katalizator koji sadrži malu količinu K2CO3 i analizira njegova aktivnost u sintezi biodizela. Katalizator je pripremljen prema sledećoj proceduri: CaO i ZnO (molski odnos 1:2), voda i K2CO3 (u različitoj količini) su tretirani mehanohemijski i nakon mlevenja zagrevani na 700 °C u atmosferi vazduha da bi se dobila smeša oksida CaO·ZnO/xK2CO3 (x = 0, 1, 2 i 4 mol K2CO3 na 10 mol CaO). Karakterizacija pripremljenih katalizatora izvršena je metodama rendgenske difrakcije (XRD), indukovane kuplovane plazme (ICP), spektroskopije fotoelektrona dobijenih X-zracima (XPS), termogravimetrijske analize (TGA), infracrvene spektroskopije (FTIR), skenirajuće elektronske mikroskopije i energetske disperzione spektroskopije (SEM/EDS), raspodele veličine čestica (PSLD), merenjem rastvorljivosti katalizatora odnosno Ca, Zn i K jona u metanolu, kao i određivanjem njihove baznosti (metodom Hametovih indikatora). Pripremljeni CaO·ZnO/xK2CO3 kompozitni prahovi testirani su kao katalizatori u reakciji metanolize suncokretovog ulja na 70 °C, pri molarnom odnosu suncokretovog ulja i metanola od 1:10 i sa 2 mas.% katalizatora u odnosu na masu ulja. Pokazano je da prisustvo K2CO3 u pripremljenim uzorcima povećava aktivnost katalizatora i da je takav efekat posledica homogeno-heterogene katalize u sintezi biodizela. PB - Association of the Chemical Engineers of Serbia T2 - Chemical Industry & Chemical Engineering Quarterly T1 - Mechanochemical synthesis of CaO·ZnO.K2CO3 catalyst: Characterization and activity for methanolysis of sunflower oil T1 - Mehanohemijska sinteza CaO·ZnO.K2CO3, katalizatora - karakterizacija i aktivnost u metanolizi suncokretovog ulja EP - 12 IS - 1-1 SP - 1 VL - 21 DO - 10.2298/CICEQ131026041K ER -
@article{ author = "Kesić, Željka and Lukić, Ivana and Zdujić, Miodrag and Jovalekić, Čedomir and Liu, Hui and Skala, Dejan", year = "2015", abstract = "The goal of this study was to prepare a CaO·ZnO catalyst containing a small amount of K2CO3 and analyze its activity for biodiesel synthesis. The catalyst was prepared using the following procedure: CaO and ZnO (mole ratio of 1:2), water and K2CO3 (in various amounts) were mechanochemically treated and after milling heated at 700°C in air atmosphere for obtaining mixed CaO·ZnO/xK2CO3 oxides (x = 0, 1, 2 and 4 mol of K2CO3 per 10 mol of CaO). All the samples were characterized by X-ray diffraction (XRD), inductively coupled plasma (ICP), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), infrared spectroscopy (FTIR), scanning electron microscopy/ energy-dispersive spectroscopy (SEM/EDS), particle size laser diffraction (PSLD) distribution, solubility measurement of Ca, Zn and K ions in methanol as well as by determination of their alkalinity (Hammett indicator method). Prepared CaO·ZnO/xK2CO3 composite powders were tested as catalysts for methanolysis of sunflower oil at 70 °C using mole ratio of sunflower oil to methanol of 1:10 and with 2 mass% of catalyst based on oil weight. The presence of K2CO3 in prepared samples was found to increase the activity of catalyst, and that such effect is caused by homogeneous-heterogeneous catalysis of biodiesel synthesis., Cilj ovih istraživanja bio je da se pripremi CaO·ZnO katalizator koji sadrži malu količinu K2CO3 i analizira njegova aktivnost u sintezi biodizela. Katalizator je pripremljen prema sledećoj proceduri: CaO i ZnO (molski odnos 1:2), voda i K2CO3 (u različitoj količini) su tretirani mehanohemijski i nakon mlevenja zagrevani na 700 °C u atmosferi vazduha da bi se dobila smeša oksida CaO·ZnO/xK2CO3 (x = 0, 1, 2 i 4 mol K2CO3 na 10 mol CaO). Karakterizacija pripremljenih katalizatora izvršena je metodama rendgenske difrakcije (XRD), indukovane kuplovane plazme (ICP), spektroskopije fotoelektrona dobijenih X-zracima (XPS), termogravimetrijske analize (TGA), infracrvene spektroskopije (FTIR), skenirajuće elektronske mikroskopije i energetske disperzione spektroskopije (SEM/EDS), raspodele veličine čestica (PSLD), merenjem rastvorljivosti katalizatora odnosno Ca, Zn i K jona u metanolu, kao i određivanjem njihove baznosti (metodom Hametovih indikatora). Pripremljeni CaO·ZnO/xK2CO3 kompozitni prahovi testirani su kao katalizatori u reakciji metanolize suncokretovog ulja na 70 °C, pri molarnom odnosu suncokretovog ulja i metanola od 1:10 i sa 2 mas.% katalizatora u odnosu na masu ulja. Pokazano je da prisustvo K2CO3 u pripremljenim uzorcima povećava aktivnost katalizatora i da je takav efekat posledica homogeno-heterogene katalize u sintezi biodizela.", publisher = "Association of the Chemical Engineers of Serbia", journal = "Chemical Industry & Chemical Engineering Quarterly", title = "Mechanochemical synthesis of CaO·ZnO.K2CO3 catalyst: Characterization and activity for methanolysis of sunflower oil, Mehanohemijska sinteza CaO·ZnO.K2CO3, katalizatora - karakterizacija i aktivnost u metanolizi suncokretovog ulja", pages = "12-1", number = "1-1", volume = "21", doi = "10.2298/CICEQ131026041K" }
Kesić, Ž., Lukić, I., Zdujić, M., Jovalekić, Č., Liu, H.,& Skala, D.. (2015). Mechanochemical synthesis of CaO·ZnO.K2CO3 catalyst: Characterization and activity for methanolysis of sunflower oil. in Chemical Industry & Chemical Engineering Quarterly Association of the Chemical Engineers of Serbia., 21(1-1), 1-12. https://doi.org/10.2298/CICEQ131026041K
Kesić Ž, Lukić I, Zdujić M, Jovalekić Č, Liu H, Skala D. Mechanochemical synthesis of CaO·ZnO.K2CO3 catalyst: Characterization and activity for methanolysis of sunflower oil. in Chemical Industry & Chemical Engineering Quarterly. 2015;21(1-1):1-12. doi:10.2298/CICEQ131026041K .
Kesić, Željka, Lukić, Ivana, Zdujić, Miodrag, Jovalekić, Čedomir, Liu, Hui, Skala, Dejan, "Mechanochemical synthesis of CaO·ZnO.K2CO3 catalyst: Characterization and activity for methanolysis of sunflower oil" in Chemical Industry & Chemical Engineering Quarterly, 21, no. 1-1 (2015):1-12, https://doi.org/10.2298/CICEQ131026041K . .