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Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst

Tin oxide-based bimetallic oxide catalysts, MOx (MOx = Al2O3, TiO2, Y2O3) with a molar ratio of MOx:SnO2 of 1:1 was prepared by the solid-state method. X-ray diffraction (XRD) analysis showed that tin oxide, SnO2, was present in all samples as a cassiterite phase with a tetragonal structure. The pr...

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Main Authors: Azami, Ain Arisya, Ramli, Irmawati, Mohamad Rasid, Shera Farisya, Khairul Lail, Muhammad Shamirul, Zakaria, Mohd Rafein, Iqbal, Sarwat
Format: Article
Language:English
Published: Malaysian Analytical Sciences Society 2024
Online Access:http://psasir.upm.edu.my/id/eprint/112007/1/3_Glycerol%20acetylation%20into%20acetins.pdf
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spelling oai:psasir.upm.edu.my:112007 http://psasir.upm.edu.my/id/eprint/112007/ Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst Azami, Ain Arisya Ramli, Irmawati Mohamad Rasid, Shera Farisya Khairul Lail, Muhammad Shamirul Zakaria, Mohd Rafein Iqbal, Sarwat Tin oxide-based bimetallic oxide catalysts, MOx (MOx = Al2O3, TiO2, Y2O3) with a molar ratio of MOx:SnO2 of 1:1 was prepared by the solid-state method. X-ray diffraction (XRD) analysis showed that tin oxide, SnO2, was present in all samples as a cassiterite phase with a tetragonal structure. The presence of other oxides, aluminum oxide (Al2O3), titanium oxide (TiO2), yttrium oxide (Y2O3) in the respective Al2O3/SnO2, TiO2/SnO2, Y2O3/SnO2 were also identified and confirmed by X-ray fluorescence (XRF) analysis. A small exothermic peak at 480 °C and 750 °C in the differential thermal gravimetric (DTG) analysis revealed the oxidation of sub-oxide defects, took place which are very common in SnO2-based samples. Further Fourier transform infrared spectroscopy (FTIR) analysis indicated the presence of Sn-O bonds, reflecting the abundance of tin-oxygen bonds in the materials. Acidity measurements by titration showed that both TiO2/ SnO2 and Y2O3/SnO2 have the same acidity value of 0.23 mmol/g whereas Al2O3/SnO2 and monoxide SnO2 at 0.20 mmol/g. These catalysts were tested for the acetylation of glycerol to monoacetin (MA), diacetin (DA) and triacetin (TA) in a batch reactor at a molar ratio of glycerol: acetic acid of 1:6 w/v, a temperature of 100°C, a reaction time of 2 h and a catalyst loading of 0.5 g. The tests showed complete conversion of glycerol by all catalysts, with the selective product being mainly MA, which was 64%, 62%, 57% and 43% for Al2O3/SnO2, Y2O3/SnO2, SnO2 and TiO2/SnO2, respectively. The percentage selectivity of the more valuable products, DA + TA, was produced in the following order, TiO2/SnO2 > SnO2 > Y2O3/SnO2 > Al2O3/SnO2 with 57%, 43%, 37%, and 35%, respectively. Further analysis of TiO2/SnO2 revealed that the catalyst not only had a high acidity, but also an increased BET surface area of 9.8 m2/g compared to 8.6 m2/g for SnO2 when TiO2 was incorporated into SnO2. Analysis of the surface elements by energy dispersive X-ray spectroscopy (EDX) revealed a high surface oxygen content, which is consistent with the high acidity of the sample. Malaysian Analytical Sciences Society 2024 Article PeerReviewed text en http://psasir.upm.edu.my/id/eprint/112007/1/3_Glycerol%20acetylation%20into%20acetins.pdf Azami, Ain Arisya and Ramli, Irmawati and Mohamad Rasid, Shera Farisya and Khairul Lail, Muhammad Shamirul and Zakaria, Mohd Rafein and Iqbal, Sarwat (2024) Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst. Malaysian Journal of Analytical Sciences, 28 (3). pp. 555-568. ISSN 1394-2506 https://mjas.analis.com.my/mjas/v28_n3/pdf/Azami_28_3_8.pdf
institution UPM IR
collection UPM IR
language English
description Tin oxide-based bimetallic oxide catalysts, MOx (MOx = Al2O3, TiO2, Y2O3) with a molar ratio of MOx:SnO2 of 1:1 was prepared by the solid-state method. X-ray diffraction (XRD) analysis showed that tin oxide, SnO2, was present in all samples as a cassiterite phase with a tetragonal structure. The presence of other oxides, aluminum oxide (Al2O3), titanium oxide (TiO2), yttrium oxide (Y2O3) in the respective Al2O3/SnO2, TiO2/SnO2, Y2O3/SnO2 were also identified and confirmed by X-ray fluorescence (XRF) analysis. A small exothermic peak at 480 °C and 750 °C in the differential thermal gravimetric (DTG) analysis revealed the oxidation of sub-oxide defects, took place which are very common in SnO2-based samples. Further Fourier transform infrared spectroscopy (FTIR) analysis indicated the presence of Sn-O bonds, reflecting the abundance of tin-oxygen bonds in the materials. Acidity measurements by titration showed that both TiO2/ SnO2 and Y2O3/SnO2 have the same acidity value of 0.23 mmol/g whereas Al2O3/SnO2 and monoxide SnO2 at 0.20 mmol/g. These catalysts were tested for the acetylation of glycerol to monoacetin (MA), diacetin (DA) and triacetin (TA) in a batch reactor at a molar ratio of glycerol: acetic acid of 1:6 w/v, a temperature of 100°C, a reaction time of 2 h and a catalyst loading of 0.5 g. The tests showed complete conversion of glycerol by all catalysts, with the selective product being mainly MA, which was 64%, 62%, 57% and 43% for Al2O3/SnO2, Y2O3/SnO2, SnO2 and TiO2/SnO2, respectively. The percentage selectivity of the more valuable products, DA + TA, was produced in the following order, TiO2/SnO2 > SnO2 > Y2O3/SnO2 > Al2O3/SnO2 with 57%, 43%, 37%, and 35%, respectively. Further analysis of TiO2/SnO2 revealed that the catalyst not only had a high acidity, but also an increased BET surface area of 9.8 m2/g compared to 8.6 m2/g for SnO2 when TiO2 was incorporated into SnO2. Analysis of the surface elements by energy dispersive X-ray spectroscopy (EDX) revealed a high surface oxygen content, which is consistent with the high acidity of the sample.
format Article
author Azami, Ain Arisya
Ramli, Irmawati
Mohamad Rasid, Shera Farisya
Khairul Lail, Muhammad Shamirul
Zakaria, Mohd Rafein
Iqbal, Sarwat
spellingShingle Azami, Ain Arisya
Ramli, Irmawati
Mohamad Rasid, Shera Farisya
Khairul Lail, Muhammad Shamirul
Zakaria, Mohd Rafein
Iqbal, Sarwat
Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst
author_facet Azami, Ain Arisya
Ramli, Irmawati
Mohamad Rasid, Shera Farisya
Khairul Lail, Muhammad Shamirul
Zakaria, Mohd Rafein
Iqbal, Sarwat
author_sort Azami, Ain Arisya
title Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst
title_short Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst
title_full Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst
title_fullStr Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst
title_full_unstemmed Glycerol acetylation into acetins over SnO2-based bimetallic oxide catalyst
title_sort glycerol acetylation into acetins over sno2-based bimetallic oxide catalyst
publisher Malaysian Analytical Sciences Society
publishDate 2024
url http://psasir.upm.edu.my/id/eprint/112007/1/3_Glycerol%20acetylation%20into%20acetins.pdf
_version_ 1819302018721775616
score 13.4562235

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