Selective synthesis of glycerol monoester with heteropoly acid as a new catalyst

Research output: Chapter in Book/Report/Conference proceedingConference contribution

3 Citations (Scopus)

Abstract

In this work, we were study the selective synthesis of GME from oleic acid and glycerol using two types of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The performance and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the sulphuric acid (H 2SO 4) as conventional homogeneous catalyst. The catalysts were then characterized their physical and chemical properties using BET, XRD, TEM and XPS. XPS analyses were shown a significant formation of W-O-Si, W-O-W and Si-O-Si bonding in STA-SG compared to that in STAB. The main spectra of O1s (90.74 %, 531.5 eV) followed by other O1s peak (9.26 %, 532.8 eV) were due to the presence of W-O-W and W-O-Si bonds, respectively. The STA-SG catalyst was found to be the more environmentally benign solid acid catalyst for the esterification reaction between oleic acid and glycerol due to its lower toxicity in terms of the relatively lower pH value (pH 3.7) than the STAB (pH 2.8). In addition, the ease of separation for STA-SG catalyst was attributed to its insoluble state in the product phase. The esterification products were then analysed by FTIR and HPLC. Both the H 2SO 4 and the STAB gave high conversion of 100% and 98%, but at a lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94%, but with a significantly higher GME selectivity of 95% rendering it the more efficient solid acid catalyst.

Original languageEnglish
Title of host publicationAdvanced Materials Research
Pages373-378
Number of pages6
Volume545
DOIs
Publication statusPublished - 2012
Event2nd International Conference on the Advancement of Materials and Nanotechnology, ICAMN II 2010 - Kuala Lumpur
Duration: 29 Nov 20101 Dec 2010

Publication series

NameAdvanced Materials Research
Volume545
ISSN (Print)10226680

Other

Other2nd International Conference on the Advancement of Materials and Nanotechnology, ICAMN II 2010
CityKuala Lumpur
Period29/11/101/12/10

Fingerprint

Glycerol
Catalysts
Sol-gels
Acids
Silica
Esterification
Oleic acid
X ray photoelectron spectroscopy
Chemical properties
Toxicity
Physical properties
Transmission electron microscopy

Keywords

  • Oleic acid
  • Silicotungstic acid bulk
  • Solid acid catalyst
  • STA-silica sol gel
  • XPS

ASJC Scopus subject areas

  • Engineering(all)

Cite this

Selective synthesis of glycerol monoester with heteropoly acid as a new catalyst. / Wan Nor Roslam, Wan Isahak; Ismail, Manal; Nordin, Norasikin Mohd; Adnan, Nadia Farhana; Md Jahim, Jamaliah; Salimon, Jumat; Yarmo, Mohd. Ambar.

Advanced Materials Research. Vol. 545 2012. p. 373-378 (Advanced Materials Research; Vol. 545).

Research output: Chapter in Book/Report/Conference proceedingConference contribution

Wan Nor Roslam, WI, Ismail, M, Nordin, NM, Adnan, NF, Md Jahim, J, Salimon, J & Yarmo, MA 2012, Selective synthesis of glycerol monoester with heteropoly acid as a new catalyst. in Advanced Materials Research. vol. 545, Advanced Materials Research, vol. 545, pp. 373-378, 2nd International Conference on the Advancement of Materials and Nanotechnology, ICAMN II 2010, Kuala Lumpur, 29/11/10. https://doi.org/10.4028/www.scientific.net/AMR.545.373
Wan Nor Roslam, Wan Isahak ; Ismail, Manal ; Nordin, Norasikin Mohd ; Adnan, Nadia Farhana ; Md Jahim, Jamaliah ; Salimon, Jumat ; Yarmo, Mohd. Ambar. / Selective synthesis of glycerol monoester with heteropoly acid as a new catalyst. Advanced Materials Research. Vol. 545 2012. pp. 373-378 (Advanced Materials Research).
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abstract = "In this work, we were study the selective synthesis of GME from oleic acid and glycerol using two types of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The performance and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the sulphuric acid (H 2SO 4) as conventional homogeneous catalyst. The catalysts were then characterized their physical and chemical properties using BET, XRD, TEM and XPS. XPS analyses were shown a significant formation of W-O-Si, W-O-W and Si-O-Si bonding in STA-SG compared to that in STAB. The main spectra of O1s (90.74 {\%}, 531.5 eV) followed by other O1s peak (9.26 {\%}, 532.8 eV) were due to the presence of W-O-W and W-O-Si bonds, respectively. The STA-SG catalyst was found to be the more environmentally benign solid acid catalyst for the esterification reaction between oleic acid and glycerol due to its lower toxicity in terms of the relatively lower pH value (pH 3.7) than the STAB (pH 2.8). In addition, the ease of separation for STA-SG catalyst was attributed to its insoluble state in the product phase. The esterification products were then analysed by FTIR and HPLC. Both the H 2SO 4 and the STAB gave high conversion of 100{\%} and 98{\%}, but at a lower selectivity of GME with 81.6{\%} and 89.9{\%}, respectively. On the contrary, the STA-SG enabled a conversion of 94{\%}, but with a significantly higher GME selectivity of 95{\%} rendering it the more efficient solid acid catalyst.",
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AU - Wan Nor Roslam, Wan Isahak

AU - Ismail, Manal

AU - Nordin, Norasikin Mohd

AU - Adnan, Nadia Farhana

AU - Md Jahim, Jamaliah

AU - Salimon, Jumat

AU - Yarmo, Mohd. Ambar

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N2 - In this work, we were study the selective synthesis of GME from oleic acid and glycerol using two types of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The performance and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the sulphuric acid (H 2SO 4) as conventional homogeneous catalyst. The catalysts were then characterized their physical and chemical properties using BET, XRD, TEM and XPS. XPS analyses were shown a significant formation of W-O-Si, W-O-W and Si-O-Si bonding in STA-SG compared to that in STAB. The main spectra of O1s (90.74 %, 531.5 eV) followed by other O1s peak (9.26 %, 532.8 eV) were due to the presence of W-O-W and W-O-Si bonds, respectively. The STA-SG catalyst was found to be the more environmentally benign solid acid catalyst for the esterification reaction between oleic acid and glycerol due to its lower toxicity in terms of the relatively lower pH value (pH 3.7) than the STAB (pH 2.8). In addition, the ease of separation for STA-SG catalyst was attributed to its insoluble state in the product phase. The esterification products were then analysed by FTIR and HPLC. Both the H 2SO 4 and the STAB gave high conversion of 100% and 98%, but at a lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94%, but with a significantly higher GME selectivity of 95% rendering it the more efficient solid acid catalyst.

AB - In this work, we were study the selective synthesis of GME from oleic acid and glycerol using two types of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The performance and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the sulphuric acid (H 2SO 4) as conventional homogeneous catalyst. The catalysts were then characterized their physical and chemical properties using BET, XRD, TEM and XPS. XPS analyses were shown a significant formation of W-O-Si, W-O-W and Si-O-Si bonding in STA-SG compared to that in STAB. The main spectra of O1s (90.74 %, 531.5 eV) followed by other O1s peak (9.26 %, 532.8 eV) were due to the presence of W-O-W and W-O-Si bonds, respectively. The STA-SG catalyst was found to be the more environmentally benign solid acid catalyst for the esterification reaction between oleic acid and glycerol due to its lower toxicity in terms of the relatively lower pH value (pH 3.7) than the STAB (pH 2.8). In addition, the ease of separation for STA-SG catalyst was attributed to its insoluble state in the product phase. The esterification products were then analysed by FTIR and HPLC. Both the H 2SO 4 and the STAB gave high conversion of 100% and 98%, but at a lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94%, but with a significantly higher GME selectivity of 95% rendering it the more efficient solid acid catalyst.

KW - Oleic acid

KW - Silicotungstic acid bulk

KW - Solid acid catalyst

KW - STA-silica sol gel

KW - XPS

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