Synthesis and characterization of silicotungstic acid nanoparticles via sol gel technique as a catalyst in esterification reaction

Wan Isahak Wan Nor Roslam, Manal Ismail, Norasikin Mohd Nordin, Noraini Hamzah, Khadijeh B. Ghoreishi, Jamaliah Md Jahim, Mohd. Ambar Yarmo

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

4 Citations (Scopus)

Abstract

Glycerol monooleate (GMO) as an esterification product of oleic acid and glycerol is highly potential as an anti-friction substance in the engine lubricant. The purpose of this work is to study the synthesis, characterization and catalytic performance of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The activity and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the homogeneous catalyst i.e. sulphuric acid (H2SO4). The synthesized catalysts were characterized by BET, XRD, TEM, XPS and TPD-NH3. BET analyses shown that the STA-SG catalyst is very high in surface area compared to STAB of 460.11 m2/g and 0.98 m2/g, respectively. From the XPS analyses, there was 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 species 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. 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 H2SO 4 and the STAB gave high conversion of 100% and 98%, while lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94%, while significantly higher GME selectivity of 95% rendering it the more efficient solid acid catalyst.

Original languageEnglish
Title of host publicationAdvanced Materials Research
Pages266-271
Number of pages6
Volume364
DOIs
Publication statusPublished - 2012
Event2011 International Conference on Nanomaterials, Synthesis and Characterization, ICNSC2011 - Selangor
Duration: 4 Jul 20115 Jul 2011

Publication series

NameAdvanced Materials Research
Volume364
ISSN (Print)10226680

Other

Other2011 International Conference on Nanomaterials, Synthesis and Characterization, ICNSC2011
CitySelangor
Period4/7/115/7/11

Fingerprint

Esterification
Sol-gels
Nanoparticles
Catalysts
Acids
Silica
Glycerol
X ray photoelectron spectroscopy
Oleic acid
Temperature programmed desorption
Lubricants
Friction
Engines
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

Synthesis and characterization of silicotungstic acid nanoparticles via sol gel technique as a catalyst in esterification reaction. / Wan Nor Roslam, Wan Isahak; Ismail, Manal; Nordin, Norasikin Mohd; Hamzah, Noraini; Ghoreishi, Khadijeh B.; Md Jahim, Jamaliah; Yarmo, Mohd. Ambar.

Advanced Materials Research. Vol. 364 2012. p. 266-271 (Advanced Materials Research; Vol. 364).

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

Wan Nor Roslam, WI, Ismail, M, Nordin, NM, Hamzah, N, Ghoreishi, KB, Md Jahim, J & Yarmo, MA 2012, Synthesis and characterization of silicotungstic acid nanoparticles via sol gel technique as a catalyst in esterification reaction. in Advanced Materials Research. vol. 364, Advanced Materials Research, vol. 364, pp. 266-271, 2011 International Conference on Nanomaterials, Synthesis and Characterization, ICNSC2011, Selangor, 4/7/11. https://doi.org/10.4028/www.scientific.net/AMR.364.266
Wan Nor Roslam, Wan Isahak ; Ismail, Manal ; Nordin, Norasikin Mohd ; Hamzah, Noraini ; Ghoreishi, Khadijeh B. ; Md Jahim, Jamaliah ; Yarmo, Mohd. Ambar. / Synthesis and characterization of silicotungstic acid nanoparticles via sol gel technique as a catalyst in esterification reaction. Advanced Materials Research. Vol. 364 2012. pp. 266-271 (Advanced Materials Research).
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abstract = "Glycerol monooleate (GMO) as an esterification product of oleic acid and glycerol is highly potential as an anti-friction substance in the engine lubricant. The purpose of this work is to study the synthesis, characterization and catalytic performance of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The activity and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the homogeneous catalyst i.e. sulphuric acid (H2SO4). The synthesized catalysts were characterized by BET, XRD, TEM, XPS and TPD-NH3. BET analyses shown that the STA-SG catalyst is very high in surface area compared to STAB of 460.11 m2/g and 0.98 m2/g, respectively. From the XPS analyses, there was 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 species 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. 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 H2SO 4 and the STAB gave high conversion of 100{\%} and 98{\%}, while lower selectivity of GME with 81.6{\%} and 89.9{\%}, respectively. On the contrary, the STA-SG enabled a conversion of 94{\%}, while 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 - Hamzah, Noraini

AU - Ghoreishi, Khadijeh B.

AU - Md Jahim, Jamaliah

AU - Yarmo, Mohd. Ambar

PY - 2012

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N2 - Glycerol monooleate (GMO) as an esterification product of oleic acid and glycerol is highly potential as an anti-friction substance in the engine lubricant. The purpose of this work is to study the synthesis, characterization and catalytic performance of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The activity and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the homogeneous catalyst i.e. sulphuric acid (H2SO4). The synthesized catalysts were characterized by BET, XRD, TEM, XPS and TPD-NH3. BET analyses shown that the STA-SG catalyst is very high in surface area compared to STAB of 460.11 m2/g and 0.98 m2/g, respectively. From the XPS analyses, there was 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 species 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. 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 H2SO 4 and the STAB gave high conversion of 100% and 98%, while lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94%, while significantly higher GME selectivity of 95% rendering it the more efficient solid acid catalyst.

AB - Glycerol monooleate (GMO) as an esterification product of oleic acid and glycerol is highly potential as an anti-friction substance in the engine lubricant. The purpose of this work is to study the synthesis, characterization and catalytic performance of solid heteropoly acid catalysts, namely silicotungstic acid bulk (STAB) and STA-silica sol gel (STA-SG). The activity and selectivity of STAB and STA-SG in the esterification reaction have been investigated and compared to the homogeneous catalyst i.e. sulphuric acid (H2SO4). The synthesized catalysts were characterized by BET, XRD, TEM, XPS and TPD-NH3. BET analyses shown that the STA-SG catalyst is very high in surface area compared to STAB of 460.11 m2/g and 0.98 m2/g, respectively. From the XPS analyses, there was 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 species 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. 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 H2SO 4 and the STAB gave high conversion of 100% and 98%, while lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94%, while 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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