Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel
The by-product of the previous transesterification, glycerol was utilised as an acid catalyst precursor for biodiesel production. The crude glycerol was treated through the sulfonation method with sulfuric acid and chlorosulfonic acid in a reflux batch reactor giving solid glycerol-SO<sub>3<...
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| Format: | Article |
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MDPI AG
2022-10-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/27/20/7142 |
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| author | Balkis Hazmi Mahnoush Beygisangchin Umer Rashid Wan Nur Aini Wan Mokhtar Toshiki Tsubota Ali Alsalme Chawalit Ngamcharussrivichai |
| author_facet | Balkis Hazmi Mahnoush Beygisangchin Umer Rashid Wan Nur Aini Wan Mokhtar Toshiki Tsubota Ali Alsalme Chawalit Ngamcharussrivichai |
| author_sort | Balkis Hazmi |
| collection | DOAJ |
| description | The by-product of the previous transesterification, glycerol was utilised as an acid catalyst precursor for biodiesel production. The crude glycerol was treated through the sulfonation method with sulfuric acid and chlorosulfonic acid in a reflux batch reactor giving solid glycerol-SO<sub>3</sub>H and glycerol-ClSO<sub>3</sub>H, respectively. The synthesised acidic glycerol catalysts were characterised by various analytical techniques such as thermalgravimetric analyser (TGA), infrared spectroscopy, surface properties adsorption-desorption by nitrogen gas, ammonia-temperature programmed desorption (NH<sub>3</sub>-TPD), X-ray diffraction spectroscopy (XRD), elemental composition analysis by energy dispersive spectrometer (EDX) and surface micrographic morphologies by field emission electron microscope (FESEM). Both glycerol-SO<sub>3</sub>H and glycerol-ClSO<sub>3</sub>H samples exhibited mesoporous structures with a low surface area of 8.85 mm<sup>2</sup>/g and 4.71 mm<sup>2</sup>/g, respectively, supported by the microscopic image of blockage pores. However, the acidity strength for both catalysts was recorded at 3.43 mmol/g and 3.96 mmol/g, which is sufficient for catalysing PFAD biodiesel at the highest yield. The catalytic esterification was optimised at 96.7% and 98.2% with 3 wt.% of catalyst loading, 18:1 of methanol-PFAD molar ratio, 120 °C, and 4 h of reaction. Catalyst reusability was sustained up to 3 reaction cycles due to catalyst deactivation, and the insight investigation of spent catalysts was also performed. |
| first_indexed | 2024-03-09T19:41:34Z |
| format | Article |
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| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-09T19:41:34Z |
| publishDate | 2022-10-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-91682842b4f44537906262eb6212e6732023-11-24T01:38:16ZengMDPI AGMolecules1420-30492022-10-012720714210.3390/molecules27207142Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to BiodieselBalkis Hazmi0Mahnoush Beygisangchin1Umer Rashid2Wan Nur Aini Wan Mokhtar3Toshiki Tsubota4Ali Alsalme5Chawalit Ngamcharussrivichai6Institute of Nanoscience and Nanotechnology, Universiti Putra Malaysia, Serdang 43400, Selangor, MalaysiaInstitute of Nanoscience and Nanotechnology, Universiti Putra Malaysia, Serdang 43400, Selangor, MalaysiaInstitute of Nanoscience and Nanotechnology, Universiti Putra Malaysia, Serdang 43400, Selangor, MalaysiaDepartment of Chemical Sciences, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, Bangi 43600, Selangor, MalaysiaDepartment of Materials Science, Graduate School of Engineering, Kyushu Institute of Technology, 1-1 Sensuicho, Tobata-ku, Kitakyushu, Fukuoka 804-8550, JapanChemistry Department, College of Science, King Saud University, Riyadh 1145, Saudi ArabiaCenter of Excellence in Catalysis for Bioenergy and Renewable Chemicals (CBRC), Faculty of Science, Chulalongkorn University, Bangkok 10330, ThailandThe by-product of the previous transesterification, glycerol was utilised as an acid catalyst precursor for biodiesel production. The crude glycerol was treated through the sulfonation method with sulfuric acid and chlorosulfonic acid in a reflux batch reactor giving solid glycerol-SO<sub>3</sub>H and glycerol-ClSO<sub>3</sub>H, respectively. The synthesised acidic glycerol catalysts were characterised by various analytical techniques such as thermalgravimetric analyser (TGA), infrared spectroscopy, surface properties adsorption-desorption by nitrogen gas, ammonia-temperature programmed desorption (NH<sub>3</sub>-TPD), X-ray diffraction spectroscopy (XRD), elemental composition analysis by energy dispersive spectrometer (EDX) and surface micrographic morphologies by field emission electron microscope (FESEM). Both glycerol-SO<sub>3</sub>H and glycerol-ClSO<sub>3</sub>H samples exhibited mesoporous structures with a low surface area of 8.85 mm<sup>2</sup>/g and 4.71 mm<sup>2</sup>/g, respectively, supported by the microscopic image of blockage pores. However, the acidity strength for both catalysts was recorded at 3.43 mmol/g and 3.96 mmol/g, which is sufficient for catalysing PFAD biodiesel at the highest yield. The catalytic esterification was optimised at 96.7% and 98.2% with 3 wt.% of catalyst loading, 18:1 of methanol-PFAD molar ratio, 120 °C, and 4 h of reaction. Catalyst reusability was sustained up to 3 reaction cycles due to catalyst deactivation, and the insight investigation of spent catalysts was also performed.https://www.mdpi.com/1420-3049/27/20/7142biodieselsulfonatedglycerolby-productPFADheterogenous catalyst |
| spellingShingle | Balkis Hazmi Mahnoush Beygisangchin Umer Rashid Wan Nur Aini Wan Mokhtar Toshiki Tsubota Ali Alsalme Chawalit Ngamcharussrivichai Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel Molecules biodiesel sulfonated glycerol by-product PFAD heterogenous catalyst |
| title | Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel |
| title_full | Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel |
| title_fullStr | Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel |
| title_full_unstemmed | Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel |
| title_short | Glycerol-Based Retrievable Heterogeneous Catalysts for Single-Pot Esterification of Palm Fatty Acid Distillate to Biodiesel |
| title_sort | glycerol based retrievable heterogeneous catalysts for single pot esterification of palm fatty acid distillate to biodiesel |
| topic | biodiesel sulfonated glycerol by-product PFAD heterogenous catalyst |
| url | https://www.mdpi.com/1420-3049/27/20/7142 |
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