Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts
Solid acid catalysts of 15 wt.%SO4/SnO2 loaded with 5–45 wt.%WO3 were prepared, calcined at 400–800 °C, and then characterized by TG–DTA, XRD, FT-IR spectra and nitrogen adsorption techniques. The surface acidity was determined by potentiometric titration with n-butylamine in acetonitrile and FT-IR...
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| Format: | Article |
| Language: | English |
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Elsevier
2017-02-01
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| Series: | Arabian Journal of Chemistry |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S1878535212002687 |
| _version_ | 1811273137027809280 |
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| author | M. Nasouh Alaya M.A. Rabah |
| author_facet | M. Nasouh Alaya M.A. Rabah |
| author_sort | M. Nasouh Alaya |
| collection | DOAJ |
| description | Solid acid catalysts of 15 wt.%SO4/SnO2 loaded with 5–45 wt.%WO3 were prepared, calcined at 400–800 °C, and then characterized by TG–DTA, XRD, FT-IR spectra and nitrogen adsorption techniques. The surface acidity was determined by potentiometric titration with n-butylamine in acetonitrile and FT-IR spectra of chemisorbed pyridine.
The presence of sulfate ions together with WO3 hindered the crystallization of tin oxide and the products at a lower temperature of ⩽ 500 °C found amorphous. The crystallinity of tin oxide increased with raising the calcination temperature to provide nanocrystalline cassiterite structure, whereas, increasing WO3 loading up to 25 wt.% decreases the process. Careful control of calcination temperature and WO3 loading was found to have a critical effect on the specific surface area and therefore on the resulted surface acidity.
The surface acidity measurements indicate that the catalysts possess very strong acid sites that designate both of Brønsted and Lewis acid sites.
Catalytic application toward esterification of propionic acid with n-butanol was tested and the effect of various parameters, i.e., reaction temperature, reactant molar ratio, weight of the catalyst, WO3 loading and calcination temperature was also investigated. The highest conversion level was found for products loaded with 25 wt.%WO3 and calcined at 400 °C. Although both of Brønsted and Lewis acid sites are responsible for the reaction, the former acid sites found more effective on catalyzing the esterification reaction. |
| first_indexed | 2024-04-12T22:53:52Z |
| format | Article |
| id | doaj.art-a7020b4475a2433d80fc380169d81ae1 |
| institution | Directory Open Access Journal |
| issn | 1878-5352 |
| language | English |
| last_indexed | 2024-04-12T22:53:52Z |
| publishDate | 2017-02-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Arabian Journal of Chemistry |
| spelling | doaj.art-a7020b4475a2433d80fc380169d81ae12022-12-22T03:13:17ZengElsevierArabian Journal of Chemistry1878-53522017-02-0110S1S705S71810.1016/j.arabjc.2012.11.012Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalystsM. Nasouh AlayaM.A. RabahSolid acid catalysts of 15 wt.%SO4/SnO2 loaded with 5–45 wt.%WO3 were prepared, calcined at 400–800 °C, and then characterized by TG–DTA, XRD, FT-IR spectra and nitrogen adsorption techniques. The surface acidity was determined by potentiometric titration with n-butylamine in acetonitrile and FT-IR spectra of chemisorbed pyridine. The presence of sulfate ions together with WO3 hindered the crystallization of tin oxide and the products at a lower temperature of ⩽ 500 °C found amorphous. The crystallinity of tin oxide increased with raising the calcination temperature to provide nanocrystalline cassiterite structure, whereas, increasing WO3 loading up to 25 wt.% decreases the process. Careful control of calcination temperature and WO3 loading was found to have a critical effect on the specific surface area and therefore on the resulted surface acidity. The surface acidity measurements indicate that the catalysts possess very strong acid sites that designate both of Brønsted and Lewis acid sites. Catalytic application toward esterification of propionic acid with n-butanol was tested and the effect of various parameters, i.e., reaction temperature, reactant molar ratio, weight of the catalyst, WO3 loading and calcination temperature was also investigated. The highest conversion level was found for products loaded with 25 wt.%WO3 and calcined at 400 °C. Although both of Brønsted and Lewis acid sites are responsible for the reaction, the former acid sites found more effective on catalyzing the esterification reaction.http://www.sciencedirect.com/science/article/pii/S1878535212002687Sulfated SnO2WO3TG–DTAXRDFTIRAcidityActivity |
| spellingShingle | M. Nasouh Alaya M.A. Rabah Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts Arabian Journal of Chemistry Sulfated SnO2 WO3 TG–DTA XRD FTIR Acidity Activity |
| title | Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts |
| title_full | Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts |
| title_fullStr | Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts |
| title_full_unstemmed | Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts |
| title_short | Preparation, characterization and catalytic activity of WO3 supported on sulfated tin oxide catalysts |
| title_sort | preparation characterization and catalytic activity of wo3 supported on sulfated tin oxide catalysts |
| topic | Sulfated SnO2 WO3 TG–DTA XRD FTIR Acidity Activity |
| url | http://www.sciencedirect.com/science/article/pii/S1878535212002687 |
| work_keys_str_mv | AT mnasouhalaya preparationcharacterizationandcatalyticactivityofwo3supportedonsulfatedtinoxidecatalysts AT marabah preparationcharacterizationandcatalyticactivityofwo3supportedonsulfatedtinoxidecatalysts |