Sulfated Iron Oxide: A Proficient Catalyst for Esterification of Butanoic Acid with Glycerol

Kaur, Kamalpreet; Wanchoo, R. K.; Toor, Amrit Pal

doi:10.1021/ie504916k

Cited by 30 publications

(21 citation statements)

References 30 publications

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“…As observed and inferred (Fig. 6(d)) conversion increased appreciably till 0.06 g mL −1 , afterward showing a flat region, this fact recommends the accessibility of an adequate number of acid sites capable of fetching the reaction to equilibrium (32,(39)(40)(41)(42)(43)(44)(45)(46)(47). This increase in the conversion is directly related to the increase in the quantity of active acid sites available for the reaction to proceed.…”

Section: Catalyst Loading Optimizationsupporting

confidence: 53%

“…So according to Le-Chatelier's principle, an excess of any one of the reactants in the reaction can shift the equilibrium toward forward direction. This increases the forward rate constant of the reaction, favoring the conversion and hence yield of the product ester (32,(39)(40)(41)(42)(43)(44)(45)(46)(47). Alcohols can be easily separated by distillation from the reaction mixture, and they are comparatively cheaper than acids.…”

Section: Effect Of Molar Ratio Of Acid To Alcohol On the Yieldmentioning

confidence: 99%

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Photochemical Synthesis of Lactic Acid Esters at Ambient Temperature Employing Sulfonically Fuctionalized N/W‐Doped Nano‐semiconductor

Verma

Wanchoo

Toor

2021

Photochem & Photobiology

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Appreciating the wide array of applications of lactic acid esters in the flavoring industry as well as in cosmetic and pharmaceutical industries, respectively, their clean and green synthesis gain immense importance. Therefore, traditional ester synthesis processes, involving high-temperature requirements, need to be replaced. A photochemical route has been adopted where visible light illumination was used as the major driving force to synthesize lactic acid esters. This process involves the application of sulfonically functionalized nitrogen/tungsten-doped nanotitania as photocatalysts. These functionalized catalysts efficiently and repeatedly catalyzed the esterification of lactic acid at ambient temperature. The photo-activity of these catalysts is attributed to the presence of a large number of active sulfonate sites on its surface. As per the proposed photochemical mechanism, illumination initiates the electron discharge from the conduction band, which migrates toward absorbed lactic acid through sulfonate sites forming lactic acid radical. This radical in turn attracts the alcohol molecules producing the desired ester. Reaction parameters were optimized to maximize the product yield. The economic validity of the photocatalyst was specked by repetitive experiments, and both the catalysts were found to be efficient even after five reusability cycles. The development of these catalysts can completely replace commercial ester synthesis strategies.

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Section: Catalyst Loading Optimizationsupporting

confidence: 53%

Section: Effect Of Molar Ratio Of Acid To Alcohol On the Yieldmentioning

confidence: 99%

Photochemical Synthesis of Lactic Acid Esters at Ambient Temperature Employing Sulfonically Fuctionalized N/W‐Doped Nano‐semiconductor

Verma

Wanchoo

Toor

2021

Photochem & Photobiology

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“…From this plateau, 600 °C is chosen as the calcination temperature to form a singlephase Fe2O3 before treated with HSO3Cl. in other researchers' study 19) . Subsequently, the Fe, O and S elemental analyses were determined using the EDX measurement and tabulated in Table 3.…”

Section: Catalyst Characterizationmentioning

confidence: 64%

Catalytic Esterification of Palm Fatty Acid Distillate into Biodiesel Over Sulfonated Iron Oxide Catalyst

Matius

Mastuli

2021

J. Jpn. Inst. Energy

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The palm fatty acid distillate (PFAD), as a low-cost feedstock, was catalytically esterified into biodiesel (also known as fatty acid methyl ester, FAME) using sulfonated iron oxide (HSO3ˉ/Fe2O3) catalyst. In this work, the catalyst was synthesised via self-propagating combustion (SPC) method, towards a greener synthesis technique, followed by sulfonation with chlorosulfonic acid (HSO3Cl) to enhance the catalyst's acid properties. The catalysts were characterised and the success of sulfonation process was determined. From this study, Fe2O3 catalysts were proven to be pure and single-phase. The success of the sulfonation then was verified by the presence of sulfur, functional groups of S-O asymmetric vibration and S=O symmetric vibration, and increasing total acidity. Then, the sulfonated Fe2O3 catalyst was used to esterify the PFAD feedstock in methanol in which the esterification parameters were also optimized to obtain maximum free fatty acid (FFA) conversion. It was found that 15:1 of methanol-to-PFAD molar ratio, 4 wt.% of catalyst loading, 80 °C of reaction temperature and 5 h of reaction time produced 95.5% of FFA conversion. Interestingly, the sulfonated Fe2O3 catalyst can be considered as a superacid solid catalyst that enables boosting the esterification of the PFAD feedstock into biodiesel.

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“…A broad band of sulfate groups observed in S/CoAl 2 O 4 (F/O = 0.5) and S/CoAl 2 O 4 (F/O = 1) spectra becomes narrower by increasing the F/O ratio because of increased availability of metal ions for bonding with sulfate groups. The broad bands could be attributed to the presence of remarkable amounts of free sulfate ions with T d symmetry on the catalyst surface, resulting in less interaction between sulfate groups and metal ions [15,38]. On the other hands, symmetric and asymmetric stretching vibrations of S-O band for the samples fabricated at high F/O ratio could detect at 995 cm −1 and 1070 cm −1 , respectively [39,40].…”

Section: Ftir Analysismentioning

confidence: 96%

Fabrication of nanosized SO42−/Co–Al mixed oxide via solution combustion method used in esterification reaction: effect of urea-nitrate ratio on the properties and performance

et al. 2019

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Recently, mixed metal aluminate as a highly active, stable, and reusable nanocatalyst was extremely used in chemical reactions such as esterification. The preparation of the samples via a simple, rapid, and cost-effective method is one of the main problems on the front of the industrial application of these materials. For this purpose, the solution combustion method (SCM) was assessed for the fabrication of spinel CoAl 2 O 4 , and the effects of fuel-to-oxidizer (F/O) ratio on crystalline structure, surface functional groups, surface area, morphology, and porosity were analyzed. The activity of the samples, which was impregnated by the sulfate group was evaluated in the esterification reaction. Morphology and texture properties of the samples indicated the crystallinity, surface area, and pore diameter of CoAl 2 O 4 were enhanced by increasing the F/O ratio. It can be related to increasing the combustion reaction time and temperature. However, at F/O ratios above two, due to limited diffusion of oxygen into the reaction medium, the reaction terminated immaturely. Sulfated cobalt aluminate fabricated at F/O ratio of two was successfully synthesized in nanoscale with same particle size. Moreover, it did not show impurity in its structure that is related to the ability of the combustion method for the fabrication of pure nanocatalyst. Evaluation of the catalytic activity of the SO 4 2− /CoAl 2 O 4 nanocatalysts in the esterification reaction confirmed the results of physicochemical studies. For instance, the sample prepared at F/O ratio of two presented the highest conversion (96.7%) at methanol/oleic acid molar ratio of nine, catalyst amount of 3 wt. %, and reaction temperature and time of 120 °C and 4 h, respectively. In addition to preserving its activity for four runs (conversion > 85%), its activity was simply recovered upon regeneration by sulfate group, making it a promising alternative for industrial production of biodiesel.

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Sulfated Iron Oxide: A Proficient Catalyst for Esterification of Butanoic Acid with Glycerol

Cited by 30 publications

References 30 publications

Photochemical Synthesis of Lactic Acid Esters at Ambient Temperature Employing Sulfonically Fuctionalized N/W‐Doped Nano‐semiconductor

Photochemical Synthesis of Lactic Acid Esters at Ambient Temperature Employing Sulfonically Fuctionalized N/W‐Doped Nano‐semiconductor

Catalytic Esterification of Palm Fatty Acid Distillate into Biodiesel Over Sulfonated Iron Oxide Catalyst

Fabrication of nanosized SO42−/Co–Al mixed oxide via solution combustion method used in esterification reaction: effect of urea-nitrate ratio on the properties and performance

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