Solketal synthesis from glycerol and acetone in the presence of metal salts: A Lewis or Brønsted acid catalyzed reaction?

Silva, Márcio José da; Rodrigues, Alana Alves; Pinheiro, Patrícia Fontes

doi:10.1016/j.fuel.2020.118164

Cited by 45 publications

(15 citation statements)

References 49 publications

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“…32%) > Co(NO 3 ) 2 = Mn(NO 3 ) 2 = Zn(NO 3 ) 2 = Ni(NO 3 ) 2 = NaNO 3 (ca. 0%) . The authors verified that the trend obeyed the acidity of solutions measured in the presence of metal salts.…”

Section: Resultssupporting

confidence: 57%

“…When we compared these results with the reactions described in this work, we concluded that the presence of silicotungstate anions plays an important role in these reactions; the activity of the metal cations was significantly improved when the nitrate anion was replaced by the silicotungstate anion. 53 The glycerol ketalization is a reversible reaction that may produce ketal with fiveand six-membered ring compounds (i.e., 2,2-dimethyl-[1,3] dioxolan-4-yl methanol (I), and 2,2dimethyl-[1,3] dioxan-5-ol (II)) (Scheme 1).…”

Section: Resultsmentioning

confidence: 99%

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Iron (III) Silicotungstate: An Efficient and Recyclable Catalyst for Converting Glycerol to Solketal

2020

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Section: Resultssupporting

confidence: 57%

Section: Resultsmentioning

confidence: 99%

Iron (III) Silicotungstate: An Efficient and Recyclable Catalyst for Converting Glycerol to Solketal

2020

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“…The Nb–SBA-15 (Nb metal modified SBA-15 catalyst) gives 95% glycerol conversion as reported by Ammaji et al 16 . Fe(NO 3 ) 3 ·9H 2 O exhibited the highest catalytic activity, virtually converting all the glycerol to solketal, with 95% selectivity as reported by Silva et al 17 . The OTS-grafted HY (organosilane modified HY) catalyst reported having high catalytic activity (89% conversion) at low temperatures as stated by Rahaman et al 18 .…”

Section: Introductionsupporting

confidence: 65%

Process optimization with acid functionalised activated carbon derived from corncob for production of 4-hydroxymethyl-2,2-dimethyl-1,3-dioxolane and 5-hydroxy-2,2-dimethyl-1,3-dioxane

Kaur

Sarma

Gera

et al. 2021

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In this article, a two-step activated carbon preparation technique from corncob has been elucidated. The derived catalysts AAC-CC has been characterized using various techniques for the determination of their structural properties and compared with AC-CC, already reported with another article. The conjugated boat structure of AAC-CC resulted in a very high surface area (779.8 m2/g) and high pore volume (0.428 cc/g). This unveils the suitability of AAC-CC as better among the two catalytic pathways for solketal production. The activated carbons so prepared have been used for the valorization of glycerol to produce 2,2-Dimethyl-1,3-dioxolane-4-methanol (solketal), oxygenated additives to fuel. The face-centered composite design (FCCD) of RSM was applied for the optimization of the reaction parameters for the ketalisation reaction using AAC-CC as a catalyst. From the optimized results, the acidic catalyst AAC-CC resulted in a glycerol conversion, i.e. 80.3% under the actual laboratory experiment. Moreover, the catalyst could be reused for three consecutive batch reactions without (< 5%) much reduction of activity and no distinctive structural deformity.

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“…This might occur due to the establishment of equilibrium of the ketalization process. Moreover, an extensive increase in the acetone to glycerol molar ratio caused the active sites on the catalyst surface to decrease due to their blockage with acetone on the surface of the catalyst, increasing the total volume of the reaction mixture [36,37]. In addition, a higher acetone to glycerol molar ratio increases the acetone concentration in the reaction mixture, resulting in difficult product separation.…”

Section: Optimization Of Solketal Yield Using Response Surface Method...mentioning

confidence: 99%

“…The highest glycerol conversion of 75% was found at the optimized reaction conditions of 335 K, 36,000 s, and 6.9:1 acetone to glycerol molar ratio. In another study, Silva et al [37] investigated the conversion of glycerol into solketal by using tin silicotungstate catalyst. The maximum glycerol conversion of 99% was achieved at the glycerol to acetone molar ratio of 16:1, keeping the other parameters as the reaction temperature of 120 min and reaction temperature of 298 K. Although the overall conversion was higher in this study, the glycerol to acetone was also kept higher.…”

Section: Optimization Of Solketal Yield Using Response Surface Method...mentioning

confidence: 99%

Valorization of Solketal Synthesis from Sustainable Biodiesel Derived Glycerol Using Response Surface Methodology

et al. 2021

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Biodiesel production has gained considerable importance over the last few decades due to the increase in fossil fuel prices as well as toxic emissions of oxygen and nitrogen. The production of biodiesel via catalytic transesterification produces crude glycerol as a co-product along with biodiesel, amounting to 10% of the total biodiesel produced. Glycerol has a low value in its impure form, and the purification of glycerol requires sophisticated technologies and is an expensive process. The conversion of crude glycerol into value-added chemicals such as solketal is the best way to improve the sustainability of biodiesel synthesis using the transesterification reaction. Therefore, the conversion of crude glycerol into the solketal was investigated in a batch reactor simulation model developed by the Aspen Plus V11.0. The non-random two liquid theory (NRTL) method was used as a thermodynamic property package to study the effect of four input ketalization parameters. The model was validated with the findings of previous experimental studies of solketal synthesis using sulfuric acid as a catalyst. The influence of the following operating parameters was investigated: reaction time of 10,000 to 60,000 s, reaction temperature of 303 to 323 K, acetone to glycerol molar ratio of 2:1 to 10:1, and catalyst concentration of 0.005 to 0.03 wt %. The optimum solketal yield of 81.36% was obtained at the optimized conditions of 313 K, 9:1, 0.03 wt %, and 40,000 s. The effect of each input parameter on the ketalization process and interaction between input and output parameters was investigated by using the response surface methodology (RSM) optimizer. The relationship between independent and response variables developed by RSM fit most of the simulation data, which showed the accuracy of the model. A second-order differential equation fit the simulation data well and showed an R2 value of 0.99. According to the findings of RSM, the influence of catalyst amount, acetone to glycerol molar ratio, and reaction time were more significant on solketal yield. The effect of temperature on the performance of the reaction was not found to be significant because of the exothermic nature of the process. The findings of this study showed that biodiesel-derived glycerol can be effectively utilized to produce solketal, which can be used for a wider range of applications such as a fuel additive. However, further work is required to enhance the solketal yield by developing new heterogeneous catalysts so that the industrial implementation of its production can be made possible.

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Solketal synthesis from glycerol and acetone in the presence of metal salts: A Lewis or Brønsted acid catalyzed reaction?

Cited by 45 publications

References 49 publications

Iron (III) Silicotungstate: An Efficient and Recyclable Catalyst for Converting Glycerol to Solketal

Iron (III) Silicotungstate: An Efficient and Recyclable Catalyst for Converting Glycerol to Solketal

Process optimization with acid functionalised activated carbon derived from corncob for production of 4-hydroxymethyl-2,2-dimethyl-1,3-dioxolane and 5-hydroxy-2,2-dimethyl-1,3-dioxane

Valorization of Solketal Synthesis from Sustainable Biodiesel Derived Glycerol Using Response Surface Methodology

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