A continuous-flow process for the acetalization of crude glycerol with acetone on zeolite catalysts

Kowalska-Kuś, Jolanta; Held, A.; Nowiǹska, Krystyna

doi:10.1016/j.cej.2020.126143

Cited by 46 publications

(18 citation statements)

References 45 publications

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“…BEA zeolite and the hierarchical zeolite of MFI structure exhibited high catalytic activity in solketal production, i.e. almost 85% of glycerol conversion and 98% selectivity to solketal were achieved as reported by Kowalska-Kuś et al 21 .…”

Section: Introductionsupporting

confidence: 61%

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

Sci Rep

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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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Section: Introductionsupporting

confidence: 61%

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

Sci Rep

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“…A mesoporous phenolsulfonic acid-formaldehyde polymeric acid catalyst was synthesized that provides glycerol conversion of 97% as reported by Laskar et al 16 .BEA zeolite and the hierarchical zeolite of MFI structure exhibited a high catalytic activity in solketal production, i.e. almost 85% of glycerol conversion and 98% selectivity to solketalwere achieved as reported by Kowalska-Kuś et al 17 .…”

Section: Introductionmentioning

confidence: 87%

Process Optimization with Acid Functionalised Activated Carbon derived from Corncob for Production of 4-Hydroxymethyl-2,2-Dimethyl-1,3-Dioxolane and5-Hydroxy-2,2-Dimethyl-1,3-Dioxane

Kaur

Sarma

Jha

et al. 2021

Preprint

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This study focuses on the application of the corncob derived base (NaOH) activated and acid (H2SO4) functionalized carbons for the glycerol valorization to produce 2,2-Dimethyl-1,3-dioxolane-4-methanol (solketal), an oxygenated additive to fuel. The two derived catalysts viz., AAC-CC and AC-CC were subjected to various techniques for the determination of their structural properties and their comparison is made on the basis of characteristics and conversion into the final product. The conjugated boat structure of AAC-CC resulted very high surface area (779.8 m2/g) and higher pore volume (0.428cc/g) of AAC-CC that unveil its suitability as better among the two catalytic pathways during the solketal production. The acidic catalyst shows the highest catalytic activity as compared to basic due to the availability of the more active sites to the catalyst that will help in the reaction for higher conversion. The face cantered composite design (FCCD) of RSM was applied for the optimization of the reaction parameters for the ketalisation reaction. From the optimized results, the acidic catalyst AAC-CC gives higher glycerol conversion, i.e. 80.3% than the basic catalyst AC-CC i.e. 72.12% 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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“…The operating temperature of ketalization reaction was kept moderate as it is exothermic in nature, which is thermodynamically not favorable at higher operating temperatures. In this series of simulation runs, a high initial molar ratio of acetone to glycerol was employed as it can significantly enhance the yield of solketal [50,51]. To ensure the equilibrium of the reaction, all the experiments were allowed to take place for enough time while monitoring the concentrations of glycerol and solketal vs. time until there was no change observed in the results (equilibrium was established).…”

Section: Influence Of Interaction Parameters On Solketal Yieldmentioning

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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A continuous-flow process for the acetalization of crude glycerol with acetone on zeolite catalysts

Cited by 46 publications

References 45 publications

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

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

Process Optimization with Acid Functionalised Activated Carbon derived from Corncob for Production of 4-Hydroxymethyl-2,2-Dimethyl-1,3-Dioxolane and5-Hydroxy-2,2-Dimethyl-1,3-Dioxane

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

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