Abstract
The acetalization of glycerol with acetone represents a strategy for its valorization into solketal as a fuel additive component. Thus, acid carbon-based structured catalyst (SO3H-C) has been prepared, characterized and tested in this reaction. The structured catalyst (L = 5 cm, d = 1 cm) showed a high surface density of acidic sites (2.9 mmol H+ g−1) and a high surface area. This catalyst is highly active and stable in the solketal reaction production in a batch reactor system and in a continuous downflow reactor, where several parameters were studied such as the variation of time of reaction, temperature, acetone/glycerol molar ratio (A/G) and weight hourly space velocity (WHSV). A complete glycerol conversion and 100% of solketal selectivity were achieved working in the continuous flow reactor equipped with distillation equipment when WHSV is 2.9 h−1, A/G = 8 at 57 °C in a co-solvent free operation. The catalyst maintained its activity under continuous flow even after 300 min of reaction.
Highlights
Glycerol excess from biodiesel production provides a good potential raw material for generation of value-added products, such as fuel additives, solvents or chemicals [1,2,3,4]
The reaction between acetone and glycerol is presented in Scheme 1, where (1) solketal (2,2-dimethyl-1, 3-dioxolone-4-methanol), (2) acetal (1,3-dioxan-5-ol) and water are formed over an acid catalyst [10]
A methodology was established to prepare a biogenic conformed carbonaceous support starting from spiral-wound laminated cellulose, considering several steps: Pyrolysis at different temperatures (400–800 ◦ C) and chemical activation (HNO3 )
Summary
Glycerol excess from biodiesel production provides a good potential raw material for generation of value-added products, such as fuel additives, solvents or chemicals [1,2,3,4]. Shirani et al [24] examined an easy-to-scale up continuous system using a heterogeneous catalyst as purolite PD206 catalyst for efficient conversion of glycerol to solketal (95% of yield), at higher residence time under the following reaction conditions of temperature, pressure, feed flow rate, and catalyst’s mass: 20 ◦ C, 120 bar, 0.1 mL min−1 and 0.77 g, respectively. Nanda et al [14] developed an efficient continuous flow process employing several heterogeneous catalysts and, in particular, using a strongly acidic amberlyst, a maximum solketal yield was achieved at 40 ◦ C, 600 psi and weight hourly space velocity (WHSV) of 4 h−1. The effect of reaction conditions (acetone/glycerol molar ratio, temperature, time of reaction and weight hourly space velocity, WHSV) was studied in a batch reactor and in a down-flow continuous reactor as the first approach to scale up the process
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