Abstract

A magnetic nano-solid acid catalyst Fe3O4-PDA-SO3H was synthetized through an efficient method, as an eco-friendly and more efficient catalyst. The obtained catalyst has uniform core-shell structure, appropriate particle size, and high acid density. Fe3O4-PDA-SO3H was applied to catalyze the esterification of levulinic acid (LA) with alcohols of different chain length to produce the levulinate esters. The catalytic effect was optimized from the aspects of catalyst dosage, reaction temperature, and acid-alcohol molar ratio. Furthermore, the response surface optimization method was used to obtain the optimal conditions. Verified under these conditions, the experimental results showed that the conversion rate of LA can reach 95.87%, which was much higher than common cationic exchange resin Amberlyst 36 and Amberlyst 46. Furthermore, the recovery and reuse of the Fe3O4-PDA-SO3H was demonstrated six times without obvious loss in the activity.

Highlights

  • In the past few years, the attention on biomass and it derivatives [1] has increased remarkably.The consumption of fossil fuels [2] and the influence of greenhouse effect continually drive the vigorous development of biomass fuels [3,4]

  • Levulinate esters were synthesized by an esterification reaction of levulinic acid (LA) with different alcohols [12,13] under acid catalyst

  • The optimal reaction conditions [25] for LA esterification, for example, the reaction temperature and the mole ratio were determined by the maximized conversion of levulinic acid

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Summary

Introduction

In the past few years, the attention on biomass and it derivatives [1] has increased remarkably. Levulinate esters were synthesized by an esterification reaction of levulinic acid (LA) with different alcohols [12,13] under acid catalyst. The magnetic nano-catalysts used in the esterification reaction can be separated from the product by applying a magnetic field [22]. These catalysts can be recycled and reused; and do not require treatment at the acid or water separation stage. A sulfonate group can be successfully loaded outside the carrier to make it a magnetic nano-solid acid catalyst, which can be applied to the synthesis of important compounds. The optimal reaction conditions [25] for LA esterification, for example, the reaction temperature and the mole ratio were determined by the maximized conversion of levulinic acid

Materials
Preparation of Fe3 O4 Nanoparticles
Preparation of Fe3 O4 -PDA Nanoparticles
Preparation of Fe3 O4 -PDA-SO3 H Nanoparticles
Characterization
Determination of Acid Density
Response
Effect of Sulfonation of Chlorosulfonic Acid
Effect of Sulfonation Time on Solid Acid Density
O4 the
XRD Characterization
EDX Characterization
FT-IR Characterization
The peaks at to
Effect of Catalyst Dosage on Esterification Reaction
Optimum
Effect of Reaction Temperature
10. Effect of Acid: Acid
Optimization
H for the esterification of levulinic acid and n-butanol are shown in
Comparison with other Typical Solid Acids
O4 -PDA-SO
Conclusions

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