γ-Valerolactone (GVL) has transpired as an ecofriendly solvent, a promising fuel additive, and a precursor to valuable chemicals. The study explores an approach to GVL synthesis by employing non-noble metals in contrast to conventional methods involving noble metals. The selective hydrogenation of levulinic acid (LA) and levulinate esters offers a pathway to GVL production, while the direct transformation from furfural (FA) enhances its potential. The study focuses on 3d transition metal-based N-doped carbon catalysts, highlighting Co/NC as the most effective catalyst for LA to GVL hydrogenation, yielding ∼100% GVL. The catalyst was also employed in a one-pot, three-step cascade reaction: FA hydrogenation to furfuryl alcohol (FOL) was performed using 10% Co/NC, ethanolysis of FOL to ethyl levulinate (EL) was facilitated by H-β, and EL hydrogenation to GVL was performed using 10% Co/NC. Each step was optimized independently. The cascade reaction was executed at 140 °C for 12 h through a comprehensive approach, achieving a noteworthy 92.1% GVL yield from FA, which was further upcycled to the gram scale, offering 86% of the final GVL yield. The catalyst characterization, catalytic activity data, and control experiments culminate in the proposed LA to GVL transformation mechanisms and the one-pot, three-step cascade FA to GVL conversion. The research significantly contributes to advancing sustainable GVL production and its multifaceted applications. 

Synthesis of γ-Valerolactone from Levulinic Acid with Co/NC, and from Furfural via Cascade Reaction Using Co/NC and H-Beta

Biofuels and value-added chemicals can be produced using biomass. These products can substitute the corresponding petroleum-based ones, reducing the carbon footprint, ensuring domestic production, and minimizing/exploiting organic wastes in a circular economy philosophy. Natural mineral-based catalysts seem to be a promising, eco-friendly, and low-cost approach for biomass valorization. This article attempts to highlight the potential of natural mineral-based catalysts for various processes targeting the above valorization. Natural zeolites and clays can be used as catalysts/CO2 adsorbents and catalytic supports in various biorefinery processes (pyrolysis, gasification, hydrothermal liquefaction, esterification/transesterification, hydrotreatment, cracking, isomerization, oxidation, condensation, etc.). Acid/base, redox, and textural properties of these materials are key factors for their catalytic performance and can be easily regulated by suitable treatments, like calcination, acid/base-washing, metal impregnation, doping, etc., which are discussed in this article. The application of natural minerals in biorefinery processes makes them greener, cost-effective, and easily scalable. 

Biomass Conversion to Value-Added Chemicals and Fuels Using Natural Minerals as Catalysts or Catalytic Supports

Controlled thermal treatment enhances catalytic activity of Y zeolite in valorization of furfural. 

Modulating acid sites in Y zeolite for valorisation of furfural to get γ-valerolactone

EFE was easily synthesized from FFalc and ethanol over commercially available, low-cost, and environmentally friendly montmorillonite K10. 

Synthesis of ethyl furfuryl ether via etherification of furfuryl alcohol with ethanol over montmorillonite K10

The valorization of biomass and its transformation into fuels are highly interesting due to the abundance of biomass and its almost neutral carbon emissions. In this article, we show the production of γ-valerolactone (GVL), a valuable product, from furfural (FF), a compound that can be easily obtained from biomass. This FF to GVL transformation involves a catalytic cascade reaction with two hydrogenation steps. Pt and/or Zr supported on sepiolite catalysts have been prepared and tested in the FF transformation reaction. A physical mixture of a Zr-based and a Pt-based catalyst has reached a yield to GVL of ca. 50% after 16 h at 180 °C. This performance largely exceeds that obtained by each of the single Pt or single Zr metal catalysts independently, showing a strong synergistic effect. These data suggest that each metal (Pt and Zr) plays an important and complementary role in different reaction steps. Furthermore, the physical mixture appears to be much more efficient than bimetallic Pt/Zr catalysts synthesized with the same amount of metals. The role of the type of acidity and the oxidation state of the surface platinum species on the catalytic performance has been discussed. Moreover, this reaction has been carried out in batch and continuous flow reactors, and a comparative study between the two operation modes has been undertaken. A certain correlation between the catalytic results obtained by both operation modes has been found.

Promoter Effect of Pt on Zr Catalysts to Increase the Conversion of Furfural to γ-Valerolactone Using Batch and Continuous Flow Reactors: Influence of the Way of the Incorporation of the Pt Sites

This work aims to develop an efficient catalyst for the cascade reaction from furfural to γ-valerolactone in a liquid-phase continuous reactor. This process requires both Lewis and Brønsted acidity; hence, a bifunctional catalyst is necessary to complete the one-pot reaction. Ti/Zr/O mixed oxide-based catalysts were chosen to this end as balancing metal oxide composition allows the acidity characteristics of the overall material to be modulated. Oxides with different compositions were then synthesized using the co-precipitation method. After characterization via porosimetry and NH3-TPD, the catalyst with equimolar quantities of the two components was demonstrated to be the best one in terms of superficial area (279 m2/g) and acid site density (0.67 mmol/g). The synthesized materials were then tested using a plug flow reactor at 180 °C, with a 10 min contact time. Ti/Zr/O (1:1) was demonstrated to be the most promising catalyst during the recycling tests as it allowed obtaining the highest selectivities in the desired products (about 45% in furfuryl isopropyl ether and 20% in γ-valerolactone) contemporaneously with 100% furfural conversion.

/pdf/ti-zr-o-mixed-oxides-for-the-catalytic-transfer-lgeuhxlh.pdf

Ti/Zr/O Mixed Oxides for the Catalytic Transfer Hydrogenation of Furfural to GVL in a Liquid-Phase Continuous-Flow Reactor

Tuning the properties and thermal treatment of Aquivion®/oxide hybrid catalysts for the one-pot production of γ-valerolactone from furfuryl alcohol

The development of multifunctional catalysts is a necessary step to effectively carry out cascade reactions, such as that from furfural to γ‐valerolactone. This research effort faces the challenge posed by the intrinsic limit of how many kinds of catalytic sites a single material can bear. In this work, the application of Spray‐Freeze Drying (SFD) as a synthetic technique for the preparation of a wide range of composite multi‐functional catalysts is reported. Herein we show that by the proper combination of Aquivion as a highly active Brønsted acid catalyst and metal oxides as Lewis acids (LAS) enable to achieve highly unique efficient and effective dual acid composite catalysts that are able to carry out the cascade reaction from furfural to γ‐valerolactone. The dual catalytic system comprised of Aq/ZrO2 with 30% polymer content prepared via spray‐freeze drying exhibited GVL yields of 25% after only 2 h at 180 °C and a remarkably high productivity of 4470 µmolGVL gCat‐1 h‐1, one of the highest reported results. Mechanistic studies based on experimental and advanced characterisation and spectroscopic techniques, such as, SEM, TEM, 15N MAS NMR and 19F MAS NMR indicate that activity arises from the proper tuning of BAS/LAS acidic properties. 

Aquivion-based spray freeze-dried composite materials for the cascade production of γ-valerolactone.

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Ti/Zr/O Mixed Oxides for the Catalytic Transfer Hydrogenation of Furfural to GVL in a Liquid-Phase Continuous-Flow Reactor

Tuning the properties and thermal treatment of Aquivion®/oxide hybrid catalysts for the one-pot production of γ-valerolactone from furfuryl alcohol

Aquivion-based spray freeze-dried composite materials for the cascade production of γ-valerolactone.

Promoter Effect of Pt on Zr Catalysts to Increase the Conversion of Furfural to γ-Valerolactone Using Batch and Continuous Flow Reactors: Influence of the Way of the Incorporation of the Pt Sites