Catalytic production of γ-valerolactone, a biofuel precursor, from furfural in one pot [Dataset]

This work presents for the first time the synergistic effect of tin and zirconium for the one pot transformation of furfural into γ-valerolactone. Furfural is a versatile product that can be easily produced from lignocellulosic biomass and can be transformed into valuable products such as γ-valerolactone, which can be used to produce different types of chemicals, fuels and as a green solvent. The transformation of furfural into γ-valerolactone in one-pot has been studied using Sn and Zr based catalysts supported on treated zeolite Y. These catalysts were characterized by N2 adsorption, IR, UV–vis, XRD, TEM, pyridine adsorption-IR and XPS in order to determine their physicochemical properties. For all the studied compositions, mixed bimetallic Sn-Zr catalysts led to higher γ-valerolactone yields than those monometallic Sn or Zr catalysts. The bimetallic catalyst with a Sn:Zr at. ratio of 1:1 achieved the best performance, reaching a yield to γ-valerolactone of ca. 80 % after only 1 h of reaction at 180 ⁰C using 2-propanol as a hydrogen source. The best performance of the bimetallic catalyst has been related to the broad dispersion of the metals on the surface of the support, forming mixed dispersed Zr-O-Sn surface species, favoring an adequate amount of Lewis and Brønsted acid sites. Moreover, for this catalyst, stability was very high, showing constant yield values to γ-valerolactone after at least 4 uses, which can be related to the high and stable interaction between the surface metal species and the support. Description of methods used for collection/generation of data: Power X-ray diffraction (XRD) patterns of catalysts were collected at two angles between 10 and 80 ⁰ using an Enraf Nonius FR590 sealed tube diffractometer (Bruker, Delft, The Netherlands) equipped with a monochromatic Cu Kα1 source (30 mA and 40 kV). In order to evaluate the Lewis and Brønsted acidity analysis of pyridine adsorption was performed using a Bruker Vertex 70 instrument equipped with a Pike DiffusIR cell attachment and recorded with an MCT detector after 128 scans and with a 4 cm−1 resolution in the region 4000–450 cm−1 to acquire in situ DRIFT spectra. Samples were loaded and pre-treated in a He flow (10 mL min−1) for 1 h at 300 ⁰C. Spectra were acquired after the pretreatment at different temperatures (300, 250, 200, 150, 100 and 50 ⁰C). After the pretreatment the samples were exposed to pyridine vapour (1 μL) for 20 min at 50 ⁰C, followed by re-evacuation at 50–300 ⁰C and IR spectra were measured at the different temperatures (50, 100, 150, 200, 250 and 300 ⁰C). Furfural conversion was carried out in an autoclave reactor, which was covered by a Teflon container of 25 mL. In a typical run, 5 mL of 2-propanol, 0.25 mmol of FF and 0.2 g of catalyst were added to the reactor. Then, the reactor was purged using N2 and sealed. It was placed in a silicon bath at the desired temperature and stirred at 800 rpm. When the reaction finished, the reactor was cooled in an ice-bath and the liquid product was recovered by filtration for the quantitative analysis.Experiments using levulinic acid, methyl levulinate and ethyl levulinate were conducted to produce GVL. The reaction was carried out using 5 mL of 2-propanol, 0.25 mmol of substrate and 0.2 g of catalyst for 1 h at 180 ⁰C.The products were analyzed by a gas chromatograph (GC), using a HP 5890 GC instrument (Hewlett Packard, Palo Alto, CA, USA). The GC has an Agilent HP-1 column (30 m × 0.32 mm × 0.25 μm) an injection port at 220 ⁰C and a flame ignition detector (FID) at 240 ⁰C. The temperature program for a typical run was as follows: (i) 35 ⁰C isothermal for 30 min, (ii) a heating rate of 1.5 ⁰C min−1 from 35 to 230 ⁰C and (iii) 230 ⁰C isothermal for 30 min. In order to identify other reaction by-products a gas chromatography-mass spectrometer was used (GC-MS5977A MSD-7890A, Agilent, Santa Clara, CA, USA). The temperature program used was the same as for the GC-FID. Methods for processing the data: Processed data are registered in files with extension csv.