Polydimethylsiloxane (PDMS) polymers are extensively used in a wide range of research and industrial fields, due to their highly versatile chemical, physical, and biological properties. Besides the different two-dimensional PDMS formulations available, three-dimensional PDMS foams have attracted increased attention. However, as-prepared PDMS foams contain residual unreacted low molecular weight species that need to be removed in order to obtain a standard and chemically stable material for use as a scaffold for different decorating agents. We propose a cleaning procedure for PDMS foams obtained using a sugar templating process, based on the use of two different solvents (hexane and ethanol) as cleaning agents. Thermogravimetry coupled with Fourier Transform Infrared Spectroscopy (TG-FTIR) for the analysis of the evolved gasses was used to characterize the thermal stability and decomposition pathway of the PDMS foams, before and after the cleaning procedure. The results were compared with those obtained on non-porous PDMS bulk as a reference. Micro-CT microtomography and scanning electron microscopy (SEM) analyses were employed to study the morphology of the PDMS foam. The thermogravimetric analysis (TGA) revealed a different thermal behaviour and crosslinking pathway between bulk PDMS and porous PDMS foam, which was also influenced by the washing process. This information was not apparent from spectroscopic or morphological studies and it would be very useful for planning the use of such complex and very reactive systems.
Innovative extraction configurations for the biorefining of a biomass waste (citrus peel) were developed in this work. Nonconventional energies, such as microwaves (MW) and ultrasounds (US), were directly irradiated to the fresh orange peel using a versatile MW coaxial dipole antenna. This particular MW configuration enabled us to build two new extraction systems: 1) a coaxial solventless MW-assisted extraction approach (SMWAE) and, 2) a simultaneous ultrasound coaxial MW-assisted hydrodistillation (US-MWHD). The yield and chemical composition of the essential oils of the orange peel obtained by the two innovative approaches were analyzed as a function of the extraction time and compared with the coaxial microwave hydrodistillation (MWHD) and conventional hydrodistillation (CH). The EOs were chemically characterized by GC and GC-MS analysis. The residue mash was then used to extract pectin by a MW-assisted procedure. Structure and thermal stability of the pectin were investigated by FTIR and TG. The biorefining of EOs and pectin from a citrus waste maximise the benefits of our proposed green methodologies, which involve safe operability, faster processing and easy scalability. Furthermore, the energy consumed per unit mass of products in each step of the orange peel biorefining clearly showed that the most promising approach is the SMWAE (since it is around around 27 times lower than the CH approach). The MWHD and US-MWHD also showed more than 60% energy savings compared to the CH
The full utilization of agricultural waste and its recycle into a new chain of value are of primary importance for the development of a sustainable and profitable agricultural industry. Chestnut shell waste (CSW) is an interesting case of study, whose valorization has been though partially investigated to date. This work aims at exploring the complete utilization of CSW, in terms of obtaining both value-added compounds and enriched cellulose and lignin fractions. The results were obtained via the unreported combined use of two classes of nonconventional organic solvents, namely natural deep eutectic solvents and bio-based ionic liquids (bio-ILs). At first, combinations of choline chloride (ChCl)-based DESs with an acid, a polyol, or a sugar as hydrogen bond donors were employed for the extraction of polyphenols from the CSW. The best performing system was found to be ChCl:oxalic acid dihydrate (ChCl:Oax2H 2 O). The extraction efficiencies of the DESs tested correlate well with the measured Kamlet−Taft α parameters. After polyphenol removal, the residual solid material was treated with a bio-IL [cholinium glycinate (ChGly)] for further separation of lignin and cellulose. The products obtained by the fractionation process were characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis, which confirmed the separation of the residue into a lignin-rich material and a cellulose-rich material. The results obtained were further corroborated by a three parallel reaction model combined with the distributed activation energy model, which allowed for predicting the composition of the pristine CSW and of the ChCl:Oax2H 2 Otreated CSW as well as the two fractions obtained after ChGly treatment. The recyclability of the best performing DES and the recovery of the bio-IL have also been proven, which make the whole process viable and amenable for large-scale applications.
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