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Journal articleFirth AEJ, Nakasu PYS, Fennell PS, et al., 2024,
An Ionic Liquid-Based Biorefinery Approach for Duckweed Utilization.
, ACS Sustain Resour Manag, Vol: 1, Pages: 842-856This study establishes a foundation for the ionic liquid (IL) pretreatment of duckweed biomass. An optimized IL-based process was designed to exploit the unique properties of duckweed including efficient metal removal, potential starch accumulation, and protein accumulation. Two ILs, namely, dimethylethanolammonium formate ([DMEtA][HCOO]) and N,N-dimethylbutylammonium hydrogen sulfate ([DMBA][HSO4]), were investigated for the pretreatment of two duckweed species (Spirodela polyrhiza and Lemna minor). The evaluation focused on starch recovery, sugar release, protein recovery, and metal extraction capabilities. [DMEtA][HCOO] demonstrated near-quantitative starch recoveries at 120 °C, while [DMBA][HSO4] showed similar performance at 90 °C within a reaction time of 2 h. Saccharification yields for most pulps exceeded 90% after 8 h of hydrolysis, outperforming "traditional" lignocellulosic biomasses such as miscanthus or sugarcane bagasse. Approximately 50 and 80 wt % of the protein were solubilized in [DMEtA][HCOO] and [DMBA][HSO4], respectively, while the remaining protein distributed between the pulp and lignin. However, the solubilized protein in the IL could not be recovered due to its low molecular weight. Regarding metal extraction, [DMEtA][HCOO] demonstrated higher efficiency, achieving 81% removal of Ni from Lemna minor's pulps, whereas [DMBA][HSO4] extracted only 28% of Ni with slightly higher pulp concentrations. These findings indicate the need for further optimization in concurrent metal extraction using ILs.
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Journal articleHou X, Feng G, Chen Z, et al., 2024,
Tailoring a suitable partner system for cholinium cation to build effective solvents for biomass deconstruction
, GREEN CHEMISTRY, Vol: 26, Pages: 5977-5987, ISSN: 1463-9262 -
Journal articleConstantinou AP, Nele V, Doutch JJ, et al., 2024,
ABC block copolymer micelles driving the thermogelation: scattering, imaging and spectroscopy
, Polymer, Vol: 302, ISSN: 0032-3861Thermoresponsive polymers have attracted much scientific attention due to their capacity for temperature-driven hydrogel formation. For biomedical applications, such as drug delivery, this transition should be tuned below body temperature to facilitate controlled and targeted drug release. We have recently developed a thermoresponsive polymer that forms gel at low concentrations (2 w/w%) in aqueous media and offers a cost-effective alternative to thermoresponsive systems currently being applied in clinics. This polymer is an ABC triblock terpolymer, where A, B, and C correspond to oligo(ethylene glycol) methyl ether methacrylate with average Mn 300 g mol−1 (OEGMA300), n-butyl methacrylate (BuMA), and di(ethylene glycol) methyl ether methacrylate (DEGMA). To investigate the self-assembly and the gelation mechanism in diluted solutions, we used small-angle neutron scattering (SANS) on 1 w/w% (below the gelation concentration) and 5 w/w% solutions (above the gelation concentration). As a comparison, we also investigated the solutions of the most studied thermoresponsive polymer, namely, Pluronic F127, an ABA triblock bipolymer made of ethylene glycol (A) and propylene glycol (B) blocks. SANS revealed that the in-house synthesised polymer forms elliptical cylinders, whose length increases significantly with temperature. In contrast, Pluronic F127 solutions form core-shell spherical micelles, which slightly elongate with temperature. Transmission electron microscopy images support the SANS findings, with tubular/worm structures being present. Variable-temperature circular dichroism (CD) and proton nuclear magnetic resonance (1H NMR) spectroscopy experiments reveal insights on the tacticity, structural changes, and molecular origin of the self-assembly.
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Journal articleChen Y, Lin X, Liu X, et al., 2024,
Thermally robust solvent-free liquid polyplexes for heat-shock protection and long-term room temperature storage of therapeutic nucleic acids
, Biomacromolecules, Vol: 25, Pages: 2965-2972, ISSN: 1525-7797Nucleic acid therapeutics have attracted recent attention as promising preventative solutions for a broad range of diseases. Nonviral delivery vectors, such as cationic polymers, improve the cellular uptake of nucleic acids without suffering the drawbacks of viral delivery vectors. However, these delivery systems are faced with a major challenge for worldwide deployment, as their poor thermal stability elicits the need for cold chain transportation. Here, we demonstrate a biomaterial strategy to drastically improve the thermal stability of DNA polyplexes. Importantly, we demonstrate long-term room temperature storage with a transfection efficiency maintained for at least 9 months. Additionally, extreme heat shock studies show retained luciferase expression after heat treatment at 70 °C. We therefore provide a proof of concept for a platform biotechnology that could provide long-term room temperature storage for temperature-sensitive nucleic acid therapeutics, eliminating the need for the cold chain, which in turn would reduce the cost of distributing life-saving therapeutics worldwide.
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Journal articleGode JN, Malaret FJ, Hallett JP, et al., 2024,
Phosphonium-based ionic liquid immobilised in sodium alginate as a novel adsorbent: Kinetics, thermodynamics, and toxicity study on 2,4-dichlorophenol removal
, CHEMICAL ENGINEERING RESEARCH & DESIGN, Vol: 205, Pages: 161-173, ISSN: 0263-8762 -
Journal articleFirth AEJ, Nakasu PYS, Hallett JP, et al., 2024,
Exploiting Cation Structure and Water Content in Modulating the Acidity of Ammonium Hydrogen Sulfate Protic Ionic Liquids
, JOURNAL OF PHYSICAL CHEMISTRY LETTERS, Vol: 15, Pages: 2311-2318, ISSN: 1948-7185 -
Journal articleCosta JM, Forster-Carneiro T, Hallett JP, 2024,
Progress in the applications of biocompatible ionic liquids: renewable commodity production, catalytic and pharmaceutical approaches - a review
, GREEN CHEMISTRY, Vol: 26, Pages: 705-719, ISSN: 1463-9262 -
Book chapterNisar S, Brandt-Talbot A, Hallett JP, et al., 2024,
Semi-mechanistic modelling of ionic liquid-based biomass fractionation
, Computer Aided Chemical Engineering, Pages: 2527-2532Fractionation of lignocellulosic biomass is a crucial step to provide cellulose, lignin, and hemicellulose for further processing. This work focuses on modelling the fractionation of woody biomass using the ionoSolv process, which employs low-cost ionic liquid water mixtures. We model a simple reaction network to describe the solvent-extraction of three main biopolymers from solid lignocellulosic biomass. We estimate the corresponding kinetic parameters and their credibility intervals using Bayesian parameter estimation and then exploit the calibrated model for a multi-criterion analysis employing three process metrics: glucan (cellulose) recovery, hemicellulose removal, and lignin removal (delignification). Specifically, we construct a probabilistic design space by propagating the model parameter uncertainty, with a view to predicting a feasible operating window for key process variables (pretreatment time, temperature and solids loading) to meet certain thresholds for each metric. Overall, the development of semi-mechanistic models provides a novel framework for the analysis and optimisation of ionic liquid-based biomass pretreatment.
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Journal articleOvejero-Pérez A, Nakasu PYS, Hopson C, et al., 2024,
Challenges and opportunities on the utilisation of ionic liquid for biomass pretreatment and valorisation.
, Npj Mater Sustain, Vol: 2Biomass processing employing ionic liquids is already an established option at the laboratory scale. Ionic liquids can disrupt and deconstruct the lignocellulosic biomass network, giving rise to multiple options for valorisation. However, there is still much work remaining to accomplish the scale-up and commercialisation of ionic liquid-based biomass processing. Important issues such as ionic liquid cost and recyclability, among others, need to be carefully addressed. In addition, ionic liquids modify the structure and properties of the recovered materials, impacting potential applications. Due to the complex nature of ionic liquids, where multiple combinations of anions and cations are possible, these issues should be considered for each process and application, making it difficult to generalise for all cases. This perspective covers the main challenges and opportunities in the employment of ionic liquids for biomass processing, both in the biomass processing stage and in the valorisation of the recovered fractions. Among them, we discuss the importance of solvent recovery and costs as two critical issues to consider in biomass processing, as well as the major role lignin condensation plays in hindering ionoSolv lignin valorisation and different approaches to valorise the recovered cellulose.
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Journal articleShikh Zahari S, Liu Y, Yao P, et al., 2023,
OPEFB pretreatment using the low-cost N,N,N-dimethylbutylammonium hydrogen sulfate ionic liquid under varying conditions
, Scientific Reports, Vol: 13, ISSN: 2045-2322This study investigates the effects of temperature and period on the pretreatment of OPEFB using the low-cost N,N,N-dimethylbutylammonium hydrogen sulfate ionic liquid ([DMBA][HSO4] IL) with 20 wt% of water. The results demonstrate that higher pretreatment temperatures (120, 150, and 170 °C) and longer periods (0.5, 1, and 2 h) enhanced lignin recovery, resulting in increased purity of the recovered pulp and subsequently enhanced glucose released during enzymatic hydrolysis. However, at 170 °C, prolonging the period led to cellulose degradation and the formation of pseudo-lignin deposited on the pulps, resulting in a decreasing-trend in glucose released. Finally, the analysis of extracted lignin reveals that increasing pretreatment severity intensified lignin depolymerisation and condensation, leading to a decrease in number average molecular weight (Mn), weight average molecular weight (Mw) and polydispersity index (Đ) values.
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