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Journal articleArtime IF, Al Ghatta A, Ouitrakoon P, et al., 2025,
Surfactant-assisted ionic liquid fractionation of spruce produces a low molar weight and less condensed lignin
, Industrial Crops and Products, Vol: 235, ISSN: 0926-6690Surfactant-assisted ionoSolv fractionation of spruce sawdust was investigated with the aim of improving the fractionation performance and the quality of the recovered fractions. Anionic surfactants sodium dodecyl sulfate (SDS) and linear alkylbenzenesulfonate (LAS) were added to ionic liquid (IL) water mixtures of N,N-dimethylbutylammonium hydrogen sulphate ([DMBA][HSO4]) containing 20–50 wt% water to process spruce sawdust at 150 and 170 °C for 30–60 min. 1H NMR spectroscopy established that the processing conditions partly hydrolysed SDS whilst leaving LAS untouched. The use of LAS surfactant decreased the fractionation time but did not encourage the use of a higher water content. IonoSolv fractionation employing 2–10 wt% LAS and 20 wt% water resulted in faster delignification, decreasing the reaction time by 50 % at 150 ºC, with small improvements in cellulose recovery (87.6 % with 2 wt% LAS vs 83.7 % without LAS at 150 ºC). Post-treatment lignin analysis showed that the lignin structure was less condensed when LAS was present during the fractionation. Addition of surfactant had a lightening effect on the colour of the recovered lignin fractions, which is a key feature for its use in applications such as coatings, cosmetics or sunscreen additives. A proportion of LAS surfactant precipitated with the lignin fraction and was found to be mainly physically associated to lignin, although traces of condensed lignin-LAS were also detected. Whilst the extent to which surfactants may assist ionoSolv fractionation was limited, the study highlights the importance of characterising both lignin and cellulose chemical compositions.
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Journal articleWang W, Nakasu PYS, Costa JM, et al., 2025,
Pectin Extracted by a Recyclable Molecular Mixture: A Promising Material for Porous Membranes in Quasi-Solid-State Na-Ion Batteries
, ACS SUSTAINABLE CHEMISTRY & ENGINEERING, Vol: 13, Pages: 18061-18074, ISSN: 2168-0485 -
Journal articleWesinger S, Rabiner A, Nisar S, et al., 2025,
Boosting POM-ionosolv biorefining of lignocellulosic biomass by using redox-balanced polyoxometalate catalysts in methanolic ionic liquid reaction media
, ChemSusChem, Vol: 18, ISSN: 1864-5631This article presents an advanced iteration of the polyoxometalate (POM)-Ionosolv concept to generate biobased methyl formate in high yield and a bleached cellulose pulp from lignocellulosic biomass in a single-step operation by using redox-balanced POM catalysts and molecular oxygen in alcoholic ionic liquid (IL) mixtures. The performance of the three Ionosolv-ILs triethylammonium hydrogen sulfate ([TEA][HSO4]), N,N-dimethylbutylammonium hydrogen sulfate ([DMBA][HSO4]), and tributylmethylphosphonium methyl sulfate ([TBMP][MeSO4]), mixed with methanol (MeOH) (30/70 wt%), is evaluated by methyl formate yield from extracted hemicellulose and lignin as well as purity of the bleached cellulose pulp in the presence of various Keggin-type POMs. The redox-balanced H8PVMnMo10O40 POM catalyst in [TBMP][MeSO4]/MeOH emerge as the most effective combination, achieving 20% methyl formate yield from commercial beech wood. The glucan content in the bleached cellulose-enriched solid consisted is over 90%, demonstrating that the use of MeOH drastically improved lignin extraction in parallel with full hemicellulose extraction. The cellulose is highly susceptible to enzymatic hydrolysis, generating a pure and concentrated cellulosic glucose stream. The formed solid catalyst complex is examined in detail to reveal its chemical nature as POM-IL-complex. The approach is applicable to disparate types of lignocellulosic biomass, including hardwood, softwood, and grass.
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Journal articleNisar S, Barbará PV, Chachuat B, et al., 2025,
Near-infrared spectroscopy for rapid compositional analysis of cellulose pulps after fractionation with ionic liquids
, Biomass and Bioenergy, Vol: 201, ISSN: 0961-9534The composition of cellulose-enriched solids is typically monitored using a laborious and expensive wet-lab analytical method. Here, the development and application of an alternative tool that uses NIR spectroscopy and a software sensor is reported, drawing on a large data set (149 training samples) consisting of untreated grass, hardwood, and softwood biomass and cellulose pulps obtained after fractionation with the low-cost ionic liquids triethylammonium hydrogen sulfate ([TEA][HSO4]) or N,N-dimethylbutylammonium hydrogen sulfate ([DMBA][HSO4]) mixed with water. A partial least squares (PLS) model was trained on compositions determined with the traditional wet-lab procedure, followed by the application of an uncertainty quantification framework to estimate confidence in the predictions. Good agreement with the wet-lab experimental data (mean absolute errors on unseen samples below 5%) was found for ionic liquid fractionated cellulose and purified cellulose samples generated with non-ionoSolv approaches. Cellulose with low crystallinity and isolated lignins generated poor fits, suggesting that more specialised models are needed. The sugar-derived pseudo-lignin (humin) content in the cellulose pulp was estimated by comparing the model with a second PLS model that excluded charred (over-treated) pulps. The study shows that NIR soft-sensors can cost- and time-effectively estimate the composition of ionoSolv-based pulps, speeding up process and product development and facilitating process operation.
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Journal articleSuleman MY, Judah HL, Bexis P, et al., 2025,
The acetate anion promotes hydrolysis of poly(ethylene terephthalate) in ionic liquid-water mixtures
, Green Chemistry, Vol: 27, Pages: 11475-11490, ISSN: 1463-9262A circular plastic economy reduces raw material consumption and discourages pollution. Chemical recycling upgrades the quality of recyclate and is a complementary approach to thermomechanical recycling of plastic waste. This study investigated the use of aprotic and protic ionic liquids (ILs) as solvents for chemical recycling by the hydrolysis of the most common polyester plastic, poly(ethylene terephthalate) (PET). Combinations of three types of cations (aprotic 1-alkyl-3-methylimidazolium, protic 1-methylimidazolium and protic 1,5-biazocyclo-[4.3.0]non-5-enium) combined with a range of anions (acetate, chloride, methanesulfonate, hydrogen sulfate, methyl sulfate, trifluoromethanesulfonate and chlorozincate) were used to hydrolyse PET in the presence of 15 wt% water as the co-solvent and reagent. PET conversion under the screening conditions (180 °C, 3 h, 5% PET loading) varied between 1 and 100%, with ILs containing the acetate anion enabling >97% PET conversion irrespective of the cation. Acidification with aqueous HCl recovered crude crystallised terephthalic acid (TPA). Significant crude yields (46–93%) were only observed for the acetate ILs. The purity of the crude TPA was 34–98%, with 1-ethy-3-methylimidazolium acetate, [C2C1im][OAc], and 1-methylimidazolium acetate, [C1Him][OAc], yielding more and purer TPA than 1,5-biazocyclo-[4.3.0]non-5-enium acetate, [DBNH][OAc]. TPA solubility, PET conversion and TPA yield generally correlated well with increasing pKa and higher hydrogen bond acceptor strength of the IL anion, suggesting that the depolymerisation mechanism in the acetate IL water mixtures is base catalysed. The screening identifies aqueous mixtures of the (pseudo)-protic IL [C1Him][OAc] as promising catalytic solvent component for the chemical recycling of PET at an industrially feasible temperature, due to high isolated TPA yields and purity achieved at a low solvent cost ($1.74–2.15 per kg). However, an effective separation a
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Journal articlePolesca C, Sobreiro-Almeida R, Passos H, et al., 2025,
Engineered from Waste: Ionic Liquid Processing of Keratin for 3D Printing Biomedical Scaffolds
, ACS MATERIALS LETTERS -
Journal articleNakasu PYS, Martinez MA, Melanie S, et al., 2025,
Chitosan-Based Biocomposite Hydrogels with Squid Pen Protein for Anionic Dyes Adsorption (vol 7, pg 1012, 2025)
, ACS MATERIALS LETTERS -
Journal articleAljohani M, Lan L, Daly H, et al., 2025,
Enhancing Hydrogen Production from Bioenergy Crops via Photoreforming
, JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, Vol: 147, Pages: 29679-29686, ISSN: 0002-7863 -
Conference paperNisar S, Seidner S, Brandt-Talbot A, et al., 2025,
Sparse regression approach to modelling the effect of ionic liquid acidity in biomass fractionation
, 14th IFAC Symposium on Dynamics and Control of Process Systems, including Biosystems DYCOPS 2025:, Publisher: Elsevier BV, Pages: 73-78, ISSN: 2405-8963Fractionation of lignocellulosic biomass is a crucial step to provide cellulose, lignin, and hemicellulose for further processing. This paper is concerned with modelling biomass fractionation using the ionoSolv process, which employs low-cost ionic liquid water mixtures, with a special focus on describing the effect of acid:base ratio of the mixture on process performance. We build on an existing semi-mechanistic modelling framework describing the solvent extraction of three main biopolymers from woody biomass for varying fractionation temperature, time, and solids loading. Since the effect of acidity is poorly understood from a mechanistic standpoint, we use sparse regression with lasso regularisation to incorporate it in the semi-mechanistic model. We investigate both polynomial and exponential functional forms and find that the latter yields more physically-consistent results. This enabled us to recalibrate the parameters of the combined semi-mechanistic and sparse data-driven models simultaneously to accurately predict the effect of varying acid:base ratio. This hybrid modelling framework opens new opportunities for further analysis and optimisation of ionic liquid-based biomass fractionation processes.
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Journal articleShmool TA, Martin LK, Jirkas A, et al., 2025,
Design principles for engineering ionic liquid-gold nanoparticles for therapeutic delivery to the brain
, ACS Nano, Vol: 19, Pages: 24806-24816, ISSN: 1936-0851Ionic liquid (IL) nanotechnology holds significant promise for designing nanoscale materials with tunable viscosity, polarity, and thermal stability for advanced therapeutic applications. However, the field currently lacks comprehensive guidelines for integrating ILs into complex therapeutic formulations. Herein, we propose the key design considerations for engineering immunoglobulin G (IgG) conjugated to gold nanoparticles (AuNPs) in the presence of choline-based ILs. By judicious IL cation and anion selection, we fine-tune the supramolecular assemblies and leverage the unique physicochemical properties of ILs to impart AuNPs with advantageous characteristics including enhanced structural, thermal, and thermodynamic stabilities, highly tunable morphologies, and markedly reduced aggregation propensities. Through systematic circular dichroism measurements, the thermodynamic parameters of the complex formulations were determined, offering insight into the IgG conformational changes and design parameters for systems of enhanced IgG conjugation to AuNP surfaces. In demonstrating the power of our design approach, the complex formulation of IgG-choline chloride-AuNPs, also including trehalose, histidine, and arginine, was delivered via focused ultrasound and microbubbles across the blood–brain barrier and showed a 7.6-fold increase in delivery in vivo compared to the traditional formulation. We demonstrate that IgG-IL-AuNPs can be easily and precisely manipulated at the nanometer scale, enabling the formation of versatile structural configurations. Holistically, we believe the rational design approach developed will advance the engineering of tailored IL-nanocarriers for targeted therapeutic delivery and broaden the scope of IL applications in biomedicine.
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