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• Journal article
  Ewulonu CM, Akromah S, Lee K-Y, Seddon AM, Polesca C, Hallett JP, Eichhorn SJet al., 2025,

  Looking Beyond Pure Cellulose to Lignocellulose for Regenerated Continuous Spun Filaments

  , ACS OMEGA, ISSN: 2470-1343
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• Journal article
  Akaya H, Ouzrour Z, Aziz K, Golenarges S, Nakasu PYS, Hallett JP, Hardacre C, Falkowska M, Altamash T, Jacquemin Jet al., 2025,

  Valorization of Moroccan Alfa Grass through Pyrolytic Conversion to Biochar for Atmospheric CO₂ Capture

  , ACS OMEGA, Vol: 10, Pages: 58991-59003, ISSN: 2470-1343
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• Journal article
  Luan S, Nisar S, Phipps J, Ovejero-Perez A, Hallett JP, Barbara PVet al., 2025,

  Optimization of the ionoSolv process for the preservation of pulp fibre dimensions

  , INDUSTRIAL CROPS AND PRODUCTS, Vol: 236, ISSN: 0926-6690
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• Journal article
  Wesinger S, Rabiner A, Meyer N, Voß D, BrandtTalbot A, Hallett J, Albert Jet al., 2025,

  Sequential fractionation and polyoxometalate‐catalyzed oxidation of lignocellulosic biomass improves cellulose purity and formic acid yield

  , Biofuels, Bioproducts and Biorefining, Vol: 19, Pages: 1862-1874, ISSN: 1932-104X

  Lignocellulosic biomass is an important source of renewable chemicals and materials but its full valorization is necessary in order to achieve economic and sustainability goals. This study proposes a two-step approach for the valorization of lignocellulosic biomass combining solvent-assisted fractionation and catalytic oxidation with molecular oxygen to generate cellulose and formic acid. An industrially relevant lignocellulosic substrate, beech wood, was fractionated under a nitrogen atmosphere using either an organosolv (methanol or ethanol) or ionosolv (ionic liquid) aqueous solvent to produce dissolved hemicellulose and lignin as well as a cellulose-rich solid. The dissolved components were oxidized catalytically to formic acid and its derivatives in a second step using the fivefold vanadium substituted Keggin-type polyoxometalate H8[PV5Mo7O40]. Enzymatic hydrolysis of the cellulose-enriched solid generated purified glucose higher in yields than the single-step comparison method. The organosolv-fractionation increased enzymatic saccharification to 78% whereas the ionosolv-fractionation increased the saccharification yield to 68%, in comparison with 18% for the one-step conversion and only 8% for the untreated beech wood. In the oxidation step, a 28% formic acid yield was achieved under 125 °C, 1200 rpm, 30 bar oxygen, and 6.5 h reaction conditions. The improvements observed for the two-step approach are attributed to the influence of the solvent on the catalyst preventing the latter from interacting with the cellulose-enriched solid, which improved the quality of the pulp and increased the overall formic acid yield.

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• Journal article
  Artime IF, Al Ghatta A, Ouitrakoon P, Damilano G, Brandt-Talbot A, Hallett JP, Barbara PVet 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: 0926-6690

  Surfactant-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 article
  Wang W, Nakasu PYS, Costa JM, D'Acierno F, Ahmad N, Titirici MM, Pontiroli D, Ricco M, Hu C, Hallett JPet 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
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• Journal article
  Wesinger S, Rabiner A, Nisar S, Schill L, Kubus MG, Poller MJ, Riisager A, Brandt-Talbot A, Hallett JP, Albert Jet 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: 1864-5631

  This 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 article
  Nisar S, Barbará PV, Chachuat B, Hallett JP, Brandt-Talbot Aet al., 2025,

  Near-infrared spectroscopy for rapid compositional analysis of cellulose pulps after fractionation with ionic liquids

  , Biomass and Bioenergy, Vol: 201, ISSN: 0961-9534

  The 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 article
  Suleman MY, Judah HL, Bexis P, Fennell P, Hallett JP, Brandt-Talbot Aet al., 2025,

  The acetate anion promotes hydrolysis of poly(ethylene terephthalate) in ionic liquid-water mixtures

  , Green Chemistry, Vol: 27, Pages: 11475-11490, ISSN: 1463-9262

  A 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 article
  Polesca C, Sobreiro-Almeida R, Passos H, Coutinho JAP, Hallett JP, Mano JF, Freire MGet al., 2025,

  Engineered from Waste: Ionic Liquid Processing of Keratin for 3D Printing Biomedical Scaffolds

  , ACS MATERIALS LETTERS
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