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9 protocols using 1 ethyl 3 methylimidazolium acetate

1

Pretreatment of MSW and Agave Bagasse

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For the MSW, paper waste materials were prepared as in [9 (link)], consisting of 15% glossy paper, 25% non-glossy paper, 32% non-glossy cardboard, and 28% glossy cardboard using a process developed by Idaho National Laboratory (INL). It is recognized that this material is not representative of real MSW streams and that there may be contaminants present that will impact pretreatment effectiveness. However, the goal of this study was to examine the effectiveness of the IL systems in this study on the types of paper that would be found in MSW. Destiladora Rubio, a tequila plant from Jalisco, Mexico, donated the AGB. The AGB was milled with a Thomas-Wiley Mini Mill fitted with a 40-mesh screen (Model 3383-L10 Arthur H. Thomas Co., Philadelphia, PA, USA). Both ground biomass samples were stored at 4 °C in a sealed plastic bag prior to their use. The 1:1 blend was prepared by mixing both MSW and AGB in the pretreatment reactor just before the heating process begins. 1-ethyl-3-methylimidazolium acetate [C2C1Im][OAc] and 1-butyl-3-methylimidazolium acetate [C4C1Im][OAc], citric acid, ethanol, glucose, xylose, sulfuric acid, and HPLC grade water were purchased from Sigma–Aldrich.
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2

Anchote Starch Extraction and Plasticization

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Anchote (Coccinia Abyssinica) starch was used in this research. Anchote tuber was obtainedfrom the local market at Nekemet, Oromia Region, Ethiopia. The anchote starch was extracted from the tuber using a modified literature procedure[19 (link)]. The plasticizers, such as glycerol, 1-ethyl-3-methylimidazolium acetate, sorbitol andtriethylene glycol, were purchased from Sigma Aldrich and used as received.
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3

Cellulose Extraction and Enzymatic Hydrolysis

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Microcrystalline cellulose: Avicel PH-101 and Whatman cellulose filter paper No. 1 were purchased from Sigma Aldrich Chemie GmbH (Darmstadt, Germany). The cellulolytic enzyme from the microscopic fungus Trichoderma reesei ATCC 26921 with an activity of 700 units/g and the ionic liquids 1-allyl-3-methylimidazolium chloride (≥97.0%) and 1-ethyl-3-methylimidazolium acetate (≥95.0%) were also purchased from Sigma Aldrich Chemie GmbH (Darmstadt, Germany).
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4

Cellulose Solutions Preparation and Characterization

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For the preparation of
cellulose solutions, three types of commercially available materials
have been used: microcrystalline cellulose (MC) from Merck Millipore
with a degree of polymerization (DP) ≈ 210–230 (according
to supplier specification); Avicel PH 101 (Avicel) from Sigma-Aldrich
with DP ≈ 18043 (link) and α–Cellulose
from Sigma-Aldrich with DP ≈ 780.44 (link) The room temperature ionic liquids 1-ethyl-3-methylimidazolium acetate
([Emim][OAc]) and 1-butyl-3-methylimidazolium acetate ([Bmim][OAc]),
both in BASF quality (≥95%), have been purchased from Sigma-Aldrich.
The ionic liquids and the cellulose materials are both hygroscopic.
[Emim][OAc] and [Bmim][OAc] water content was ≤1.1% according
to supplier specification. Because in our previous works we had demonstrated
that traces of water do not hinder cellulose solubilization and do
not have a negative impact to the phase separation process,45 (link) all materials were used as received. Further
on, we considered that this may also facilitate the up-scaling if
desired. Dimethylsulfoxide (DMSO; analytical reagent, assay ≥99.5%)
from VWR International was used as co-solvent for cellulose dissolution.
The precipitation of the porous films was performed in water purified
with a Merck–Millipore purification system and having a resistivity
of ∼18.2 MΩ.cm and a TOC value below 5 ppm.
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5

Eucalyptus Kraft Pulp Dissolution in Ionic Liquids

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The Eucalyptus Bleached Hardwood Kraft Pulp (BHKP) provided by one Chilean Kraft Pulp Mill was used in all the experiments. The chemical composition of the BHKP is listed in Table 1.
Chemical reagents: dimethyl sulfoxide or DMSO (CAS No.67-68-5, purity ≥ 99.7), 1-butyl-3-methylimidazolium chloride or [bmim][Cl] (CAS No.79917-90-1, purity > 98%), 1-butyl-3-methylimidazolium acetate or [bmim][Ac] (CAS No.284049-75-8, purity > 95%), 1-butyl-3-methylimidazolium hydrogen sulfate or [bmim][HSO4] (CAS No. 262297-13-2, purity > 95%), 1-Ethyl-3-methylimidazolium chloride or [emim][Cl] (CAS No.65039-09-0, purity = 98%) and 1-Ethyl-3-methylimidazolium acetate or [emim][Ac] (CAS No. 143314-17-4, purity = 97%) were purchased from Sigma-Aldrich and stored in inert atmosphere until its use. The ILs’ water content before drying was measured for all ILs by Karl Fischer titration, as in our previous work [33 (link)]. The water content of all ILs previous drying was less than 2800 ppm or 0.28% w/w. Therefore, a vacuum drying step was added in order to ensure a water content lower than this percentage. Despite this, it was challenging to precisely measure the water content of the IL in the pulp dissolving process due to environment condensed water and that within the pulp.
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6

Pretreatment of 1-Ethyl-3-methylimidazolium Acetate

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1-Ethyl-3-methylimidazolium acetate (95%)
was purchased from Sigma-Aldrich. The ionic liquid was pretreated
in a vacuum oven (30 inHg) at 50 °C for 24 h to increase the
solubility of the solvent.
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7

Ionic Liquid-Based Manganese Synthesis

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The ionic liquid, 1-ethyl-3-methylimidazolium
acetate, and 97% ([EMIM][OAc]) were purchased from Sigma-Aldrich.
Anhydrous manganese acetate, 98%, was purchased from Alfa Aesar. The
ionic liquid was vacuum dried at 90 °C for 12 h prior to use.
All chemicals were stored in an inert nitrogen atmosphere glovebox.
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8

Nanoparticle Formulation and Evaluation

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Avicel PH-101 (MCC), Brij L23, dichloromethane (DCM Z 99.9%), methanol (MeOH, Z99.9%), 1-ethyl-3-methylimidazolium acetate (EMIMAc, 95%), pyrene (Z99.0%) and (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazoliumbromid) (MTT) were purchased from Sigma-Aldrich. Acetone (Z99.8%, VWR Chemicals), ethanol (EtOH, 99.5%, Solveco), poly(D,L-lactide-co-glycolide) (PLGA, 70 : 30 L : G, M w 10 kDa, Polysciences Inc.) and poly(vinyl alcohol) (PVA, 95% hydrolyzed, M w 95 kDa, Acros Organics) were also used. Eagle's minimum essential medium with Earle's balanced salt solution buffered with NaHCO 3 , non-essential amino acids, stable glutamine, fetal bovine serum and trypan blue stain were purchased from Gibco Life Technologies. Sodium pyruvate, penicillin-streptomycin, trypsin-EDTA and DPBS without Ca 2+ were purchased from GE Healthcare HyClone. All chemicals were used as received. Unless otherwise specified, water of MilliQ quality (resistivity Z 18 MO cm) was used.
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9

Electrochemical Characterization of Cellulose-based Ionic Liquid Composites

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All reagents such as NaCl (≥98% purity), acetic acid (≥99.8% purity), 1-ethyl-3-methyl-imidazolium acetate ([EMIm][OAc]), dimethyl sulfoxide (DMSO), ethanol (absolute), α-cellulose (C8002, powder), chitosan (75-85% deacetylated) with low molecular weight (26 kDa), medium molecular weight (109 kDa), agarose, and high molecular weight (310-375 kDa) were purchased from Sigma-Aldrich and used without any further purification. All solutions used in the electrochemical studies were prepared in high purity demineralised and filtered water (18.2 MΩ cm resistivity).
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