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8 protocols using dimethyl carbonate dmc

1

Fabrication of ZrO2 Nanoparticle-Polymer Composite

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Zirconia (ZrO2) nanoparticles (~45 nm) were purchased from SRL. Poly [(vinylidene fluoride)-co-hexafluoropropylene] (PVDF-HFP) (Kynar flex 2801) was procured from Arkema Acetone, dimethylacetamide and Lithium hexafluorophosphate (LiPF6) were purchased from Sigma-Aldrich. Ethyl carbonate (EC) was procured from Alfa Aesar and Dimethyl Carbonate (DMC) from Merck. All the chemicals are of analytical grade and used without any further purification.
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2

Synthesis and Characterization of Fluorinated Polymers

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Vinylidene fluoride (VDF) and tert-butyl 2-(trifluoromethyl)acrylate (MAF-TBE) were kindly supplied by Arkema and Tosoh Finechem Corp., respectively, and used as received. Complexes 1, 2, 3, 5, and 6 were synthesized as described in a previous contribution [23 (link)]. Dimethyl carbonate (DMC, ≥99%, Merck KGaA), acetone (VMR Chemicals), pentane (VMR Chemicals), dimethyl formamide (VMR Chemicals), benzene-d6 (99.5%D, Eurisotop), acetone-d6 (99.5%D, Eurisotop), DMSO-d6 (99.5%D, Eurisotop) and DMF-d7 (99.5%D, Eurisotop) were used as received.
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3

Synthesis of Ethylene-Based Copolymer

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EXAMPLE 4

In this example, an Ethylene-based polymer was produced by incorporating trimethylsilyl-protected methyl vinyl glycolate to assay a number of polymer properties for the resulting compositions.

Ethylene (99.95%, Air Liquide, 1200 psi) and azobisisobutyronitrile (AIBN, 98% Sigma Aldrich) were used as received. Dimethyl carbonate (DMC, anhydrous 99%, Sigma Aldrich) was distilled before use and stored under nitrogen.

Synthesis of copolymer with Ethylene and trimethylsilyl-protected methyl vinyl glycolate (Sample E1)

8 g trimethylsilyl-protected methyl vinyl glycolate, 80 g dimethyl carbonate and 0.1 g of azobisisobutyronitrile were added to a 300 mL Parr reactor. The reactor was sealed and flushed three times with 1000 psi pressure of nitrogen while stirring. The system was then heated, at 70° C. at an Ethylene pressure of 1200 psi and allowed to stir for the desired time. The reaction mixture was collected and the reactor was washed with THF at 60° C. The solvent in the reaction mixture and wash was removed by rotary evaporation. The resulting polymer was dissolved in THF and precipitated into cold methanol, then vacuum filtered.

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4

Synthesis of Sodium Cyclopentadienylide

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Sodium cyclopentadienylide (NaCPD; 2.4 M solution in THF; Sigma-Aldrich, St. Louis, MO, USA,); dimethyl carbonate (DMC; Sigma-Aldrich, St. Louis, MO, USA, anhydrous, >99%); H2SO4 (Fluka, Buchs, Switzerland, p.a. 95–97%); MgSO4 (Sigma-Aldrich, St. Louis, MO, USA, anhydrous, reagent plus, >99.5%); toluene (Sigma-Aldrich, St. Louis, MO, USA, p.a.); isopropanol (Sigma-Aldrich, St. Louis, MO, USA, p.a.); KOH (Kemika, Zagreb, Croatia, p.a., ACS reagent); tetrahydrofuran (THF; Merck, Darmstadt, Germany, p.a. ACS reagent); n-hexane (Sigma-Aldrich, St. Louis, MO, USA, p.a., ACS reagent); ethyl acetate (Sigma-Aldrich, St. Louis, MO, USA, p.a., ACS reagent, >99.5%); silica gel 60 (Merck, Darmstadt, Germany, 0.040–0.063 mm, for column chromatography); 4-(dimethyl amino)pyridine (DMAP; Sigma-Aldrich, St. Louis, MO, USA, ReagentPlus, >99%); HCl, (Fluka, Buchs, Switzerland, p.a., ACS reagent, fuming, >37%, APHA < 10).
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5

Single-cell Li-ion battery electrochemical testing

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All of the electrochemical experiments were performed in a single-compartment teflon cell (Supplementary Fig. 1). The electrolyte consisted of 1 M LiPF6/EC/DEC (EC:DEC=1:2 v/v) (Novolyte Technologies, BASF) with or without 5% VC or FEC additive. Dimethyl carbonate (DMC) (>99.9%, high-performance liquid chromatography grade, Sigma-Aldrich) was used as the rinsing solvent. The counter and reference electrodes were made of Li, whereas the working electrodes were cut from Si(100) wafers with or without micropillars. All potentials reported in this work are referred to the Li/Li+ redox couple. All electrochemical tests were performed inside a glove box filled with Ar gas (H2O and O2 contents <10 p.p.m.). A multi-channel potentiostat (Multistat 1480, Salartron Analytical) was used for potential/current control.
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6

Synthesis of Humins-based Biopolymers

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Gerhumin® (a registered predominantly non-furanic humins solution) was supplied by L.Gobbi S.r.L. (Campo Ligure, Italy). Gerhumin® is extracted in Germany by E. Gerlach GmbH (Lübbecke, Germany). Gerhumin® solution contains 21% solids, 80% of which are organic materials, and 61% of the total solids are humic substances, with 0.7% organic nitrogen on dry material and C/N ratio of 57.1, and pH 9–10. Commercial Mimosa bark condensed tannin extract was supplied by Silva Chimica (St. Michele Mondovì, Italy). Hexamethylene diamine 98%, and dimethyl carbonate (DMC) were bought from Sigma-Aldrich (Saint Louis, France).
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7

Synthesis of Layered Cathode Materials

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The chemicals Mn(NO3)2 (≥ 99 wt%), FeSO4·7H2O (≥ 99 wt%), LiOH (≥ 98 wt%), NH3 solution (30 wt%), H3PO4 (≥ 85%), citric acid monohydrate (C6H8O7·H2O, ≥ 99.5 wt%), polyvinylidene fluoride (PVDF), ethylene carbonate (EC, 98 wt%), and dimethyl carbonate (DMC, ≥ 99 wt%) were purchased from Sigma-Aldrich. All the other chemicals were of analytical grade and used without further purification. All the aqueous solutions were prepared with deionized water (DI water, 18.2 MΩ.cm) for all the experiments.
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8

Graphite-Cellulose Composite Electrode

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Graphite (2000 mesh) was obtained from Aladdin Industries Ltd.; bacterial cellulose (0.80%) under further purification was purchased from Qihong Technology; analytical grade isopropyl alcohol (IPA) was purchased from Tianli Co., Ltd., Shanghai, China. Sodium was purchased from Shenzhen Youyan Technology Co., Ltd. (Shenzhen, China). Sodium hexafluorophosphate (NaPF6) was supplied by Alfa Aesar (purity, ≥99%). Dimethyl carbonate (DMC) and ethylene carbonate (EC) was provided by Sigma-Aldrich. The current collector aluminum foil was supplied by Hefei Kejing Material Technology Co., Ltd., Hefei, China.
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