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2 protocols using de hibit 200

1

ATRP Synthesis and Purification of Polymers

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Acrylonitrile (Merck, Darmstadt, Germany, 99%) was passed through a macroreticular ion exchange resin (De-Hibit-200, Polysciences Inc., Warrington, PA, USA) to remove the inhibitor. Methyl methacrylate (99%), 2-bromopropionitrile (BPN, 97%), CuBr (98%), 2,2′-bipyridine (99%), N,N,N′,N′,N″-pentamethyldiethylenetriamine (99%), N,N-dimethylformamide (DMF, 99.8%), 2-cyanopyridine (2CNP, 99%), ethylene carbonate (EC, >99%), sulfur (>99%, rhombic sulfur), methanol, and 2-propanol were purchased from Merck and used as received.
All the polymer syntheses were carried out by copper-mediated atom transfer radical polymerization (ATRP) in EC or 2CNP, using BPN or bromine-terminated PAN as initiators for homopolymerization and copolymerization, respectively, following previously reported procedures [19 (link),20 (link)]. At the end of the polymerization, the reaction mixture was dissolved in DMF, and the polymer was precipitated in a methanol/2-propanol (3/1 v/v) mixture. The polymer was filtered, washed several times with methanol and water, dried under vacuum to constant weight, and finally purified, passing its DMF solution through alumina columns to remove Cu and other residues. Carbon was synthesized in a tubular furnace (Carbolite, Sheffield, UK) operating under O2 or N2 flow.
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2

Polymer Synthesis and Characterization

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Methanol, n-hexane, acetone (analytical grade), and triethylamine (TEA) (HPLC grade) were from J.T. Baker (USA). Tetrahydrofuran (THF), deuterated chloroform (CDCl3), methyl methacrylate (MMA, 99%), and dimethyl 2-(aminoethyl) methacrylate (DMAEMA, 98%) were from Sigma-Aldrich (USA) and their polymerization inhibitor, MEHQ, was removed using De-HiBit-200 (Polysciences, Inc., USA) macroreticular ion exchange resin. 2,2′-azobisisobutyronitrile (AIBN, 98%), 1,1′-azobis(cyclohexane carbonitrile) (ACHN, 98%), 2-cyano-2-propyl dodecyl trithiocarbonate (chain transfer agent, CTA), and buffers were from Sigma-Aldrich. NaH2PO4, boric acid, HCl, and NaOH were from Merck (Germany). Isopropyl β-D-1-thiogalactopyranoside (IPTG) and 5-bromo-4-chloro-3-indolyl β-D-galactoside (X-Gal) were from Thermo Scientific (USA). Gel permeation chromatography (GPC) standard for average molar mass determination was Poly(methyl methacrylate) Standard ReadyCal Set, Mp 500-2,700,000, from Sigma Aldrich.
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