Synthesis of PAN-b-PMMA block copolymer
This protocol is extracted from research article:
Block copolymer–based porous carbon fibers
Sci Adv, Feb 1, 2019; DOI: 10.1126/sciadv.aau6852

According to our previous report, the PAN-b-PMMA block copolymer was synthesized by RAFT polymerization (31). First, a mixture of MMA (35.0 ml, 310 mmol), CDB (84.28 mg, 0.3094 mmol), and AIBN (25.42 mg, 0.1548 mmol) was dissolved in benzene (51.6 ml) in a 100-ml Schlenk flask. The mixture was subjected to three cycles of freeze-pump-thaw (FPT), followed by back-filling with N2. Then, the flask was placed in an oil bath at 60°C and stirred for 24 hours. The resulting PMMA macro–chain transfer agent (macro-CTA) was precipitated in methanol and dried under vacuum for 12 hours to completely evaporate the remaining solvent. The purified PMMA macro-CTA (Mn, SEC = ~62 kDa; PDI, 1.04) was used to synthesize PAN-b-PMMA block copolymers. PMMA macro-CTA (0.65 g, 11 μmol), AN (2.6 ml, 43 mmol), AIBN (0.44 mg, 2.7 μmol), and DMSO (7.22 ml) were mixed in a 40-ml Schlenk flask equipped with a magnetic stirring bar. The mixture was degassed by three FPT cycles and then heated in an oil bath at 65°C under N2 atmosphere for 24 hours. A PAN-b-PMMA block copolymer (Mn, SEC = ~173 kDa) with a PDI of 1.14 and a PAN volume fraction of 64% was obtained. The PAN-b-PMMA block copolymer was purified similarly to PMMA macro-CTA.

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