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Journal of Materials Chemistry A
Page 7 of 9
DOI: 10.1039/C7TA02205K
Journal Name
tetrabutylammonium phosphate in acetonitrile.
ARTICLE
A
Pt counter
Acknowledgements
electrode and a SCE reference electrode were used. Scan rate: 100
mV/s, T = 25 oC.
This work was supported by the National Natural Science
Foundation of China (No. 51473064, 61435005 and 21274050).
Synthesis of CF-HCP. The monomer CF (100.0 mg, 0.196 mmol) and
FDA (0.08 mL, 0.783 mmol), anhydrous FeCl3 (0.127 g, 0.783 mmol)
and 1,2-dichloroethane (4.0 mL) were added into a 10 mL Schlenk
bottle at room temperature. Then the mixture was degassed via
three freeze-pump-thaw cycles. The bottle was flame-sealed and
heated at 80 oC for 24 h under a nitrogen atmosphere. The mixture
was then cooled to room temperature, the precipitated network
was filtered and washed with water, methanol, dichloromethane
and acetone, respectively. The further purification of the network
was carried out by Soxhlet extraction from methanol for 24 h. The
product was dried in vacuum for 10 h at 80 oC to give CF-HCP as a
deep-red powder (101.0 mg, 92% yield). Elemental analysis (%)
calcd.: C 75.46, H 4.41, N 7.65; found: C 74.63, H 4.31, N 6.54; IR
(KBr): 2925, 2812, 1724, 1605, 1562, 1479, 1448, 1323, 1227, 1191,
1083,1017, 885, 837, 789, 741, 699, 645 and 591 cm-1. The surface
area (SABET) of CF-HCP (CF:FeCl3:FDA = 1:4:4) is 1217 m2 g-1. The
molar ratio of monomer CF:FeCl3:FDA = 1:2:2 and 1:6:6 in the
polymerization reaction were investigated, in order to achieve high
surface areas for the resulting polymer networks. The isolation
yields for obtained under various reaction conditions are 76.9% for
CF-HCP (CF:FeCl3:FDA = 1:2:2) and 99.5% for CF-HCP (CF:FeCl3:FDA =
1:6:6), respectively. Then the molar ratio of FDA to the monomer CF
was set at 4:1, the obtained polymer has the highest surface area.
The nitrogen sorption isotherms of CF-HCPs under different
reaction conditions are shown in Fig. S1.
Notes and references
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Weber, J. D. Epping, M. Antonietti A. Thomas, Adv. Mater.,
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