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178 Chapter 7
7.3.4 Synthesis of Cu-DEMOF samples (D1-8)
D1
H3BTC (100mg, 0.48 mmol) and ip (80mg, 0.48 mmol) equaling a 1:1 ratio were mixed
with Cu(BF4)2 6H2O (488 mg, 1.4 mmol) and placed into a 20 ml screw jaw. Subsequently
14 ml N,N-Dimethylformamide (DMF) was added. The screw jaw was then sealed and put
into a pre-heated oven at 80 °C for 20 h. The resulting blue powder products were
collected by centrifugation. Afterwards, they were washed by DMF (30 ml x 3), EtOH (30
ml x 3) and acetone (30 ml x 3) subsequently. The final powder was collected and dried
under air at room temperature. The activation of the solids was performed by heating at
170 °C for 24 h under dynamic vacuum (ca. 10 -3 mbar).
Figure 7.15. 1 H-NMR spectra of the acid-digest D1 sample (solvent: DMSO-d 6 , DCl).