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www.nature.com/scientificreports/ Figure 1. A schematic illustration of the formation of Cu-ABF@ASMNPs nanocatalysts. Figure 2. XRD pattern of (a) MNPs and (b) SMNPs. General reaction procedure for cycloaddition reaction of epoxide. In a dried 10 mL round bottom flask, 5 mmol of epoxide, 4 mol% of 1,8-Diazabicyclo(5.4.0)undec-7-ene (DBU) and 50 mg Cu-ABF@ASMNPs were added. The reaction mixture was stirred at 80 °C for 12 h under atmospheric pressure of CO2. After comple- tion of the reaction, the catalyst was accumulated at the side of the vessel using an external magnet. Finally, the resulting solution was extracted with ethyl acetate and dried over anhydrous Na2SO4. The products were analysed and verified by GC-MS. Results and Discussion X-ray diffraction studies (XRD). The crystalline nature of the nanoparticles (MNPs and SMNPs), was confirmed by XRD studies. The diffraction peaks co-ordinated well with the standard XRD data of the Fe3O4 crystal with cubic inverse spinel structure when compared with the Joint Committee on Powder Diffraction Standards (JCPDS) database (card number, 19-0629) (Fig. 2a). The mean crystalline size of MNPs was measured by Debye–Scherrer equation and found to be 7.8 nm. After encapsulation with silica, a new broad peak at 23° appeared which indicates the presence of amorphous silica coating (JCPDS card number, 82-1574). All the other peaks of MNPs remained intact, exhibiting the phase stability of the magnetic nanoparticles (Fig. 2b)69,70. The XRD studies of catalyst Cu-ABF@ASMNPs were mentioned in Supplementary Fig. S1. Cu ions present in very low concentration in our Cu-ABF@ASMNPs. Therefore, signals for Cu nanoparticles (NPs) were not observed in the XRD pattern of Cu-ABF@ASMNPs. Fourier transform-infrared (FT-IR) spectroscopy. The FT-IR spectroscopy was used to characterize the functionality of the resulting MNPs, SMNPs, ASMNPs, ABF@ASMNPs and Cu-ABF@ASMNPs (Fig. 3). FT-IR spectra revealed the distinctive peak at 583 cm−1 due to vibration of the Fe-O bond of the iron oxide nanoparticles (MNPs) and the broad peak at 3393 cm−1 of O-H stretching vibration due to absorbed water (Fig. 3a). The silica coating on the surface of MNPs was verified by peaks at 1090 cm−1 and 802 cm−1, ascribed to symmetrical and asymmetrical vibration of Si-O-Si bonds respectively (Fig. 3b). Functionalisation of aminopropyl group on the SCientifiC RepoRts | (2018) 8:1901 | DOI:10.1038/s41598-018-19551-3 3PDF Image | copper-based magnetic nanocatalyst for the fixation of carbon dioxide
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