Materials and methods 1 PROS Dini Iflakhah, Ratna E Modulated synthesis fulltext

D. Iflakhah, R. Ediati SWUP BC.65 pivalik acid, trichloroacetic acid and acid trifluoroasetik. Ren 2014 have reported also modulation UiO-66 using formic acid to produce crystals of crystalline and reduced agglomeration by increasing the concentration of formic acid is added. Bimetallic Ni-MOF5 was reported by Li and co-workers in 2012. The results demonstrated that the Ni-MOF5 not only exhibit larger specific surface areas and larger pores than the MOF-5, but also significantly enhance water resistance of the framework. Herein, we report the modulated synthesis of bimetallic Ni-UiO66 with solvothermal method. 2. Materials and methods 2.1 Materials Zirconium tetrachloride ZrCl 4 Sigma-Aldrich 99,0, 1,4-benzen dicarbocarboxylic acid BDC, Sigma-Aldrich 99.0, N-N -dimethyl formamide DMF, Merck 99.8, Chloroform CHCl 3 , Merck 99.9, Acetic acid CH 3 COOH, Sigma-Aldrirh, 99.85, Nickel II nitrate NiNO 3 2 .6H 2 O, Sigma-Aldrich, 96. All chemicals were pure analysis and used without purification. 2.2 Procedures Synthesis of Ni-UiO66. ZrCl 4 0.3381 g, 1.5 mmol, BDC 0.25 g, 1.5 mmol, NiNO 3 2 6H 2 O 0.0654 g, 0.225 mmol were dissolved in 45 ml DMF at room temperature. 10 HCl 0.052 ml, 1.5 mmol was added. The mixture was stirred at room temperature for 1h. The mixture was transferred into a 50 ml vial, which was sealed and maintained at 140 o C for 6h. The vial was then removed from the oven and allowed to cool to room temperature. The white solid was filtrated, washed with DMF and chloroform and dried at vacuum condition. Ni-UiO66 Mod5 The mixture of Ni-UiO66 as described above was prepared. 5eq of acetic acid 0.5 ml, 7.5 mmol was added. The mixture was stirred at room temperature for 1h. The mixture was transferred into a 50 ml vial, which was sealed and maintained at 140 o C for 6h. The vial was then removed from the oven and allowed to cool to room temperature. The white solid was filtrated, washed with DMF and chloroform and dried at vacuum condition. Ni-UiO66 Mod10 or Ni-UiO66 Mod20 The procedure was similar as described above. However, instead of 5eq of acetic acid, 10eq 0.86 ml, 15 mmol or 20eq 1.71 ml, 30 mmol was used. 2.3 Characterization X-ray diffractometer PXRD, D8 Advance-Bruker aXS using Cu Ka radiation k = 1.54056 Å in the range of 2 = 0 50 was used to confirm the isostructural Ni-UiO66 obtained from modulated synthesis with UiO-66 by Cavka 2009. FTIR Spectrum 100-FT-IR Spectrometer, Perkin-Elmer was used to check the stability of the functional groups on the organic ligands. The spectrum was scanned from 600 to 4000 cm -1. SEM Zeiss EVO MA 10. Analysis was used to capture and determine the morphologies of the crystalline samples. All samples were mounted on a carbon tape and coated with gold prior to measurement. Thermal stability of Ni-UiO-66 obtained from modulated synthesis was checked by a thermogravimetric analysis TGA, TGADSC1 STARe system-METTLER TOLEDO instrument. 10 mg of samples was loaded into a sample holder and heated to 800 C at a rate of 10 Cmin. Modulated synthesis and characterization of Ni-UiO66 SWUP BC.66 3. Results and discussion 3.1 Modulated synthesis of Ni-UiO66