Preparation and Characterization of Cu and Ni on Alumina Supports and Their Use in the Synthesis of Low-Temperature Metal-Phthalocyanine Using a Parallel-Plate Reactor

Materials (Basel). 2013 Sep 30;6(10):4324-4344. doi: 10.3390/ma6104324.

Abstract

Ni- and Cu/alumina powders were prepared and characterized by X-ray diffraction (XRD), scanning electronic microscope (SEM), and N₂ physisorption isotherms were also determined. The Ni/Al₂O₃ sample reveled agglomerated (1 μm) of nanoparticles of Ni (30-80 nm) however, NiO particles were also identified, probably for the low temperature during the H2 reduction treatment (350 °C), the Cu/Al₂O₃ sample presented agglomerates (1-1.5 μm) of nanoparticles (70-150 nm), but only of pure copper. Both surface morphologies were different, but resulted in mesoporous material, with a higher specificity for the Ni sample. The surfaces were used in a new proposal for producing copper and nickel phthalocyanines using a parallel-plate reactor. Phthalonitrile was used and metallic particles were deposited on alumina in ethanol solution with CH₃ONa at low temperatures; ≤60 °C. The mass-transfer was evaluated in reaction testing with a recent three-resistance model. The kinetics were studied with a Langmuir-Hinshelwood model. The activation energy and Thiele modulus revealed a slow surface reaction. The nickel sample was the most active, influenced by the NiO morphology and phthalonitrile adsorption.

Keywords: Cu-phthalocyanine; Cu/Al2O3; Ni-phthalocyanine; Ni/Al2O3; parallel-plate reactor; phthalocyanine; phthalonitrile.