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2.1. Preparation and characterization of catalysts In-situ CoPc/TiO2 is prepared with the advanced sol–gel proce-dure illustrated in Fig. 1. The precursor is titanium(IV) butoxide. To avoid precipitation during polycondensation and formation of unstable colloidal sols, the hydrolyzing water is homogeneously released by the esterification of alcohol and acetic acid. Then 1,2-dicyanobenzene and analytically pure soluble cobalt chloride are used as the reactants of CoPc and added into the sol precursors. The mixed solutions are adjusted to pH 4 by the addition of HCl and stirred for 12 h at ambient temperature, then aged for 48 h, left in an oven at 60 _C for about 24 h, and finally the resulting xerogels are transferred to a furnace and calcined at 360 _C for 1 h. The sample is crushed into powder. For comparison, the CoPc/TiO2 catalysts are prepared by equilibrium adsorption of CoPc on TiO2 from a solution in dime-thylformamide for about 12 h. The amorphous state of the prepared catalysts is confirmed by X-ray diffraction spectra (XRD) recorded on a Rigaku 2304 diffractometer with Ni-filtered Cu Ka radiation from 8_ to 80_ at a scanning speed of 2_/min. FT-IR and UV–vis spectra of the solid catalysts are recorded on a Perkin–Elmer FT-IR1760 spectrometer and a Lambda Bio40 spectrophotometer, respectively. UV–vis spectrum of the liquid sol sample is recorded by a TU-1901 spec-trophotometer. To understand the thermal behavior of the cata-lysts, we carried out thermogravimetry and differential thermal analysis (DTA–TG) using a WCT-2 equipment in the temperature range of 25–900 _C at a heating rate of 10 _C/min in air. |
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