Samples of 5 wt.% Pd/SiO2 catalyst reduced at moderate (400 graduateC) and high temperature (600 graduate C) were investigated in the reaction of 1,2-dichloroethane hydrodechlorination (HDC). The highly reduced catalyst exhibited a higher selectivity towards ethylene, approaching 70% at 300 graduate C, whereas the catalyst reduced at 400 graduateC gave mainly ethane (SC2H6 ~90% at 300 graduate C). Reduction of Pd/SiO2 at 600 graduate C leads to the formation of palladium silicide. In consequence, incorporation of Si in Pd surface lowers the hydrogenating strength of palladium, contributing to a higher ethylene selectivity. Such a behaviour resembles an analogous situation with Pd modified by Ag. It was shown that the catalysts deactivated rapidly at temperatures between 200 and 300 graduate C. After reaction, much larger amounts of carbon were found in the sample reduced at 400 graduate C. X-ray diffraction studies showed that a considerable part of this carbon was located in the bulk of palladium phase, i.e. forming a PdCx solution.
The stable products of radiolysis of 1,2-dichloroethane (12DCE) ?-irradiated in an oxygen-free atmosphere were investigated. The pure products of radiolysis were separated by preparative gas chromatography and identified by 1H, 13C NMR and mass spectroscopy as well as quantitative gas chromatography. In the gas phase we have obtained H2 and HCl; in the liquid phase: chloroethane, 1,1-dichloroethane, 1,1,2-trichloroethane, 1,2,4-trichlorobutane and 1,2,3,4-tetrachlorobutanes (dland meso-: [2R,3R] or [2S,3S] and [2R,3S]-isomers). On the basis of the results obtained a preliminary scheme for the formation of the stable products is proposed.
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