| 摘要 |
882,005. Making organo-metallic compounds, electrolytically. NALCO CHEMICAL CO. April 11, 1960 [May 6, 1959], No. 12771/60. Class 41. Organo-metallic compounds are made by electrolysis of a solution of a Grignard reagent in an anhydrous solvent using a sacrificial metal anode, and adding an organic halide of the same organic radical as the Grignard reagent, whereby there is formed a metal compound from the anode linked to hydrocarbon radicals. For example, a lead anode immersed in ethyl magnesium chloride dissolved in a solvent, e.g. diethyl or dibutyl glycol ether tri-hexylamine or pyridine, with added ethyl chloride forms lead tetraethyl which is separated from the electrolyte by distillation. Any magnesium metal formed at the inert cathode is reconverted to Grignard reagent by the ethyl chloride present. Voltage applied is 12 to 14V increasing to 24V, and at 35‹ to 60‹ C. or higher. Organo-metal compounds include methyl up to butyl and higher homologues; phenyl, and benzyl compounds of Pb, Ca, Zn, Hg, Mn, La, Te, Se, Tl, As and Bi. Magnesium halide also formed is removed to prevent resin formation, by adding dioxane or pyridine which forms complex insoluble substances. The process may be effected under pressure where volatile solvents are present. |
