摘要 |
<p>Phosphorus sulphochloride, PSCl2, is manufactured by reacting powdered, or granular, sulphur and phosphorus trichloride, PCl3, in liquid phase, with a metallic aluminium or aluminium alloy catalyst and stirring, at the boiling temperature of PCl3 and atmospheric pressure, wherein the S and PCl3 are added in successive stoichiometric proportions in the presence of a quantity of PSCl2 as medium and moderator at the commencement of the reaction, and PCl3 is simultaneously refluxed back into the reaction mixture. The reaction is a batch process and the weight of PSCl2 present should be at least 3 times the weight of the first S addition. Chippings or small waste of aluminium or alloy are used in excess of 3%. A small excess of PCl3 is added during the last stages of the reaction to ensure absence of unreacted S. When the capacity of the reaction vessel is exhausted, excess PCl3 is distilled off, followed by PSCl2 at 124 DEG -126 DEG C., until a residual fraction is left in the reaction vessel sufficient for the next batch.</p> |