GB770789A - Improvements in or relating to the preparation of condensation reaction products of phosphoryl chloride and ammonia - Google Patents

Abstract

<PICT:0770789/III/1> A condensation product containing combined nitrogen and phosphorus is prepared by reacting phosphoryl chloride and gaseous ammonia in the absence of a solvent at a temperature maintained below 100 DEG C., heating the resulting mixture of phosphoryl amide and ammonium chloride to at least 120 DEG C., e.g. to 120-130 DEG C. for a water soluble product, or to about 200 DEG C. for a water insoluble product, and removing ammonium chloride from the mixture by teaching with a solvent. Phosphonyl chloride from elongated container 23 is fed through spout 24 over the surface of revolving horizontal cylinder 1 cooled by water circulating therethrough from pipe 28. Ammonia enters the housing 7, which may be brick, cement or metal, through pipe 25. The mixture of phosphornyl amide and ammonium chloride is scraped off the drum by scraper 34 on to moving conveyer 20, passing through heat insulating wall 6a, which prevents heating of the ammonia gas in the reaction compartment. Fabric curtains 22 are provided to prevent ammonia escape. Conveyer 20, which may be metal or asbestos or glass cloth, carries the mixture under electric heater 32, which heats it to 120-130 DEG C. or to about 200 DEG C. The ammonium chloride may be leached out by water or dilute methanol from pipes 35 and washed into tank 36, and the condensation product may be dried by air or heat, e.g. at 70-120 DEG C. Conveyer 20 and cylinder 1 are both driven by electric motor 11. The phosphonyl chloride may be under pressure, and may be sprayed on to the cylinder, and spout 24 may be directed to one side of the axial plane of the cylinder. Heater 32 may be replaced by steam heated pipes or a gas heater, and a screw conveyer may be used in place of conveyer 20. Ammonia pipe 25 may be directed at the spout 24 to blow away incrustation.