Verfahren zur Herstellung von Alkali-und/oder Erdalkaliphosphaten

摘要

In a process for the preparation of alkali and/or alkaline earth metal phosphates, the hydroxides and/or salts having a volatile anion, at least partially in the form of an aqueous solution or suspension, are sprayed in a reaction chamber into, or in the immediate vicinity of a flame produced by burning phosphorus in a free oxygen-containing gas, and the phosphates are removed in the form of a melt. As shown, the reaction chamber is surrounded by graphite walls 2 having bores and channels through which cooling gas, e.g. air, may pass. The walls may be surrounded by a jacket 12. Phosphorus, preferably liquid, fed through line 5 is sprayed by means of compressed air supplied by line 6 while the solution or suspension is fed through line 3 to the centre of nozzle 1, and atomized by air fed through line 4. At least part of the solution or suspension may be sprayed towards the centre of the flame by means of additional, preferably two-component, nozzles arranged circumferentially around nozzle 1. Warm air or steam may be used in the case of concentrated solutions. The slit widths of nozzle 1 are preferably such that the speed of the phosphorus is 0.5-5 metres/sec., that of the solution or suspension 1-12 metres/sec., that of the gas for spraying the liquid 300-1500 metres/sec. and that of the gas for burning and spraying the phosphorus 50 to 350 metres/sec. In one embodiment, part of the metal compound may be introduced as finely-divided solid, preferably via the central nozzle. Cooling is adjusted so that the temperature of the wall is maintained at below 900 DEG C., preferably below 750 DEG C., but not lower than 100 DEG C. below the temperature at which the phosphate melt begins to flow. Cooling may be regulated so that a layer of wholly or partially solidified melt, at most 20 mm. thick, is formed on the internal surface of the wall. Alternatively the graphite may have previously been impregnated with phosphate by means of a thinly liquid phosphate melt having metal oxide: P2O5 molar ratio of less than 1.3. During impregnation the pressure in the cooling system is lower than that in the vessel, while during reaction the opposite obtains. The cooling gases are distributed according to the temperature gradient within the vessel. The product preferably accumulates as a melt on the lower end of the vessel, is maintained molten by supplementary heating, and is withdrawn therefrom via discharge 13, developed as a dam, in such quantities that there remains in the chamber the amount of melt produced in more than ten minutes, preferably more than thirty minutes. An off-gas pipe leading to the two or multi-stage scrubbing tower 8 is located in the vicinity of the liquid surface, preferably immediately above, and has baffle plates 14 and at least one nozzle 15 for spraying scrubbing liquid, consisting of water or dilute H3PO4, into the off-gases, reducing the temperature from 500-900 DEG C. to 100 DEG C. or less. The solids content, i.e. excess P2O5 and entrained product, in the scrubbing solution may be 10-60% by weight. More dilute solutions from subsequent stages are continuously supplied to the first stage. The scrubbing solution may be recycled by means of pumps, and concentrated phosphate solution removed through lines 9 and two-component nozzles 7 into the phosphorus flame, if desired after dilution by means of line 10. Fresh water is introduced at 11. The solution may be freed of arsenic, by means of H2S or Na2S before being returned to the reaction vessel. Finely divided solid starting material may be suspended in the recycled scrubbing liquid for introduction to the reaction zone. The liquid may contain 10-90% by weight of solid material.