Semi-continuous process for preparing phosphorus trichloride

Chemistry of inorganic compounds – Phosphorus or compound thereof – Halogen containing

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C01B 2510

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active

052523063

ABSTRACT:
There is disclosed an improved process for the semi-continuous production of phosphorus trichloride by the reaction of elemental phosphorus and chlorine in a liquid phosphorus trichloride layer. In accordance with the present invention periodic termination of the process by discontinuing phosphorus feed thereby creating a heel containing residual phosphorus is rendered more safe and less waste is produced by the improvement which comprises chlorinating the residual phosphorus at a substantially constant flow rate and continuing the chlorine feed rate until after observing at least one of either a step-wise decrease in the pressure within the reactor or a step-wise decrease in the flow rate of phosphorus trichloride removed from the reactor and then terminating the chlorine feed when said pressure and flow rate achieve a substantially steady state at a lower value.

REFERENCES:
patent: 4319894 (1982-03-01), Kempner et al.
Schumann, Rudolph; Rapid Method for Determining Elemental Phosphorus Trichloride; Chem. Tech. (Leipzig) vol. 24, No. 6, p. 363 (1972).
Kirievskaya et al., Gas-Chromatographic Determination of White Phosphorus and of certain Phosphorus Chloride; Zhurnal Prickladnoi Khimmi, vol. 45, No. 9, pp. 2074-2076, (Sept., 1972).
Gantner et al., Applications of Laser Raman Spectrometry in Process Control Central Using Optical Fibers; Fresenius J. anal Chem. vol. 338 pp. 2-8 (1990).
Keeler, R. A. et al.; Analysis of Mixtures of White Phosphorus, Phosphorus Oxychloride and Phosphorus Trichloride; Anal Chem. vol. 26, No. 5, pp. 933-934 (1954).

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