| 摘要 |
FIELD: production of inorganic and organic substances. SUBSTANCE: method is based on interaction of phosphorus trichloride with tert-butanol at molar ratio 1:3, process being carrying out in presence of phosphorous acid taken in amount from 0.1 to 1 mol per 1 mol of final product. Reaction is effected by way of adding phosphorus trichloride to boiling tert-butanol- phosphorous acid mixture. Under these conditions, crystallization of final product occurs yet in the course of reaction as formation of the product proceeds. In absence of phosphorous acid initially added, its crystallization takes place usually after termination of the process, sometimes only upon addition of "seed". In such a case crystallization occurs practically instantaneously and is accompanied with large liberation of heat which leads to a danger of outburst of reaction mixture. So introduction of phosphorous acid in the beginning of process ensures its safety. Crystalline acid obtained is practically insoluble in tert-butyl chloride. This fact enables practically quantitative isolation of the two products with high purity degree using no other procedure as simple decantation. EFFECT: increased yield of phosphorous acid and provided isolation of pure coproduct. |
