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    • 126. 发明授权
    • Process for making halogenated phosphonophosphoric acid-esters and their
use
    • 制备卤代膦酸磷酸酯的方法及其用途
    • US4894469A
    • 1990-01-16
    • US128805
    • 1987-12-04
    • Horst StaendekeWerner Krause
    • Horst StaendekeWerner Krause
    • C07F9/40C08K5/5337
    • C08K5/5337C07F9/4006C07F9/4015
    • Halogenated phosphonophosphoric acid esters of the general formula ##STR1## in which X stands for a halogenR' stands for an alkylene having from 1 to 4 carbon atomsA stands for ##STR2## R'" stands for identical or different alkyl groups having from 1 to 4 carbon atoms, a halogen or hydrogen, and R.sup.IV stands for a halogen or hydrogen, are made. To this end, phosphorus (III) chloride is reacted in a first step with an alkylene oxide in the presence of a catalyst; the resulting reaction product consisting substantially of phosphorous acid trialkylesters is freed from alkylene oxide in excess and reacted in a second step with a suitable halogenoacyl halide in a molar ratio of 2:1-1.5; the resulting phosphonophosphoric acid ester is repeatedly scrubbed with water and/or an aqueous solution of ammonia and then either separated or halogenated in a third step under ultraviolet light, repeatedly scrubbed with water and/or an aqueous ammonia solution, and separated.
    • 其中X代表卤素R'的通式为“IMAGE”的卤化膦磷酸酯代表具有1至4个碳原子的亚烷基。A代表相同或不同的烷基 具有1至4个碳原子的基团,卤素或氢,RIV表示卤素或氢。 为此,氯化磷(III)在催化剂存在下在第一步与环氧烷反应; 基本上由亚磷酸三烷基酯组成的反应产物不含过氧化烯烃,在第二步中与合适的卤代酰卤反应,摩尔比为2:1-1.5; 得到的膦酸磷酸酯用水和/或氨水反复洗涤,然后在紫外线下在第三步骤中分离或卤化,用水和/或氨水溶液反复洗涤并分离。