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    • 7. 发明授权
    • Process for preparing ethanebis(alkylphosphinic) acids
    • 制备乙烷二(烷基次膦酸)酸的方法
    • US06583315B2
    • 2003-06-24
    • US10025739
    • 2001-12-19
    • Martin SickenNorbert WeferlingHans-Peter Schmitz
    • Martin SickenNorbert WeferlingHans-Peter Schmitz
    • C07F930
    • C07F9/305
    • The invention relates to a process for preparing ethanebis(alkylphosphinic) acids by a) reacting elemental yellow phosphorus with alkyl halides in the presence of alkali metal hydroxide or of alkaline earth metal hydroxide to give a mixture whose main constituents are the alkali metal salts and/or alkaline earth metal salts of alkylphosphonous, phosphorous, and hypophosphorous acid, b) liberating alkylphosphonous, phosphorous, and hypophosphorous acid by adding mineral acids, and also at the same time precipitating the alkali metal ions and, respectively, alkaline earth metal ions in the form of their salt of the mineral acids, and then c) esterifying the alkylphosphonous acid from the mixture of the alkylphosphonous, phosphorous, and hypophosphorous acid, d) isolating the ester of alkylphosphonous acid from the mixture and hydrolyzing the same to give alkylphosphonous acid, and e) preparing, from the alkylphosphonous acid, the corresponding ethanebis(alkylphosphinic) acid of the general formula (I) where R1 and R2 may be identical or different and are hydrogen, a carboxy group, a carboxylic acid derivative, an unsubstituted or substituted alkyl group having from 1 to 10 carbon atoms, phenyl, benzyl, or alkyl-substituted aromatics, and R3 and R4 are identical or different and are an unsubstituted or substituted alkyl group having from 2 to 20 carbon atoms, by free-radical-initiated reaction with alkynes, and also to the use of the ethanebis(alkylphosphinic) acids prepared by this process as starting material for preparing flame retardants and precursors for the synthesis of other phosphorus-containing compounds.
    • 本发明涉及通过在碱金属氢氧化物或碱土金属氢氧化物的存在下使元素黄磷与烷基卤反应来制备乙烷二(烷基次膦酸)的方法,得到主要成分为碱金属盐和/或碱金属盐的混合物 烷基磷酸,亚磷酸和次磷酸的碱土金属盐,b)通过添加无机酸释放烷基磷酸,磷和次磷酸,同时沉淀碱金属离子和分别形成的碱土金属离子 的无机酸盐,然后c)从烷基亚磷酸,磷酸和次磷酸的混合物中酯化烷基亚磷酸,d)从混合物中分离出烷基亚磷酸的酯,并将其水解,得到烷基亚磷酸,和e) 从烷基亚磷酸制备相应的通式为的乙烷二(烷基次膦酸)酸 (I)其中R 1和R 2可以相同或不同并且是氢,羧基,羧酸衍生物,未取代或取代的具有1-10个碳原子的烷基,苯基,苄基或烷基取代的芳族化合物, R3和R4相同或不同,是具有2至20个碳原子的未取代或取代的烷基,通过与炔进行自由基引发反应,以及使用通过该方法制备的乙烷二(烷基次膦酸) 作为制备阻燃剂的原料和用于合成其它含磷化合物的前体。
    • 9. 发明授权
    • Process for preparing dialkylphosphinic acids and their salts
    • 制备二烷基次膦酸及其盐的方法
    • US06359171B1
    • 2002-03-19
    • US09577463
    • 2000-05-24
    • Norbert WeferlingMartin SickenGünter KolbeHans-Peter Schmitz
    • Norbert WeferlingMartin SickenGünter KolbeHans-Peter Schmitz
    • C07F930
    • C07F9/48C07F9/30
    • The invention relates to a process for the preparation of dialkylphosphinic acids and salts thereof, which comprises a) reacting elemental yellow phosphorus with alkylating agents in the presence of a base to give a mixture which comprises, as principal constituents, the (metal) salts of alkylphosphonous, phosphorous and hypophosphorous acids, b) esterifying the principal constituents of the mixture from a) to give an ester mixture, c) isolating the ester of the alkylphosphonous acid from the ester mixture, d) preparing the corresponding ester of the dialkylphosphinic acid from the ester of the alkylphosphonous acid by free-radical-initiated reaction with olefins, e) converting the ester of the dialkylphosphinic acid into the free acid or into the dialkylphosphinic acid salts of metals from groups IA, IIA, IIIA, IVA, VA, IIB, IVB, VIIB or VIIIB of the Periodic Table or of cerium. The invention likewise relates to the use of the dialkylphosphinic acids/salts prepared by this process for the preparation of various products, in particular flame retardants.
    • 本发明涉及一种制备二烷基次膦酸及其盐的方法,该方法包括:a)在碱存在下使元素黄磷与烷基化剂反应得到一种混合物,该混合物包含作为主要成分的烷基磷酸的(金属)盐 ,磷和次磷酸,b)从a)酯化混合物的主要成分得到酯混合物,c)从酯混合物中分离出烷基亚磷酸的酯,d)从相应的二烷基次膦酸的酯 通过与烯烃的自由基引发的反应,烷基亚磷酸的酯,e)将二烷基次膦酸的酯转化为游离酸或转化成IA,IIA,IIIA,IVA,VA,IIB族的金属的二烷基次膦酸盐, 周期表IVB,VIIB或VIIIB或铈。本发明同样涉及通过该方法制备的二烷基次膦酸/盐在p 各种产品的修补,特别是阻燃剂。