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1. 发明授权

US06278012B1 Process for preparing phosphinate esters 失效
标题翻译：制备次膦酸酯的方法
公开(公告)号：US06278012B1
公开(公告)日：2001-08-21
申请号：US09577465
申请日：2000-05-24
申请人： Sebastian Hörold , Norbert Weferling , Heinz-Peter Breuer , Martin Sicken
发明人： Sebastian Hörold , Norbert Weferling , Heinz-Peter Breuer , Martin Sicken
IPC分类号： C07F902
CPC分类号： C07F9/4816 , C07F9/3211
摘要： The present invention relates to a process for the preparation of phosphinic acid esters, 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) adding the resultant ester of the alkylphosphonous acid onto an olefin containing a functional group. The invention likewise relates to the use of the phosphinic acid esters prepared by this process, inter alia as flame retardants and precursors for further syntheses.
摘要翻译：本发明涉及一种制备次膦酸酯的方法，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，其中包含作为主要成分的烷基磷酸盐的（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）将得到的烷基亚磷酸酯加到烯烃上含有官能团。本发明同样涉及通过该方法制备的次膦酸酯的用途，特别是作为进一步合成的阻燃剂和前体。

2. 发明授权

US06855757B2 Preparation of glycol carboxyethylmethylphosphinate 失效
标题翻译：乙二醇羧乙基甲基次膦酸盐的制备
公开(公告)号：US06855757B2
公开(公告)日：2005-02-15
申请号：US10283909
申请日：2002-10-30
申请人： Sebastian Hörold , Heinz-Peter Breuer , Elisabeth Jung
发明人： Sebastian Hörold , Heinz-Peter Breuer , Elisabeth Jung
IPC分类号： C09K21/12 , C07F9/32 , C08K5/5313 , C08K5/51 , C08G63/18 , C08G63/19
CPC分类号： C08K5/5313 , C07F9/3211 , C07F9/3264
摘要： The invention relates to a process of preparing glycol carboxyethylmethylphosphinate, which comprises a) reacting elemental yellow phosphorus with methyl chloride in the presence of an alkali or alkaline earth metal hydroxide to form a mixture which includes the alkali and/or alkaline earth metal salts of methylphosphonous, phosphorous and hypophosphorous acids as main constituents, b) esterifying the methylphosphonous acid from the mixture obtained by a), c) removing the methylphosphonous ester from the mixture, d) adding the thus obtained methylphosphonous ester to an acrylic ester, e) hydrolyzing the diester thus obtained, f) esterifying the resulting carboxyethylmethylphosphinic acid with ethylene glycol directly to the glycol carboxyethylmethylphosphinate. The invention also relates to the use of the glycol carboxyethylmethylphosphinates prepared according to the invention as reactive flame retardants for polymers.
摘要翻译：本发明涉及一种制备二羧酸乙基甲基次膦酸二甲酯的方法，该方法包括：a）在碱金属或碱土金属氢氧化物存在下，使元素黄磷与氯甲烷反应形成一种混合物，该混合物包括甲基亚磷酸的碱金属和/或碱土金属盐，磷和次磷酸作为主要成分，b）从a）中得到的混合物中酯化甲基亚膦酸，c）从混合物中除去甲基亚膦酸酯，d）将得到的甲基亚膦酸酯加入到丙烯酸酯中，e）水解二酯 f）将得到的羧乙基甲基次膦酸与乙二醇直接酯化至二羧酸乙乙基甲基次膦酸酯。本发明还涉及根据本发明制备的二羧酸乙基甲基次膦酸酯作为聚合物的反应性阻燃剂。

3. 发明授权

US6090968A Process for preparing phosphinic esters 失效
标题翻译：制备次膦酸酯的方法
公开(公告)号：US6090968A
公开(公告)日：2000-07-18
申请号：US342772
申请日：1999-06-29
申请人： Sebastian Horold , Norbert Weferling , Heinz-Peter Breuer
发明人： Sebastian Horold , Norbert Weferling , Heinz-Peter Breuer
IPC分类号： B01J31/02 , C07B61/00 , C07F9/32 , C07F9/48 , C08G18/32 , C08K5/5313 , C08L33/00 , C09K21/12
CPC分类号： C09K21/12 , C07F9/3211 , C07F9/48 , C08K5/5313
摘要： The present invention relates to a process for preparing phosphinic esters which comprisesa) reacting elemental yellow phosphorus with alkyl halides in the presence of alkali metal hydroxide or alkaline earth metal hydroxide to form a mixture which comprises as main constituents the alkali metal salts and/or alkaline earth metal salts of alkylphosphonous acid, phosphorous acid and hypophosphorous acidb) removing the alkylphosphonous acid from the mixture obtained as described in a),c) esterifying the alkylphosphonous acid,d) adding the resultant ester of the alkylphosphonous acid to a compound having at least one C.dbd.C double bond.The invention likewise relates to the use of the phosphinic esters prepared by this process inter alia as flame retardants and as precursor for further syntheses.
摘要翻译：本发明涉及一种制备次膦酸酯的方法，该方法包括：a）在碱金属氢氧化物或碱土金属氢氧化物存在下使元素黄磷与烷基卤化物反应，形成一种混合物，该混合物包含作为主要成分的碱金属盐和/或 b）烷基亚磷酸，亚磷酸和次磷酸的碱土金属盐b）从如a）所述获得的混合物中除去烷基亚磷酸，c）酯化烷基亚磷酸，d）将得到的烷基亚磷酸酯加入到具有至少一个C = C双键。本发明同样涉及通过该方法制备的次膦酸酯作为阻燃剂和作为进一步合成的前体的用途。

4. 发明授权

US6090967A Process for preparing phosphonous esters 失效
标题翻译：膦酸酯的制备方法
公开(公告)号：US6090967A
公开(公告)日：2000-07-18
申请号：US342771
申请日：1999-06-29
申请人： Sebastian Horold , Norbert Weferling , Heinz-Peter Breuer
发明人： Sebastian Horold , Norbert Weferling , Heinz-Peter Breuer
IPC分类号： B01J31/02 , C07B61/00 , C07F9/48 , C07F9/28
CPC分类号： C07F9/48
摘要： The present invention relates to a process for preparing phosphonous esters which comprisesa) reacting elemental yellow phosphorus with alkyl halides in the presence of alkali metal hydroxides and/or alkaline earth metal hydroxides to form a mixture which comprises, as main components, the alkali metal salts and/or alkaline earth metal salts of the alkylphosphonous, phosphorous and hypophosphorous acids,b) removing the alkylphosphonous acid from the mixture obtained by a)c) esterifying the alkylphosphonous acid.The invention likewise relates to the use of the phosphonous esters prepared by this process.
摘要翻译：本发明涉及一种制备膦酸酯的方法，该方法包括：a）在碱金属氢氧化物和/或碱土金属氢氧化物存在下使元素黄磷与烷基卤化物反应，形成一种混合物，其中以碱金属烷基磷酸，磷酸和次磷酸的盐和/或碱土金属盐，b）通过a）c）酯化烷基亚磷酸得到的混合物中除去烷基亚磷酸。本发明同样涉及通过该方法制备的膦酸酯的用途。

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