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    Method for producing silane
    7.
    发明授权
    Method for producing silane 失效
    硅烷的制造方法

    公开(公告)号：US06852301B2

    公开(公告)日：2005-02-08

    申请号：US10450207

    申请日：2001-11-21

    申请人： Hans-Dieter Block ,  Leslaw Mleczko ,  Andreas Bulan ,  Rainer Weber ,  Sigurd Buchholz ,  Torsten Sill

    发明人： Hans-Dieter Block ,  Leslaw Mleczko ,  Andreas Bulan ,  Rainer Weber ,  Sigurd Buchholz ,  Torsten Sill

    IPC分类号： C01B33/04 ,  C01B33/18

    CPC分类号： C01B33/046 ,  C01B33/043 ,  C01B33/18

    摘要： The invention relates to a method for producing silane (SiH4) by a) reacting metallurgical silicon with silicon tetrachloride (SiCl4) and hydrogen (H2), to form a crude gas stream containing trichlorosilane (SiHCl3) and silicon tetrachloride (SiCl4), b) removing impurities from the resulting crude gas stream by washing with condensed chlorosilanes, c) condensing and subsequently, separating the purified crude gas stream by distillation, d) returning the partial stream consisting essentially of SiCl4 to the reaction of metallurgical silicon with SiCl4 and H2, e) disproportionating the partial stream containing SiHCl3, to form SiCl4 and SiH4 and f) returning the SiH4 formed by disproportionation to the reaction of metallurgical silicon with SiCl4 and H2, the crude gas stream containing trichlorosilane and silicon tetrachloride being liberated from solids as far as possible by gas filtration before being washed with the condensed chlorosilanes. The washing process with the condensed chlorosilanes is carried out at a pressure of 25 to 40 bar and at a temperature of at least 150° C. in a single-stage distillation column and is carried out in such a way that 0.1 to 3 wt. % of the crude gas stream containing trichlorosilane and silicon tetrachloride is recovered in the form of a condensed liquid phase consisting essentially of SiCl4, this liquid phase then being removed from the SiCl4 circuit and expanded to a pressure of 1 bar outside said SiCl4 circuit and cooled to a temperature of 10 to 40° C., whereby dissolved impurities separate out and are then removed by filtration.

    摘要翻译： 本发明涉及一种通过以下步骤制备硅烷（SiH 4）的方法：a）使冶金硅与四氯化硅（SiCl 4）和氢（H 2）反应，形成含有三氯硅烷（SiHCl 3）和四氯化硅（SiCl 4）的粗气流，b） 通过用冷凝的氯硅烷洗涤从所得粗气流中除去杂质，c）冷凝并随后通过蒸馏分离纯化的粗气流，d）将基本上由SiCl 4组成的部分流返回到冶金硅与SiCl 4和H 2的反应中， e）歧化含SiHCl3的部分流，以形成SiCl4和SiH4，以及f）将通过歧化形成的SiH 4返回至冶金硅与SiCl4和H2的反应，将含有三氯硅烷和四氯化硅的粗气流从固体释放至 在用冷凝的氯硅烷洗涤之前可能通过气体过滤。 冷凝氯硅烷的洗涤过程在单级蒸馏塔中在25至40巴的压力和至少150℃的温度下进行，并以0.1至3重量％ 含有三氯硅烷和四氯化硅的粗气流的％以基本上由SiCl 4组成的冷凝液相的形式回收，然后将该液相从SiCl4回路除去并在SiCl 4回路外扩张至1巴的压力，并冷却 温度为10〜40℃，由此分离出溶解的杂质，然后通过过滤除去。

    Production of 2-phosphonobutane-1,2,4-tricarboxylic acid and the alkali metal salts thereof
    9.
    发明授权
    Production of 2-phosphonobutane-1,2,4-tricarboxylic acid and the alkali metal salts thereof 失效
    2-膦酰基丁烷-1,2,4-三羧酸及其碱金属盐的制备

    公开(公告)号：US5639909A

    公开(公告)日：1997-06-17

    申请号：US650681

    申请日：1996-05-20

    申请人： Christoph Holzner ,  Wolfgang Ohlendorf ,  Hans-Dieter Block ,  Horst Bertram ,  Roland Kleinstuck ,  Hans-Heinrich Moretto

    发明人： Christoph Holzner ,  Wolfgang Ohlendorf ,  Hans-Dieter Block ,  Horst Bertram ,  Roland Kleinstuck ,  Hans-Heinrich Moretto

    IPC分类号： C07F9/38 ,  C07F9/40

    CPC分类号： C07F9/3808 ,  C07F9/4006

    摘要： This invention relates to an improved process for the production of 2-phosphono-butane-1,2,4-tricarboxylic acid (PBTC) and the alkali metal salts thereof, in which process dialkyl phosphite, preferably dimethyl or diethyl phosphite, and ethene-1,2-dicarboxylic acid dialkyl ester, in particular the dimethyl or diethyl ester of maleic acid and/or fumaric acid, are initially reacted in the presence of a basic catalyst to yield a phosphonosuccinic acid tetraalkyl ester, the resultant ester is thereupon reacted without further working up with acrylic acid alkyl ester, preferably methyl or ethyl acrylate, in the presence of an alkaline catalyst and the reaction product obtained in this manner is saponified without further working up to yield PBTC or the alkali metal salts thereof. The product when mixed with bleaching lye exhibits reduced chlorine depletion.

    摘要翻译： 本发明涉及一种制备2-膦酰基 - 丁烷-1,2,4-三羧酸（PBTC）及其碱金属盐的改进方法，其中亚磷酸二烷基酯，优选亚磷酸二甲酯或二乙酯和乙烯 - 1,2-二羧酸二烷基酯，特别是马来酸和/或富马酸的二甲基酯或二乙酯，最初在碱性催化剂存在下反应，得到磷酸二琥珀酸四烷基酯，得到的酯随后反应而没有 进一步用丙烯酸烷基酯，优选丙烯酸甲酯或丙烯酸乙酯在碱性催化剂的存在下进行处理，将以这种方式获得的反应产物进行皂化而不进一步加工得到PBTC或其碱金属盐。 当与漂白碱液混合时，产品会减少氯的消耗。