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    Process for the preparation of naphthalene-1,3,6-trisulphonic acid
    1.
    发明授权
    Process for the preparation of naphthalene-1,3,6-trisulphonic acid 失效
    制备萘-1,3,6-三磺酸的方法

    公开(公告)号：US4180521A

    公开(公告)日：1979-12-25

    申请号：US886696

    申请日：1978-03-15

    申请人： Horst Behre ,  Rolf Putter ,  Guido Steffan

    发明人： Horst Behre ,  Rolf Putter ,  Guido Steffan

    IPC分类号： C07C309/35 ,  C07C20060101 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C143/30

    CPC分类号： C07C309/00

    摘要： A process has been invented for the preparation of naphthalene-1,3,6-trisulphonic acid by sulphonating naphthalene with sulphuric acid and oleum, characterized in that naphthalene and most of the oleum are simultaneously metered into sulphuric acid or oleum of low concentration, which has been initially introduced, at about 140.degree. to 240.degree. C., the temperature is kept at about 140.degree. to 240.degree. C. for some time, the remainder of the oleum is then added at about 140.degree. to 240.degree. C. and the mixture is then further stirred for some time.Naphthalene-1,3,6-trisulphonic acid is a known important intermediate used, for example, in the preparation of T-acid, H-acid and chromotropic acid.

    摘要翻译： 已经发明了通过用硫酸和发烟硫酸磺化萘来制备萘-1,3,6-三磺酸的方法，其特征在于萘和大多数发烟硫酸同时计量成低浓度的硫酸或发烟硫酸，其中 最初在约140℃至240℃下引入，温度保持在约140℃至240℃一段时间，然后在约140℃至240℃加入发烟硫酸的其余部分， 然后将混合物进一步搅拌一段时间。 萘-1,3,6-三磺酸是已知的重要中间体，例如用于制备T酸，H酸和变色酸。

    Process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid)
    2.
    发明授权
    Process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid) 失效
    制备3-硝基 - 萘-1,5-二磺酸镁盐（硝基 - 阿姆斯壮酸）的方法

    公开(公告)号：US4348334A

    公开(公告)日：1982-09-07

    申请号：US113412

    申请日：1980-01-18

    申请人： Bernhard Albrecht ,  Hans Frey ,  Vinzenz Habermacher ,  Horst Behre ,  Lutz Kienitz ,  Wolfgang Schenk ,  Guido Steffan ,  Axel Vogel

    发明人： Bernhard Albrecht ,  Hans Frey ,  Vinzenz Habermacher ,  Horst Behre ,  Lutz Kienitz ,  Wolfgang Schenk ,  Guido Steffan ,  Axel Vogel

    IPC分类号： C07C309/40 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C303/22 ,  C07C303/32 ,  C07C143/55

    CPC分类号： C07C309/00

    摘要： A process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid by sulfonating naphthalene, nitrating the sulfonation product, and separating the pure magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid, which process comprises:(a) sulfonating naphthalene with liquid SO.sub.3 in the presence of an inert organic solvent at temperatures between -40.degree. and +20.degree. C.;(b) adding to the reaction mixture obtained a mixture consisting of about equal parts of 100% sulfuric acid and fully reacted crude nitration mixture from nitration of a previous nitration charge, separating from the resulting two-phase system the upper organic solvent phase by decanting, and removing from the Armstrong's acid anhydride acid slurry the remainder of organic solvent by distillation, or removing it during or after subsequent nitration, subsequently adding to the residue the amount of nitric acid required for nitration, and then nitrating;(c) adding then firstly water and afterwards, in the absence of the inert organic solvent, at 90.degree. to 120.degree. C., a compound releasing magnesium ions, the amount being such that, per mol of 3-nitronaphthalene-1,5-disulfonic acid, 1.1 to 1.3 mols of magnesium ions are added, and a sulfuric acid concentration of between 40 and 60 percent by weight (relative to the sulfuric acid and water) is maintained; and(d) separating the crystallized magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid at a temperature of between 20.degree. and 70.degree. C., and subsequently optionally washing it with a maximum of 60 percent by weight of sulfuric acid and/or water, and optionally drying the product.

    摘要翻译： 通过磺化萘，硝化磺化产物和分离3-硝基萘-1,5-二磺酸的纯镁盐来生产3-硝基 - 萘-1,5-二磺酸的镁盐的方法，该方法包括 ：（a）在-40℃〜+ 20℃的温度下，在惰性有机溶剂的存在下，用液态SO 3磺化萘。 （b）向反应混合物中加入由约等量的100％硫酸组成的混合物和来自先前硝化装置的硝化的完全反应的粗硝化混合物，通过倾析从所得两相体系中分离出上部有机溶剂相 ，并通过蒸馏从阿姆斯壮的酸酐酸浆中除去剩余的有机溶剂，或者在后续硝化过程中或之后将其除去，随后向残余物中加入硝化所需的硝酸量，然后硝化; （c）然后首先加入水，然后在不存在惰性有机溶剂的情况下，在90〜120℃下，加入释放镁离子的化合物，其用量为每摩尔3-硝基萘-1,5 二磺酸，加入1.1〜1.3摩尔的镁离子，硫酸浓度保持在40〜60重量％之间（相对于硫酸和水）; 和（d）在20℃至70℃的温度下分离3-硝基萘-1,5-二磺酸的结晶镁盐，随后任选地用最多60重量％的硫酸洗涤， /或水，并任选地干燥产品。

    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid)
    5.
    发明授权
    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) 失效
    制备1-氨基-8-萘酚-3,6-二磺酸（H酸）的方法

    公开(公告)号：US4166826A

    公开(公告)日：1979-09-04

    申请号：US920032

    申请日：1978-06-28

    申请人： Willi Schossler ,  Rolf Putter ,  Horst Behre

    发明人： Willi Schossler ,  Rolf Putter ,  Horst Behre

    IPC分类号： C07C309/50 ,  C07C67/00 ,  C07C301/00 ,  C07C303/22 ,  C07C303/32 ,  C07C143/66

    CPC分类号： C07C303/22

    摘要： A process has been invented for the preparation of a mono-alkali metal of 1-amino-8-naphthol-3,6-disulphonic acid, comprising reacting 1-naphthylamine-3,6,8-trisulphonic acid and/or a salt thereof and/or a naphthylamine trisulphonic acid isomer mixture and/or salt thereof with an alkali metal hydroxide solution in the presence of an alcohol and/or alcoholate and in the presence of a substance which contains at least one oxygen atom bonded to a nitrogen atom, at elevated pressure and elevated temperature, and separating out the mono-alkali metal salt of 1-amino-8-naphthol-3,6-disulphonic acid by acidification. The process results in the procurement of higher yields of the desired product and in the formation of less by-products.

    摘要翻译： 已经发明了一种制备1-氨基-8-萘酚-3,6-二磺酸的单碱金属的方法，包括1-萘胺-3,6,8-三磺酸和/或其盐 和/或萘胺三磺酸异构体混合物和/或其盐与碱金属氢氧化物溶液在醇和/或醇化物的存在下，在含有至少一个与氮原子键合的氧原子的物质存在下， 在升高的压力和升高的温度下，通过酸化分离出1-氨基-8-萘酚-3,6-二磺酸的单碱金属盐。 该过程导致采购更高产量的所需产品和形成较少的副产物。

    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid)
    6.
    发明授权
    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) 失效
    制备1-氨基-8-萘酚-3,6-二磺酸（H酸）的方法

    公开(公告)号：US4178308A

    公开(公告)日：1979-12-11

    申请号：US920033

    申请日：1978-06-28

    申请人： Willi Schossler ,  Horst Behre ,  Rolf Putter

    发明人： Willi Schossler ,  Horst Behre ,  Rolf Putter

    IPC分类号： C07C309/50 ,  C07C67/00 ,  C07C301/00 ,  C07C303/22 ,  C07C303/32 ,  C22B34/12 ,  H03D13/00 ,  C07C143/66

    CPC分类号： C22B34/12

    摘要： A process has been invented for the preparation of a mono-alkali metal salt of 1-amino-8-naphthol-3,6-disulphonic acid comprising reacting 1-naphthylamine-3,6,8-trisulphonic acid and/or a salt thereof and/or a naphthylamine-trisulphonic acid isomer mixture and/or salt thereof with an alkali metal hydroxide solution at elevated pressure and elevated temperature and in the presence of an alcohol or alcoholate, and separating out the mono-alkali metal salt by acidification. The process results in the procurement of higher yields of the desired product and in the formation of less by-products.

    摘要翻译： 已经发明了一种制备1-氨基-8-萘酚-3,6-二磺酸的单碱金属盐的方法，其包括使1-萘胺-3,6,8-三磺酸和/或其盐 和/或萘胺 - 三磺酸异构体混合物和/或其盐与碱金属氢氧化物溶液在升高的压力和升高的温度下，在醇或醇化物的存在下，通过酸化分离出单碱金属盐。 该过程导致采购更高产量的所需产品和形成较少的副产物。

    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid)
    8.
    发明授权
    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) 失效
    制备1-氨基-8-萘酚-3,6-二磺酸（H酸）的方法

    公开(公告)号：US4325889A

    公开(公告)日：1982-04-20

    申请号：US186884

    申请日：1980-09-12

    申请人： Horst Behre ,  Albert Hullen ,  Bruno Kruger ,  Guido Steffan

    发明人： Horst Behre ,  Albert Hullen ,  Bruno Kruger ,  Guido Steffan

    IPC分类号： C07C143/66

    摘要： The invention relates to a process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) as the mono-alkali metal salt from napthylamine-trisulphonic acid isomer mixtures by alkaline hydrolysis under pressure. The separation of the H-acid is effected by utilizing an aqueous sulphuric acid which contains naphthalene- and/or nitronaphthalene- and/or naphthylamine- and/or naphthol- and/or aminonaphthol-mono-, -di-and/or-tri-sulphonic acids.

    摘要翻译： 本发明涉及通过碱性水解在压力下从萘胺 - 三磺酸异构体混合物制备作为单碱金属盐的1-氨基-8-萘酚-3,6-二磺酸（H-酸）的方法。 H酸的分离是通过利用含有萘和/或硝基萘和/或萘胺和/或萘酚和/或氨基萘酚 - 单 - 和 - 或 - 三 - 磺酸。