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11. 发明授权

US4003924A Process for preparing 1-amino anthraquinone 失效
标题翻译： 1-氨基蒽醌的制备方法
公开(公告)号：US4003924A
公开(公告)日：1977-01-18
申请号：US546833
申请日：1975-02-03
申请人： Wolfgang Auge , Karl-Werner Thiem , Rutger Neeff , Paul Losacker , Rudolf Braden
发明人： Wolfgang Auge , Karl-Werner Thiem , Rutger Neeff , Paul Losacker , Rudolf Braden
IPC分类号： C09B1/22 , C07C20060101 , C07C225/34 , C07C97/24
CPC分类号： C07C225/34
摘要： 1-Amino anthraquinone is prepared by reacting 1-nitro-anthraquinone with ammonia in water and/or an organic solvent and thereafter treating the 1-amino-anthraquinone imine formed with water thereby converting said imine into 1-amino anthraquinone.
摘要翻译： 1-氨基蒽醌通过1-硝基 - 蒽醌与氨在水和/或有机溶剂中的反应制备，然后处理由水形成的1-氨基 - 蒽醌亚胺，从而将所述亚胺转化为1-氨基蒽醌。

12. 发明授权

US3996252A Preparation of pure 1,8-dinitroanthraquinone 失效
标题翻译：纯1,8-二硝基蒽醌的制备
公开(公告)号：US3996252A
公开(公告)日：1976-12-07
申请号：US672690
申请日：1976-04-01
申请人： Bernd Schroeder , Wolfgang Auge , Karl-Werner Thiem , Rutger Neeff
发明人： Bernd Schroeder , Wolfgang Auge , Karl-Werner Thiem , Rutger Neeff
IPC分类号： C07C205/47 , C07C20060101 , C07C67/00 , C07C201/00 , C09B1/00 , C07C79/37
CPC分类号： C07C225/34
摘要： A mixture of dinitroanthraquinones of which at least 70% is 1,8-dinitroanthraquinone is dissolved at elevated temperature in a halogenated aromatic hydrocarbon, a carboxylic acid nitrile or a cyclic sulphone and is thereafter cooled selectively to precipitate substantially pure 1,8-dinitroanthraquinone. Preferred solvents are 1-chloronaphthalene, sulpholane and adipic acid dinitrile. The particular temperature of dissolution and cooling will depend upon the particular solvent.
摘要翻译：其中至少70％为1,8-二硝基蒽醌的二硝基蒽醌的混合物在升高的温度下溶解在卤代芳族烃，羧酸腈或环状砜中，然后选择性地冷却以沉淀基本上纯的1,8-二硝基蒽醌。优选的溶剂是1-氯萘，环丁砜和己二酸二腈。溶解和冷却的特定温度将取决于具体的溶剂。

13. 发明授权

US4064147A Process for the production of aromatic mononitro compounds 失效
标题翻译：芳香族单硝基化合物的制备方法
公开(公告)号：US4064147A
公开(公告)日：1977-12-20
申请号：US685467
申请日：1976-05-12
申请人： Bernd Thelen , Wolfgang Auge , Karl-Werner Thiem
发明人： Bernd Thelen , Wolfgang Auge , Karl-Werner Thiem
IPC分类号： C07C205/05 , C07C67/00 , C07C201/00 , C07C201/08 , C07C205/06 , C07C205/12 , C07C205/47 , C07C49/68 , C07C79/10 , C07C79/12
CPC分类号： C07C201/08 , C07C2103/24
摘要： Aromatic mononitro compounds are prepared by nitrating aromatic compounds with nitric acid having a concentration between 70 and 100% by weight, working up of the nitration mixture in a rectification column and separation of the aromatic mononitro compound.In the nitration mixture and in the rectification column, depending upon the concentration of the nitric acid present, the ratio by weight of nitric acid plus water is controlled and not lowered below defined figures. Optionally water or nitric acid is introduced into the rectification column.BACKGROUND
摘要翻译：通过用浓度为70-100重量％的硝酸硝化芳族化合物，在精馏塔中处理硝化混合物并分离芳族单硝基化合物来制备芳族单硝基化合物。

14. 发明授权

US4261908A Process for isolating aromatic dinitro compounds 失效
标题翻译：芳族二硝基化合物的分离方法
公开(公告)号：US4261908A
公开(公告)日：1981-04-14
申请号：US50905
申请日：1979-06-21
申请人： Bernd Schroeder , Bernd Thelen , Wolfgang Auge , Karl-Werner Thiem
发明人： Bernd Schroeder , Bernd Thelen , Wolfgang Auge , Karl-Werner Thiem
IPC分类号： C07C67/00 , C07C201/00 , C07C201/16 , C07C205/06 , C07C205/47 , C07C50/18 , C07C79/10
CPC分类号： C07C201/16
摘要： A process has been developed for isolating aromatic dinitro compounds by using nitric acid in specified concentrations in different portions of a rectifying column and separating off the mixture of aromatic dinitro compounds from the sump of the rectifying column.
摘要翻译：已经开发了一种通过在精馏塔的不同部分使用特定浓度的硝酸并从精馏塔的贮槽中分离出芳族二硝基化合物的混合物来分离芳族二硝基化合物的方法。

15. 发明授权

US4141799A Process for the purification of high-melting organic products 失效
标题翻译：纯化高熔点有机产品的方法
公开(公告)号：US4141799A
公开(公告)日：1979-02-27
申请号：US824198
申请日：1977-08-12
申请人： Bernd Thelen , Hans-Walter Brandt , Wolfgang Auge , Karl-Werner Thiem
发明人： Bernd Thelen , Hans-Walter Brandt , Wolfgang Auge , Karl-Werner Thiem
IPC分类号： C07C46/10 , B01D20060101 , B01D1/22 , B01D3/00 , B01D3/14 , C07B31/00 , C07B63/00 , C07C45/00 , C07C50/18 , C07C50/20 , C07C50/34 , C07C67/00 , C07C201/00 , C07C205/47 , C07C225/34
摘要： The purification of high-melting organic products, such an anthraquinone and substituted anthraquinones, which is substantially free from lower-boiling impurities, by melting the product to be purified by heating, while mechanically conveying the same along a path with a screw conveyer, as for example, in a melting screw; degassing the melt at a reduced pressure in a column, as for example, at a pressure of 50 to 400 mm Hg; passing the degassed melt through a thin film evaporator at a reduced pressure of, for example, 5 to 250 mm Hg to evaporate the high-melting organic product and discharging the remaining high-boiling impurities and such impurities which are not capable of being distilled from the evaporator through a conically tapering sump, while mechanically scraping residue from the sump wall, preferably with the use of a rotating helical screw in the sump; the discharge from the sump being effected into and through an enclosed path at a rate sufficient to prevent liquid accumulating in the sump, while maintaining the central portion of the enclosed discharge path at a lower temperature than its end portion to form a crystal sludge in the central portion, which acts as a pressure seal; and solidifying and recovering the product discharging from the enclosed path. The enclosed path is preferably established through a screw-type pump which feeds into a crystallizing screw where the solidification takes place, the crystallizing screw being preferably maintained above the screw-type pump and is maintained filled with an amount of sump product which approximately corresponds to the amount of product in the sump take-off screw. The vapors produced in the thin film evaporator are passed via a heated rectifying column into a condenser, and a portion of the condensate is passed to the column as a reflux and another portion taken off and solidified in a crystallizing screw.
摘要翻译：通过将通过加热净化的产品熔化，同时用螺旋输送机沿着路径机械地输送，从而净化基本上不含低沸点杂质的高熔点有机产物，例如蒽醌和取代的蒽醌，作为例如，在熔化螺杆中; 例如在压力为50至400mm Hg的柱中，在减压下对熔体进行脱气; 将脱气的熔体通过薄膜蒸发器在例如5至250mm Hg的减压下通过，以蒸发高熔点有机产物并排出不能从蒸馏出的剩余的高沸点杂质和这些杂质蒸发器通过锥形锥形槽，同时机械地刮擦来自贮槽壁的残留物，优选地使用在贮槽中的旋转螺旋螺杆; 从贮槽中的排放物以足以防止液体积聚在贮槽中的速率进入并通过封闭路径，同时将封闭排放路径的中心部分保持在比其端部部分更低的温度，以在其中形成结晶污泥中心部分，用作压力密封; 并固化并回收从封闭路径排放的产品。封闭路径优选通过螺旋式泵来建立，所述螺旋式泵进料到结晶螺杆中，其中发生固化，结晶螺杆优选地保持在螺旋式泵上方，并且保持充满一定量的贮槽产品，其大致对应于产品的数量在油底壳起飞螺丝中。在薄膜蒸发器中产生的蒸汽通过加热的精馏塔进入冷凝器，一部分冷凝物作为回流通入塔中，另一部分在结晶螺杆中脱去固化。

16. 发明授权

US4112005A Process for the preparation of mononitro-aromatic compounds 失效
标题翻译：制备单硝基芳族化合物的方法
公开(公告)号：US4112005A
公开(公告)日：1978-09-05
申请号：US795249
申请日：1977-05-09
申请人： Karl-Werner Thiem , Adolf Hamers , Josef Heinen
发明人： Karl-Werner Thiem , Adolf Hamers , Josef Heinen
IPC分类号： C07C67/00 , C07C201/00 , C07C201/08 , C07C205/06 , C07C205/12 , C07C79/10 , C07C79/12
CPC分类号： C07C201/08 , Y02P20/582
摘要： The present invention relates to an improved continuous process for the preparation of mononitro-aromatic compounds which comprises (1) nitrating a reactive aromatic compound in the absence of sulphuric acid until mono-nitration is essentially complete, said nitration being carried out in 40 to 68% strength by weight nitric acid, (2) separating mechanically the nitration reaction mixture into an inorganic phase and an organic phase, (3) washing of the organic phase with water and dilute alkali solution and subsequent separation of the unconverted starting material end of the adhering water by means of rectification (4) feeding the inorganic phase and, if necessary, the wash water of the first water wash of the organic phase, to a rectification column in which (a) water is withdrawn over the top (b) optionally a fraction which has a lower nitric acid content than the feed is withdrawn from a sidestream takeoff in the rectifying section of the column and (c) a fraction which has a higher nitric acid content than the feed is taken off from the sump, (5) recycling said material withdrawn from the sump of the column to the nitration reaction vessel with the addition of fresh concentrated nitric acid and (6) withdrawing from the system an amount of the top product from the column which corresponds to the water of reaction and that which enters with the nitric acid that is added.
摘要翻译：本发明涉及一种用于制备单硝基芳族化合物的改进的连续方法，其包括（1）在不存在硫酸的情况下硝化反应性芳族化合物直到单硝化基本上完成，所述硝化在40至68 硝酸重量％，（2）将硝化反应混合物机械分离成无机相和有机相，（3）用水和稀碱溶液洗涤有机相，随后将未转化的原料末端分离通过精馏（4）将无机相和必要时将有机相的第一次水洗涤的洗涤水进料到精馏塔（1）将顶部（b）中的水排出任选地硝酸含量低于进料的馏分从柱的精馏段的侧流起飞中取出，（c）馏分具有较高的馏分硝酸含量比原料从油底壳中取出，（5）加入新鲜的浓硝酸使从塔的集油槽抽出的物料回收到硝化反应容器，（6）从系统中取出一定量的对应于反应水的塔的顶部产物和加入的硝酸进入的顶部产物。

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