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1. 发明授权

US06258986B1 Process for the production of dinitrotoluene 失效
标题翻译：生产二硝基甲苯的方法
公开(公告)号：US06258986B1
公开(公告)日：2001-07-10
申请号：US08511028
申请日：1995-08-03
申请人： Uwe Klingler , Thomas Schieb , Dietmar Wastian , Gerhard Wiechers , Jürgen Zimmerman
发明人： Uwe Klingler , Thomas Schieb , Dietmar Wastian , Gerhard Wiechers , Jürgen Zimmerman
IPC分类号： C07C20500
CPC分类号： C07C201/08 , C07C205/06
摘要： Dinitrotoluene is produced by nitrating toluene with nitrating acid under adiabatic conditions in a manner such that some mononitrotoluene is present in reaction mixture. The nitration reaction mixture is then treated to remove at least 5% by weight of water before the reaction mixture is separated into an acid phase and an organic phase. The product dinitrotoluene is recovered from the organic phase. The acid phase may be recycled after nitric acid has been added to replace that which was used in the nitration reaction.
摘要翻译：二硝基甲苯通过在绝热条件下以硝酸将硝酸甲苯以使得一些单硝基甲苯存在于反应混合物中的方式制备。然后处理硝化反应混合物以除去至少5重量％的水，然后将反应混合物分离成酸相和有机相。从有机相中回收产物二硝基甲苯。在添加硝酸后，酸相可以循环使用，以代替硝化反应中所用的酸相。

2. 发明授权

US5679873A Process for the production of dinitrotoluene 失效
标题翻译：生产二硝基甲苯的方法
公开(公告)号：US5679873A
公开(公告)日：1997-10-21
申请号：US510992
申请日：1995-08-03
申请人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers , Jurgen Zimmermann
发明人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers , Jurgen Zimmermann
IPC分类号： C07C201/08 , C07C201/16 , C07C205/06
CPC分类号： C07C201/08
摘要： Dinitrotoluene is produced in a two-stage process from toluene and nitric acid in the presence of sulfuric acid under adiabatic conditions in the presence of nitrating acids made up of specified components. The reaction product of the first phase is separated into an acid phase and an organic phase containing the mononitrotoluene. Some water is removed from the acid phase, nitric acid is added and the resultant mixture is recycled. The organic phase containing mononitrotoluene is further nitrated to produce the dinitrotoluene. This nitration mixture is also separated into an acid phase and an organic phase. The acid phase is treated to remove some water, nitric acid is added and the resultant acid mixture is recycled. Dinitrotoluene is recovered from the organic phase. This process is advantageous in that dilute nitric acid may be used and the heat of the nitration reaction is utilized.
摘要翻译：在绝酸条件下，在由特定组分组成的硝酸的存在下，在硫酸存在下，甲苯和硝酸二步法生产二硝基甲苯。将第一相的反应产物分离成酸相和含有一硝基甲苯的有机相。从酸相中除去一些水，加入硝酸并将所得混合物回收。含有单硝基甲苯的有机相进一步硝化以产生二硝基甲苯。该硝化混合物也分离成酸相和有机相。处理酸相以除去一些水，加入硝酸并将所得酸混合物再循环。从有机相回收二硝基甲苯。该方法的优点在于可以使用稀硝酸并利用硝化反应的热。

3. 发明授权

US5689018A Process for the production of dinitrotoluene 失效
标题翻译：生产二硝基甲苯的方法
公开(公告)号：US5689018A
公开(公告)日：1997-11-18
申请号：US510803
申请日：1995-08-03
申请人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers , Jurgen Zimmermann
发明人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers , Jurgen Zimmermann
IPC分类号： C07C201/08 , C07C201/16 , C07C205/06 , C07C205/00
CPC分类号： C07C201/08
摘要： Dinitrotoluene is produced from toluene and nitric acid in the presence of sulfuric acid in a two stage process in the first stage, toluene and nitric acid are reacted under isothermal conditions in amounts such that mononitrotoluene is produced. The reaction mixture is then separated into an organic phase and an acid phase. The organic phase is then further reacted with nitric acid under adiabatic conditions to produce dinitrotoluene. The reaction mixture is then separated into an organic phase and an acid phase. Dinitrotoluene is recovered from the organic phase. After at least 5% by weight water is removed from the acid phase and sufficient nitric acid to replace that consumed during the nitration reaction has been added, the acid phase may be recycled.
摘要翻译：二硝基甲苯在甲酸和硝酸的存在下，在第一阶段的两阶段工艺中由甲苯和硝酸制成，甲苯和硝酸在产生单硝基甲苯的条件下在等温条件下反应。然后将反应混合物分离成有机相和酸相。然后在绝热条件下，有机相进一步与硝酸反应生成二硝基甲苯。然后将反应混合物分离成有机相和酸相。从有机相回收二硝基甲苯。在从酸相中除去至少5重量％的水后，加入足够的硝酸代替在硝化反应期间消耗的硝酸，可以回收酸相。

4. 发明授权

US5616818A Process for the polynitration of aromatic compounds 失效
标题翻译：芳香族化合物多元化方法
公开(公告)号：US5616818A
公开(公告)日：1997-04-01
申请号：US543095
申请日：1995-10-13
申请人： Hans-Georg Pirkl , Reinhard Schom acker , Uwe Klingler , Thomas Schieb , Gerhard Wiechers , J urgen Zimmermann
发明人： Hans-Georg Pirkl , Reinhard Schom acker , Uwe Klingler , Thomas Schieb , Gerhard Wiechers , J urgen Zimmermann
IPC分类号： B01J10/00 , B01J14/00 , B01J19/24 , B01J19/26 , C07C201/08 , C07C205/06 , C07C205/12
CPC分类号： C07C201/08 , B01J10/002 , B01J14/00 , B01J19/0066 , B01J19/242 , B01J19/26 , B01J2219/00103 , B01J2219/00155 , B01J2219/00777 , B01J2219/185 , B01J2219/1943 , Y02P20/582
摘要： An aromatic compound is polynitrated in a continuous process in a single apparatus under adiabatic conditions in an emulsion as the reaction medium. From 1.3 to 3.5 mol of HNO.sub.3 per mol of aromatic compound are introduced in the form of a nitronium ion solution into the reactor with the aromatic compound under conditions such that an emulsion forms. The emulsion, which has a tendency to coalesce, is maintained by repeated dispersion. The first dispersion of the liquid streams to produce the emulsion takes place in less than one second. At least 20% of the total amount of HNO.sub.3 to be used should generally be present during this first dispersion. It is preferred, however, that the total amount of nitronium ion solution to be used be present at the time the aromatic compound and nitronium ion solution are first dispersed.
摘要翻译：芳族化合物在绝热条件下在单一设备中以乳液作为反应介质在连续方法中多次化。以硝酸离子溶液的形式，将1.3〜3.5mol的HNO 3 /芳族化合物以芳香族化合物的形式引入反应器中，形成乳状液。具有聚结倾向的乳液通过反复分散保持。液体流的第一种分散体产生乳液发生在不到一秒钟内。在第一次分散时，HNO3总量的至少20％一般应该存在。然而，优选在首先分散芳族化合物和硝鎓离子溶液时存在使用的硝鎓离子溶液的总量。

5. 发明授权

US5696305A Process for the production of nitroaromatic compounds 失效
标题翻译：制备硝基芳族化合物的方法
公开(公告)号：US5696305A
公开(公告)日：1997-12-09
申请号：US510888
申请日：1995-08-03
申请人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers , Jurgen Zimmermann
发明人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers , Jurgen Zimmermann
IPC分类号： C07C201/08 , C07C205/06 , C07C205/12
CPC分类号： C07C201/08
摘要： Nitroaromatic compounds are produced by continuously reacting an aromatic compound with nitrating acid. The reaction mixture is separated into an organic phase from which the desired nitroaromatic compound is recovered and an acid phase. The acid phase is subjected to flash evaporation to remove at least 5% by weight of the water present therein. The vapors generated during the flash evaporation are introduced into a jet spray of coolant to produce a condensate made up coolant, condensed vapors and suspended organic compounds. A portion of the condensate is subjected to phase separation to remove water and organic compounds present therein. The water and organic compounds may be reused. The process of the present invention is particularly advantageous in that deposits which block pipelines and interfere with heat transfer are not generated.
摘要翻译：硝基芳族化合物是通过使芳族化合物与硝酸进行连续反应来制备的。将反应混合物分离成有机相，从中回收所需的硝基芳族化合物和酸相。将酸相进行闪蒸以除去其中存在的至少5重量％的水。在闪蒸期间产生的蒸汽被引入冷却剂的喷射喷雾中以产生冷却剂，冷凝蒸汽和悬浮的有机化合物的冷凝物。将一部分冷凝物进行相分离以除去其中存在的水和有机化合物。水和有机化合物可以重复使用。本发明的方法特别有利的是不产生堵塞管道并干扰热传递的沉积物。

6. 发明授权

US5663462A Process for the production of dinitrotoluene and isomeric mixtures of dinitrotoluene 失效
标题翻译：制备二硝基甲苯和二硝基甲苯异构体混合物的方法
公开(公告)号：US5663462A
公开(公告)日：1997-09-02
申请号：US657513
申请日：1996-06-04
申请人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers
发明人： Uwe Klingler , Thomas Schieb , Gerhard Wiechers
IPC分类号： C07C201/08 , C07C201/16 , C07C205/06
CPC分类号： C07C201/08
摘要： Dinitrotoluene and isomer mixtures of dinitrotoluene are produced in a single stage, continuous process by nitrating mononitrotoluene or an isomer mixture of mononitrotoluene in which the ortho-mononitrotoluene content is low with a nitrating acid made up of (1) from about 80 to about 100 wt. % inorganic constituents and (2) up to 20 wt. % organic constituents. The inorganic constituents of the nitrating acid include: (a) from about 60 to about 90 wt. % sulfuric acid, (b) from about 1 to about 20 wt. % nitric acid, and (c) at least 5 wt. % water. The organic constituents of the nitrating acid include: from about 70 to about 100% by weight nitrotoluene isomers and up to about 30% by weight nitration by-products. The nitration reaction is carrier out under adiabatic conditions. The molar ratio of nitric acid to mononitrotoluene during the nitration reaction is generally from about 0.7:1 to about 1.4:1. The phases generated during the nitration are subsequently separated and the acid phase is treated to remove at least 5 wt. % of the water present therein. The water may be removed by distillation or flash vaporization, optionally with simultaneous heat supply. After removal of the water, nitric acid having a concentration of from about 50 to about 100 wt. % is added to the treated acid phase in amount sufficient to satisfy the compositional limits for a nitrating acid useful in the process of the present invention. This reconcentrated acid phase is then returned to the nitration reaction.
摘要翻译：二硝基甲苯和二硝基甲苯的异构体混合物通过硝化单硝基甲苯或单硝基甲苯的异氰酸甲酯的异构体混合物在单一阶段中生产，其中邻硝基甲苯含量低于由（1）约80至约100重量％。％无机成分和（2）最多20重量％％有机成分。硝酸的无机组分包括：（a）约60至约90wt。％硫酸，（b）约1至约20wt。％硝酸，和（c）至少5wt。％水。硝酸的有机成分包括：约70至约100重量％的硝基甲苯异构体和至多约30重量％的硝化副产物。硝化反应在绝热条件下载运。在硝化反应期间硝酸与单硝基甲苯的摩尔比通常为约0.7:1至约1.4:1。随后分离硝化过程中产生的相，并处理酸相以除去至少5wt。存在于其中的水的百分比。水可以通过蒸馏或闪蒸除去，任选地同时供热。除去水后，浓度为约50至约100wt。以足以满足本发明方法中有用的硝酸的组成限度的量将经加入的酸相中的％加入到处理的酸相中。然后将该再浓缩的酸相返回到硝化反应。

7. 发明授权

US5345012A Process for the preparation of dinitrotoluene 失效
标题翻译：制备二硝基甲苯的方法
公开(公告)号：US5345012A
公开(公告)日：1994-09-06
申请号：US147654
申请日：1993-11-03
申请人： Thomas Schieb , Gerhard Wiechers , Rudolf Sundermann , Uwe Zarnack
发明人： Thomas Schieb , Gerhard Wiechers , Rudolf Sundermann , Uwe Zarnack
IPC分类号： C07C201/08 , C07C205/06
CPC分类号： C07C201/08
摘要： A continuous process for the preparation of isomeric mixtures of dinitrotoluene by a single stage nitration of toluene under adiabatic conditions. The reaction enthalpy is used for the removal by distillation of the water of reaction formed during nitration. In this process, toluene is reacted with a nitrating acid having from about 80 to about 100% by weight of an inorganic component having a specified composition and from about 0 to about 20% by weight of an organic component having a specified composition.
摘要翻译：在绝热条件下通过单阶段甲苯硝化甲苯制备二硝基甲苯的异构体混合物的连续方法。反应焓用于通过蒸馏除去硝化过程中形成的反应的水。在该方法中，甲苯与具有约80至约100重量％的具有指定组成的无机组分和约0至约20重量％的具有指定组成的有机组分的硝酸反应。

8. 发明授权

US5395995A Process for the preparation and purification of nitroaromatics 失效
标题翻译：硝基芳族化合物的制备和纯化方法
公开(公告)号：US5395995A
公开(公告)日：1995-03-07
申请号：US059783
申请日：1993-05-10
申请人： Dieter Grenner , Thomas Schieb , Gerhard Wiechers
发明人： Dieter Grenner , Thomas Schieb , Gerhard Wiechers
IPC分类号： C07C201/08 , C07C201/16 , C07C205/06
CPC分类号： C07C201/16 , C07C201/08
摘要： A process for the preparation and purification of nitroaromatics by nitration of the corresponding aromatics and subsequent melt crystallization. The residual melts which occur are recycled.
摘要翻译：通过硝化相应的芳族化合物和随后的熔融结晶来制备和纯化硝基芳族化合物的方法。发生的残余熔体被回收。

9. 发明授权

US07495136B2 Process for the production of dinitrotoluene 失效
标题翻译：生产二硝基甲苯的方法
公开(公告)号：US07495136B2
公开(公告)日：2009-02-24
申请号：US11827502
申请日：2007-07-12
申请人： Fritz Pohl , Wolfgang Lorenz , Juergen Muennig , Bernd Pennemann , Gerhard Wiechers
发明人： Fritz Pohl , Wolfgang Lorenz , Juergen Muennig , Bernd Pennemann , Gerhard Wiechers
IPC分类号： C07C205/00
CPC分类号： C07C201/08 , C07C205/06
摘要： Dinitrotoluene is produced by nitration of toluene with nitrating acid (mixture of nitric acid and sulfuric acid) in which, in a first stage, the toluene is converted to mononitrotoluene (MNT) and then the mononitrotoluene is converted in a second stage to dinitrotoluene (DNT). Control of the weight ratio of the aqueous to organic phases, dispersion of the organic phase in the aqueous phase and use of less than 2.06 moles of nitric acid per mole of toluene are key features of this process.
摘要翻译：二硝基甲苯通过用硝酸（硝酸和硫酸的混合物）硝化甲苯来制备，其中在第一阶段将甲苯转化为一硝基甲苯（MNT），然后将一硝基甲苯转化为二硝基甲苯（DNT ）。控制水相与有机相的重量比，有机相在水相中的分散和每摩尔甲苯使用小于2.06摩尔硝酸是该方法的关键特征。

10. 发明申请

US20080146847A1 Process for the preparation of toluenediamines by catalytic hydrogenation of dinitrotoluenes 有权
标题翻译：通过二硝基甲苯的催化氢化制备甲苯二胺的方法
公开(公告)号：US20080146847A1
公开(公告)日：2008-06-19
申请号：US12001879
申请日：2007-12-13
申请人： Fritz Pohl , Wolfgang Lorenz , Lars Padeken , Bernd Pennemann , Friedhelm Steffens , Gerhard Wiechers
发明人： Fritz Pohl , Wolfgang Lorenz , Lars Padeken , Bernd Pennemann , Friedhelm Steffens , Gerhard Wiechers
IPC分类号： C07C209/36
CPC分类号： C07C209/36 , C07C211/50
摘要： The present invention relates to a process for the preparation of toluenediamine, in which dinitrotoluene is reacted with hydrogen in the presence of a catalyst. The dinitrotoluene required by this process has a content of carbon dioxide, in either physically dissolved or chemically bonded form, of not more than 0.175 mol %, based on the molar amount of the dinitrotoluene.
摘要翻译：本发明涉及一种制备甲苯二胺的方法，其中二硝基甲苯与氢气在催化剂存在下反应。该方法所需的二硝基甲苯的物理溶解或化学键合形式的二氧化碳含量以二硝基甲苯的摩尔量计不超过0.175mol％。

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