Recovery of nitrating acid mixtures from nitration processes
    23.
    发明申请
    Recovery of nitrating acid mixtures from nitration processes 有权
    从硝化过程中回收硝酸混合物

    公开(公告)号:US20070088183A1

    公开(公告)日:2007-04-19

    申请号:US11581523

    申请日:2006-10-16

    CPC classification number: C07C201/16 C07C205/12 C07C205/06

    Abstract: The invention relates to a process for removing and recovering nitrating acid mixtures, in particular nitric acid, sulphuric acid and oxides of nitrogen, from the nitrated crude products occurring in the nitration of nitratable aromatic compounds after the nitrating acid has been separated off, by acidic scrubbing by means of a multistage extraction process, the extraction process comprising a cross-flow extraction with downstream countercurrent extraction. The process permits essentially complete recovery of the abovementioned acids, including the oxides of nitrogen, in high concentrations, so that they can be recycled to the nitration and no longer pollute the wastewater.

    Abstract translation: 本发明涉及一种从硝化酸分离后硝化酸性混合物,特别是硝酸,硫酸和氮氧化物的硝化粗产物硝化硝酸化硝酸的硝化产物中除去和回收的方法。 通过多级提取方法进行洗涤,提取方法包括具有下游逆流提取的交叉流提取。 该方法允许基本上完全回收上述酸,包括高浓度的氮氧化物,使得它们可以再循环到硝化中,并且不再污染废水。

    Process for the two-step production of dinitrotoluene
    24.
    发明授权
    Process for the two-step production of dinitrotoluene 有权
    两步生产二硝基甲苯的方法

    公开(公告)号:US06984762B2

    公开(公告)日:2006-01-10

    申请号:US10780266

    申请日:2004-02-17

    CPC classification number: C07C201/16 C07C201/08 C07C205/06

    Abstract: The invention relates to a process for the production of dinitrotoluene by the two-stage nitration of toluene. In the first stage of this process, toluene was reacted adiabatically with nitrating acid so that at least 90% of the toluene was reacted off and no more than 70% of the toluene formed dinitrotoluene. The resulting organic phase containing mononitrotoluene and the aqueous acid phase containing sulfuric acid were separated, and the aqueous acid phase containing sulfuric acid was concentrated by flash evaporation. The resulting concentrated sulfuric acid was recycled into the reaction in the first stage, and/or into the reaction in the second stage, and/or into the concentration in the second stage.In the second stage, the organic phase containing mononitrotoluene from the first stage was completely reacted isothermally with nitrating acid. The organic phase and the aqueous acid phase containing sulfuric acid were then separated, and the aqueous acid phase containing sulfuric acid was concentrated by vacuum evaporation. The resulting concentrated sulfuric acid was recycled into the reaction in the first stage and/or the second stage.

    Abstract translation: 本发明涉及通过甲苯二段硝化生产二硝基甲苯的方法。 在该方法的第一阶段,将甲苯与硝酸进行绝热反应,使得甲苯的至少90%反应,并且不超过70%的甲苯形成二硝基甲苯。 分离含有单硝基甲苯和含硫酸水相的所得有机相,通过闪蒸浓缩含硫酸水相。 将所得浓硫酸在第一阶段循环进入反应,和/或在第二阶段进入反应,和/或在第二阶段中浓缩。 在第二阶段,含有来自第一阶段的一硝基甲苯的有机相与硝酸一起等温共同反应。 然后分离含有硫酸的有机相和含水酸相,真空蒸发浓缩含硫酸的酸水溶液。 所得浓硫酸在第一阶段和/或第二阶段循环进入反应。

    Process for working up secondary components in the preparation of dinitrotoluene
    26.
    发明申请
    Process for working up secondary components in the preparation of dinitrotoluene 有权
    在制备二硝基甲苯时处理次要组分的方法

    公开(公告)号:US20040267062A1

    公开(公告)日:2004-12-30

    申请号:US10878079

    申请日:2004-06-28

    Abstract: The present invention relates to a process for working up organic secondary components which are formed in the one-stage or two-stage nitration of toluene to dinitrotoluene. These organic secondary components are present in the acidic and alkaline waste water from the dinitrotoluene washing step and in the aqueous distillate from the sulfuric acid concentration step, together with small amounts of mononitrotoluene and dinitrotoluene. This process comprises a) combining the acidic and alkaline waste waters from the washing step and the aqueous distillate from the sulfuric acid concentration step such that the resulting mixture has a pH below 5, b) separating the aqueous and organic phases which form by phase separation, and c) recycling the organic phase from step b) into the nitration process.

    Abstract translation: 本发明涉及一种处理甲苯一硝基甲苯硝化成二硝基甲苯形成有机二次成分的方法。 这些有机次要组分存在于来自二硝基甲苯洗涤步骤的酸性和碱性废水中以及来自硫酸浓缩步骤的含水馏出物中,以及少量的一硝基甲苯和二硝基甲苯。 该方法包括:a)从硫酸浓缩步骤中将洗涤步骤的酸性和碱性废水与含水馏出物混合,使得所得混合物的pH值低于5,b)分离通过相分离形成的水相和有机相 ,和c)将来自步骤b)的有机相再循环到硝化过程中。

    Resolution of DL-racemic mixtures
    27.
    发明授权
    Resolution of DL-racemic mixtures 失效
    DL-外消旋混合物的拆分

    公开(公告)号:US06673942B1

    公开(公告)日:2004-01-06

    申请号:US10181411

    申请日:2002-07-23

    Abstract: The present invention relates to a process for the resolution of DL-racemic mixtures of compounds which crystalize in the form of a conglumerate. Both, the D and L-enantiomers are obtained according to the invention in a industrially feasable process by adding chiral enantioselective polymers to the supersaturated solution of the racemat to inhibit crystalization of one enantiomer. Next a DL-racemic mixture of said compound is suspended in about twice the amount of the crystallized enantiomer. Consequently, the opposite enantiomer could be recovered by said suspension by physical separation.

    Abstract translation: 本发明涉及一种分解化合物的DL-外消旋混合物的方法,所述化合物以共聚物的形式结晶。 根据本发明,在工业上可行的方法中,D和L-对映异构体都是通过向消旋体的过饱和溶液中加入手性对映选择性聚合物以抑制一种对映异构体的结晶而获得的。 接下来将所述化合物的DL-外消旋混合物悬浮在约两倍量的结晶对映异构体中。 因此,相反的对映异构体可以通过物理分离由所述悬浮液回收。

    Treatment/removal of byproduct aqueous effluents comprising
hydroxynitro-aromatic compounds
    29.
    发明授权
    Treatment/removal of byproduct aqueous effluents comprising hydroxynitro-aromatic compounds 失效
    包含羟基硝基芳族化合物的副产物含水废水的处理/除去

    公开(公告)号:US5820764A

    公开(公告)日:1998-10-13

    申请号:US959731

    申请日:1997-10-28

    CPC classification number: C02F1/66 C07C201/16 C02F2103/36 Y10S210/909

    Abstract: Objectionable byproduct aqueous effluents containing contaminating amounts of hydroxynitroaromatic compounds, in particular those aqueous effluents produced during the synthesis of nitroaromatic compounds, e.g., dinitrotoluenes, via reaction of an aromatic compound with nitric acid in the presence of sulfuric acid, are efficiently, facilely and economically treated/removed by (a) intimately contacting a mixture of at least one nitroaromatic compound and at least one hydroxynitroaromatic compound with an aqueous wash medium containing a neutralizing agent, (b) separating the resulting admixture into an organic phase and an aqueous phase, (c) recycling a fraction of the separated aqueous phase to the aqueous wash medium to thus constitute a portion thereof, and (d) periodically draining a fraction of the wash medium, whether to destruction thereof or to waste.

    Abstract translation: 含有污染量的羟基硝基芳族化合物的有害副产物含水废水,特别是在硫酸存在下通过芳族化合物与硝酸的反应合成硝基芳族化合物(例如二硝基甲苯)期间产生的含水废水,是有效,便利和经济的 通过(a)使至少一种硝基芳族化合物和至少一种羟基硝基芳族化合物的混合物与含有中和剂的水性洗涤介质紧密接触来处理/除去,(b)将所得混合物分离成有机相和水相( c)将分离的水相的一部分循环到水性洗涤介质中,从而构成其一部分,和(d)定期排出洗涤介质的一部分,不管其是否破坏或浪费。

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