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    VERFAHREN ZUR DESTILLATIVEN REINIGUNG VON EDA
    3.
    发明公开
    VERFAHREN ZUR DESTILLATIVEN REINIGUNG VON EDA 有权

    公开(公告)号：EP3116850A1

    公开(公告)日：2017-01-18

    申请号：EP15709173.7

    申请日：2015-03-11

    申请人： BASF SE

    发明人： LUYKEN, Hermann ,  JAEGLI, Stephanie ,  LORENZ, Michael ,  BRASCHE, Gordon ,  JEGELKA, Markus ,  BECKER, Barbara ,  BAUMANN, Robert ,  MELDER, Johann-Peter ,  BUSCHHAUS, Boris ,  KRUG, Thomas

    IPC分类号： C07C209/16 ,  C07C211/10 ,  C07C209/48 ,  C07C209/84 ,  C07C213/04 ,  C07C253/08 ,  C07C253/30

    CPC分类号： C07C209/84 ,  C07C209/16 ,  C07C209/48 ,  C07C213/04 ,  C07C253/08 ,  C07C253/30 ,  C07C211/10 ,  C07C255/16 ,  C07C255/25 ,  C07C215/08

    摘要： The invention relates to a method for the distillative purification of ethylenediamine (EDA), having the steps a) and b). In step a) a mixture (G1) containing water, EDA, and N-methyl ethylenediamine (N-MeEDA) is supplied into a distillation device (D1) from which the main quantity of the water contained in the mixture (G1) is separated via the head at a pressure of more than 4.8 barA. The water-depleted mixture (G2) is supplied from the sump of (D1) to a distillation device (D2) in step b), and the main quantity of N-MeEDA is distilled out via the head of (D2). The stream S3 obtained from the sump of (D2) contains EDA. The components of water and N-MeEDA contained in the mixture (G1) are largely or completely depleted. Optionally, additional distillation steps can be carried out in order to obtain pure EDA if additional diethylenetriamine (DETA) is contained in the mixture (G1) for example. As long as additional ammonia is contained in the mixture (G1), an ammonia separation process is additionally carried out in the method according to the invention preferably prior to carrying out step a).

    摘要翻译： 本发明涉及具有步骤a）和b）的乙二胺（EDA）蒸馏提纯方法。 在步骤a）中，将含有水，EDA和N-甲基乙二胺（N-MeEDA）的混合物（G1）供给到蒸馏装置（D1）中，混合物（G1）中所含的主要水分离 通过头部压力超过4.8巴。 在步骤b）中，从（D1）的贮槽向蒸馏装置（D2）供给贫水混合物（G2），通过（D2）的头蒸馏出主要量的N-MeEDA。 从（D2）的贮槽获得的流S3包含EDA。 包含在混合物（G1）中的水和N-MeEDA的组分大部分或完全耗尽。 任选地，如果在混合物（G1）中包含另外的二亚乙基三胺（DETA），则可以进行额外的蒸馏步骤以获得纯EDA。 只要混合物（G1）中含有另外的氨，在本发明的方法中，优选在进行步骤a）之前，另外进行氨分离处理。

    VERFAHREN ZUR SAUREN WÄSCHE VON DINITROTOLUOL IN GEGENWART VON BLAUSÄURE
    4.
    发明公开
    VERFAHREN ZUR SAUREN WÄSCHE VON DINITROTOLUOL IN GEGENWART VON BLAUSÄURE 有权
    VERFAHREN ZUR SAURENWÄSCHEVON DINITROTOLUOL在GEGENWART VONBLAUSÄURE

    公开(公告)号：EP3060543A1

    公开(公告)日：2016-08-31

    申请号：EP14786934.1

    申请日：2014-10-22

    申请人： BASF SE ,  Josef Meissner GmbH & Co. KG

    发明人： NETO, Samuel ,  FRITZ, Rüdiger ,  HEMPEL, Renate ,  ALLARDT, Holger ,  DAI, Yuanshen ,  BECKER, Barbara ,  AHRENS, Sebastian ,  LESCHINSKI, Julia ,  HERMANN, Heinrich ,  HÄNDEL, Mirko ,  PÖHLMANN, Jürgen

    IPC分类号： C07C201/16 ,  C07C205/06

    CPC分类号： C07C201/16 ,  B01D11/0488 ,  B01D11/0492 ,  B01D2011/002 ,  C02F1/20 ,  C02F1/26 ,  C02F3/00 ,  C02F2101/18 ,  C02F2103/36 ,  C07C205/06

    摘要： A process for scrubbing a crude mixture which is obtained in the nitration of toluene after separating off the nitrating acid and comprises dinitrotoluene, nitric acid, nitrogen oxides and sulfuric acid, which comprises two scrubbing steps (WS-I) and (WS II), wherein i) in a first scrubbing step (WS-I), the crude mixture is extracted with a scrubbing acid I comprising nitric acid, nitrogen oxides and sulfuric acid in a scrub comprising at least one extraction stage, where the scrubbing acid discharged from the first extraction stage (WS-I-1) of the first scrubbing step (WS-I) has a total acid content of from 10 to 40% by weight and a content of from 80 to 350 ppm of hydrocyanic acid, giving a prescrubbed crude mixture, ii) in a second scrubbing step (WS-II), the prescrubbed crude mixture comprising dinitrotoluene is extracted with a scrubbing acid II in a scrub comprising at least one, preferably at least 2, extraction stage(s), where the scrubbing acid discharged from the first extraction stage (WS-II-1) of the second scrubbing step (WS-II) has a pH of less than or equal to 4, giving a dinitrotoluene-comprising mixture which is essentially free of nitric acid, sulfuric acid, nitrogen oxides and hydrocyanic acid and has a content of not more than 300 ppm of nitric acid and nitrogen oxides, not more than 3 ppm of sulfate and not more than 50 ppm of hydrocyanic acid.

    摘要翻译： 分离出硝化酸后硝酸甲苯中得到的粗混合物的方法，包括二硝基甲苯，硝酸，氮氧化物和硫酸，其包括两个洗涤步骤（WS-I）和（WS-II） 其中i）在第一洗涤步骤（WS-1）中，所述粗混合物在包含至少一个萃取阶段的洗涤中用包含硝酸，氮氧化物和硫酸的洗涤酸I萃取，其中洗涤酸从 第一洗涤步骤（WS-1）的第一提取阶段（WS-I-1）的总酸含量为10至40重量％，含量为80至350ppm的氢氰酸，得到预先混合的粗品 混合物，ii）在第二次洗涤步骤（WS-II）中，包含二硝基甲苯的预混合粗混合物在洗涤中用洗涤酸II萃取，所述洗涤包括至少一个，优选至少2个萃取阶段，其中洗涤 酸从第一次提取出来 在第二洗涤步骤（WS-II）的阶段（WS-II-1）具有小于或等于4的pH，得到基本上不含硝酸，硫酸，氮氧化物的二硝基甲苯混合物， 氢氰酸，硝酸和氮氧化物含量不超过300ppm，硫酸盐不超过3ppm，氢氰酸不大于50ppm。

    VERFAHREN ZUR WÄSCHE VON DINITROTOLUOL
    9.
    发明公开
    VERFAHREN ZUR WÄSCHE VON DINITROTOLUOL 有权
    洗黑钱方法二硝基甲苯

    公开(公告)号：EP2841412A1

    公开(公告)日：2015-03-04

    申请号：EP13719491.6

    申请日：2013-04-24

    申请人： BASF SE ,  Josef Meissner GmbH & Co. KG

    发明人： NETO, Samuel ,  FRITZ, Rüdiger ,  HEMPEL, Renate ,  ALLARDT, Holger ,  BECKER, Barbara ,  LESCHINSKI, Julia ,  AHRENS, Sebastian ,  HAENDEL, Mirko ,  POEHLMANN, Juergen ,  HERMANN, Heinrich

    IPC分类号： C07C201/16

    CPC分类号： C07C201/16 ,  C07C205/06

    摘要： The invention relates to a method for washing a raw mixture that is produced during the nitration of toluene following separation of the nitrating acid, and that contains dinitrotoluene, nitric acid, nitrogen oxides and sulphuric acid. Said method comprises two washing steps (WS-1iI) and (WS-II) in which i) in a first washing step (WS-1i), the raw mixture is extracted in a wash comprising at least one extraction stage, using a wash acid I that contains nitric acid, nitrogen oxides and sulphuric acid, the wash acid discharged from the first extraction stage (WS-1-1) of the first washing step (WS-1) having a total acid content of 20 to 40 wt.%, and a prewashed raw mixture being obtained, and ii) in a second washing step (WS-II), the prewashed raw mixture containing dinitrotoluene is extracted in a wash comprising at least one extraction stage, using a wash acid II, the wash acid discharged from the first extraction stage (WS-II-1) of the second washing step (WS-II) having a pH value of less than or equal to 4, and a mixture that contains dinitrotoluene and is substantially devoid of nitric acid, sulphuric acid and nitrogen oxides being obtained.