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    VERFAHREN ZUR WÄSCHE VON DINITROTOLUOL
    12.
    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

    Applicant: BASF SE ,  Josef Meissner GmbH & Co. KG

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

    IPC: C07C201/16

    CPC classification number: C07C201/16 ,  C07C205/06

    Abstract: 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.

    VERFAHREN ZUR HERSTELLUNG VON TOLUYLENDIAMIN DURCH HYDRIERUNG VON DINITROTOLUOL
    15.
    发明公开
    VERFAHREN ZUR HERSTELLUNG VON TOLUYLENDIAMIN DURCH HYDRIERUNG VON DINITROTOLUOL 有权

    公开(公告)号：EP2571844A1

    公开(公告)日：2013-03-27

    申请号：EP11718109.9

    申请日：2011-05-09

    Applicant: BASF SE

    Inventor： RAICHLE, Andreas ,  COELHO TSOU, Joana ,  NETO, Samuel ,  PENZEL, Urlich ,  OEHLENSCHLÄGER, Steffen ,  ZÖLLINGER, Michael ,  BRAUNSBERG, Holgar ,  HAASE, Stefanie ,  BÜTTNER, Johannes

    IPC: C07C209/36 ,  C07C211/49

    CPC classification number: C07C209/36 ,  C07C211/50

    Abstract: The invention relates to a process for continuous preparation of tolylenediamine by liquid phase hydrogenation of dinitrotoluene with hydrogen in the presence of a suspended nickel-containing catalyst in a reactor with a product removal unit connected downstream of the reactor to obtain a product output from the reactor comprising a liquid phase containing tolylenediamine and dinitrotoluene in which the nickel-containing catalyst is suspended, wherein the concentration of dinitrotoluene in the liquid phase of the product output from the reactor in the region between the reactor and the downstream product removal unit is adjusted to a value in the range from 1 to 200 ppm by weight, based on the total weight of the liquid phase of the product output from the reactor.

    Abstract translation: 本发明涉及一种通过在反应器中悬浮的含镍催化剂存在下用氢气对二硝基甲苯进行液相氢化来连续制备甲苯二胺的方法，其中产物除去单元连接在反应器的下游，以获得反应器的产物 包括含有甲苯二胺和二硝基甲苯的液相，其中悬浮有含镍催化剂，其中在反应器和下游产物除去单元之间的区域中从反应器输出的产物的液相中二硝基甲苯的浓度被调节至 基于从反应器输出的产物的液相的总重量，重量在1至200重量ppm的范围内。

    VERFAHREN ZUR SAUREN WÄSCHE VON DINITROTOLUOL IN GEGENWART VON BLAUSÄURE
    18.
    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

    Applicant: BASF SE ,  Josef Meissner GmbH & Co. KG

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

    IPC: C07C201/16 ,  C07C205/06

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

    Abstract: 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.

    Abstract translation: 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。

    ÜBERWACHUNG DES STÖCHIOMETRISCHEN VERHÄLTNISSES BEI DER UMSETZUNG VON NITROAROMATEN MIT WASSERSTOFF
    19.
    发明公开
    ÜBERWACHUNG DES STÖCHIOMETRISCHEN VERHÄLTNISSES BEI DER UMSETZUNG VON NITROAROMATEN MIT WASSERSTOFF 有权
    监测的化学计量比在氢气硝基芳烃的执行情况

    公开(公告)号：EP2812308A1

    公开(公告)日：2014-12-17

    申请号：EP13702651.4

    申请日：2013-02-07

    Applicant: BASF SE

    Inventor： RAICHLE, Andreas ,  HAASE, Stefanie ,  BRAUNSBERG, Holgar ,  BÜTTNER, Johannes ,  PENZEL, Ulrich ,  NETO, Samuel

    IPC: C07C209/36

    CPC classification number: C07C209/36 ,  C07C211/47

    Abstract: The present invention relates to a continuous method for producing at least one aromatic amine by hydrogenation of at least one nitroaromatic with hydrogen, wherein a liquid phase containing at least the aromatic amine and a gaseous phase containing at least hydrogen are present, in the presence of a catalyst suspended in the liquid phase, at a temperature of 50-250°C and a pressure of 5-0 bar. The pressure in the reactor is held substantially constant by continuously adjusting the quantity of hydrogen supplied to the reactor, the total amount of hydrogen supplied to the reactor is monitored and the supply of the at least one nitroaromatic is interrupted if the hydrogen uptake of the reactor does not amount to at least 50 mol% of the hydrogen quantity required for stoichiometric reaction of the at least one nitroaromatic to form the at least one aromatic amine.

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