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    Exhaust gas cleaning in a method for continuously producing dinitrotoluene
    294.
    发明授权
    Exhaust gas cleaning in a method for continuously producing dinitrotoluene 有权

    公开(公告)号：US09896407B2

    公开(公告)日：2018-02-20

    申请号：US15514107

    申请日：2015-09-29

    Applicant: Covestro Deutschland AG

    Inventor： Thomas Knauf ,  Jürgen Münnig ,  Wolfgang Lorenz ,  Bernd Pennemann

    IPC: C07C201/08 ,  C07C201/16 ,  C07C205/06 ,  B01D53/00

    CPC classification number: C07C201/08 ,  B01D53/002 ,  B01D2257/7027 ,  C07C201/16 ,  C07C205/06

    Abstract: The invention relates to a method for producing dinitrotoluene, comprising the following steps: a) nitrating toluene with a mixture of nitric acid and sulfuric acid and subsequently separating a sulfuric-acid-containing aqueous phase that arises in the nitration, wherein a raw dinitrotoluene is obtained, b) washing the raw dinitrotoluene in a water wash with neutral and/or alkaline washing water, wherein a pre-cleaned dinitrotoluene, which contains at least water in addition to dinitrotoluene, is obtained after the washing water used in the last wash has been separated, and c) separating the water from the pre-cleaned dinitrotoluene, d) collecting the waste water from steps a), b), and/or c), e) optionally extracting the collected waste water from step d) with toluene and returning the thus obtained organic phase to step a), f) freeing the collected waste water from step d), or, if the optional step e) is performed, the extracted waste water from step e), of toluene in a toluene stripper, wherein a toluene-containing exhaust gas flow is obtained, g) feeding at least one exhaust gas flow from steps a), b), c), d), e), or f) into an exhaust gas condenser and removing the toluene contained in the at least one exhaust gas flow in said exhaust gas condenser, wherein the method comprises the following further step: h) feeding the exhaust gas flow arising in step g) after the condensing out of the toluene to a thermal exhaust air cleaning, wherein nitrogen is added to the exhaust gas flow to be fed to the exhaust gas condenser or to the exhaust gas flow leaving the exhaust gas condenser, wherein preferably a nitrogen concentration in the exhaust gas flow of at least 0.1 vol % is set, especially preferably of at least 0.5 vol %.

    EXHAUST GAS CLEANING IN A METHOD FOR CONTINUOUSLY PRODUCING DINITROTOLUENE
    295.
    发明申请
    EXHAUST GAS CLEANING IN A METHOD FOR CONTINUOUSLY PRODUCING DINITROTOLUENE 有权

    公开(公告)号：US20170291869A1

    公开(公告)日：2017-10-12

    申请号：US15514107

    申请日：2015-09-29

    Applicant: Covestro Deutschland AG

    Inventor： Thomas KNAUF ,  Jürgen MÜNNIG ,  Wolfgang LORENZ ,  Bernd PENNEMANN

    IPC: C07C201/08 ,  C07C201/16 ,  B01D53/00

    CPC classification number: C07C201/08 ,  B01D53/002 ,  B01D2257/7027 ,  C07C201/16 ,  C07C205/06

    Abstract: The invention relates to a method for producing dinitrotoluene, comprising the following steps: a) nitrating toluene with a mixture of nitric acid and sulfuric acid and subsequently separating a sulfuric-acid-containing aqueous phase that arises in the nitration, wherein a raw dinitrotoluene is obtained, b) washing the raw dinitrotoluene in a water wash with neutral and/or alkaline washing water, wherein a pre-cleaned dinitrotoluene, which contains at least water in addition to dinitrotoluene, is obtained after the washing water used in the last wash has been separated, and c) separating the water from the pre-cleaned dinitrotoluene, d) collecting the waste water from steps a), b), and/or c), e) optionally extracting the collected waste water from step d) with toluene and returning the thus obtained organic phase to step a), f) freeing the collected waste water from step d), or, if the optional step e) is performed, the extracted waste water from step e), of toluene in a toluene stripper, wherein a toluene-containing exhaust gas flow is obtained, g) feeding at least one exhaust gas flow from steps a), b), c), d), e), or f) into an exhaust gas condenser and removing the toluene contained in the at least one exhaust gas flow in said exhaust gas condenser, wherein the method comprises the following further step: h) feeding the exhaust gas flow arising in step g) after the condensing out of the toluene to a thermal exhaust air cleaning, wherein nitrogen is added to the exhaust gas flow to be fed to the exhaust gas condenser or to the exhaust gas flow leaving the exhaust gas condenser, wherein preferably a nitrogen concentration in the exhaust gas flow of at least 0.1 vol % is set, especially preferably of at least 0.5 vol %.

    Method and apparatus for purifying nitration products
    297.
    发明授权
    Method and apparatus for purifying nitration products 有权
    净化硝化产物的方法和装置

    公开(公告)号：US09540313B2

    公开(公告)日：2017-01-10

    申请号：US14632086

    申请日：2015-02-26

    Applicant: JOSEF MEISSNER GMBH & CO. KG

    Inventor： Jürgen Pöhlmann ,  Heinrich Hermann ,  Mirko Händel ,  Jürgen Gebauer

    IPC: C07C201/16 ,  B01J19/24

    CPC classification number: C07C201/16 ,  B01J19/24 ,  B01J2219/24 ,  C07C205/06

    Abstract: The present invention relates to a method for removing impurities from nitrated crude products obtained during the nitration of nitratable aromatic compounds, after removal of the final nitrating acid, by treatment with a washing medium, and also to a plant or apparatus suitable for implementing this method. Further provided by the invention is a production plant for the nitration of nitratable aromatic compounds with subsequent purification of the nitrated products.

    Abstract translation: 本发明涉及一种从硝化硝化硝酸中除去硝化酸后，通过用洗涤介质处理而得到的硝化粗产物中除去杂质的方法，以及适用于实施该方法的设备或装置 。 本发明进一步提供了一种用于硝化硝化的芳族化合物的生产设备，随后硝化产物的纯化。

    PROCESS FOR ACIDIC SCRUBBING OF DINITROTOLUENE IN THE PRESENCE OF HYDROCYANIC ACID
    298.
    发明申请
    PROCESS FOR ACIDIC SCRUBBING OF DINITROTOLUENE IN THE PRESENCE OF HYDROCYANIC ACID 有权
    氨基酸在酸性酸存在下的酸洗过程

    公开(公告)号：US20160251302A1

    公开(公告)日：2016-09-01

    申请号：US15031100

    申请日：2014-10-22

    Applicant: BASF SE ,  JOSEF MEISSNER GMBH & CO. KG

    Inventor： SAMUEL NETO ,  Rüdiger FRITZ ,  Renate HEMPEL ,  Holger ALLARDT ,  Yuan Shen DAI ,  Barbara BECKER ,  Sebastian AHRENS ,  Julia LESCHINSKI ,  Henrich HERMANN ,  Mirko HAENDEL ,  Jürgen PÖHLMANN

    IPC: C07C201/16 ,  C02F1/26 ,  C02F1/20 ,  B01D11/04 ,  C02F3/00

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

    Abstract: 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: 在分离出硝酸后，除去硝化硝酸甲苯后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，所述粗混合物用包含硝酸，氮氧化物和硫酸的洗涤酸I在包含至少一个萃取阶段的洗涤中萃取，其中所述洗涤酸从 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，得到预先粗制的粗品 混合物，ii）在第二次洗涤步骤（WS-II）中，包含二硝基甲苯的预先混合的粗混合物用洗涤酸II在洗涤中提取，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）上具有小于或等于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。

    Process for the preparation of nitrobenzene by adiabatic nitration
    299.
    发明授权
    Process for the preparation of nitrobenzene by adiabatic nitration 有权
    通过绝热硝化制备硝基苯的方法

    公开(公告)号：US09302978B1

    公开(公告)日：2016-04-05

    申请号：US14785763

    申请日：2014-04-24

    Applicant: Covestro Deutschland AG

    Inventor： Antoni Mairata ,  Thomas Knauf

    IPC: C07C205/00 ,  C07C201/08 ,  C07C201/16

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

    Abstract: The present invention relates to a continuously operated adiabatic process for the preparation of nitrobenzene by nitration of benzene with nitric acid and sulfuric acid, in which the dilute sulfuric acid obtained after the nitration has taken place and the crude nitrobenzene has been separated off from the aqueous phase is concentrated for the purpose of re-use in the nitration, and after its concentration, at least one minute before it comes into contact with fresh nitric acid again an oxidizing agent is added such that a concentration of the oxidizing agent of from 10 ppm to 5,000 ppm, based on the total weight of the concentrated sulfuric acid to be recycled into the nitration, is established.

    Abstract translation: 本发明涉及用硝酸和硫酸硝化苯来制备硝基苯的连续操作的绝热方法，其中在硝化发生后获得的稀硫酸和粗硝基苯已从水溶液中分离出来 浓缩的浓度是为了在硝化中重复使用，并且在其浓缩之后，再次与新鲜硝酸接触至少一分钟，加入氧化剂使得氧化剂的浓度为10ppm 至5,000ppm，基于要再循环到硝化中的浓硫酸的总重量。

    Process for the production of nitrobenzene by adiabatic nitration
    300.
    发明授权
    Process for the production of nitrobenzene by adiabatic nitration 有权
    通过绝热硝化生产硝基苯的方法

    公开(公告)号：US09284256B2

    公开(公告)日：2016-03-15

    申请号：US14415794

    申请日：2013-07-23

    Applicant: Bayer MaterialScience AG

    Inventor： Thomas Knauf ,  Michael Merkel

    IPC: C07C201/00 ,  C07C201/08 ,  C07C201/16

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

    Abstract: The present invention provides a continuous process for the production of nitrobenzene by nitration of benzene with mixtures of sulfuric and nitric acid using a stoichiometric excess of benzene, in which the content of aliphatic organic compounds in the feed benzene during the start-up period of the production plant is always maintained at less than 1.5 wt. %, based on the total mass of the feed benzene. This is achieved either by mixing the feed benzene comprising recycled unreacted benzene (recycled benzene) and benzene newly supplied to the reaction (fresh benzene) in appropriate quantitative ratios during the start-up period, depending on the purity of the two streams, or by completely omitting the recycling of unreacted benzene during the start-up period, i.e. the feed benzene consists only of benzene newly supplied to the reaction.

    Abstract translation: 本发明提供了一种使用化学计量过量的苯硝化苯与硫酸和硝酸的混合物来生产硝基苯的连续方法，其中在起始时期的进料苯中的脂族有机化合物的含量 生产厂总是维持在1.5重量％以下。 ％，基于进料苯的总质量。 这可以通过在启动期间将包含再循环的未反应苯（再循环苯）和新提供给反应的苯（新鲜苯）的进料苯与合适的定量比例混合，取决于两个流的纯度，或者通过 在启动期间完全省略未反应苯的再循环，即进料苯仅由新提供给反应的苯组成。

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