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    • 4. 发明授权
    • Exhaust gas cleaning in a method for continuously producing dinitrotoluene
    • US09896407B2
    • 2018-02-20
    • US15514107
    • 2015-09-29
    • Covestro Deutschland AG
    • Thomas KnaufJürgen MünnigWolfgang LorenzBernd Pennemann
    • C07C201/08C07C201/16C07C205/06B01D53/00
    • C07C201/08B01D53/002B01D2257/7027C07C201/16C07C205/06
    • 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 %.
    • 5. 发明申请
    • EXHAUST GAS CLEANING IN A METHOD FOR CONTINUOUSLY PRODUCING DINITROTOLUENE
    • US20170291869A1
    • 2017-10-12
    • US15514107
    • 2015-09-29
    • Covestro Deutschland AG
    • Thomas KNAUFJürgen MÜNNIGWolfgang LORENZBernd PENNEMANN
    • C07C201/08C07C201/16B01D53/00
    • C07C201/08B01D53/002B01D2257/7027C07C201/16C07C205/06
    • 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 %.
    • 8. 发明申请
    • PROCESS FOR ACIDIC SCRUBBING OF DINITROTOLUENE IN THE PRESENCE OF HYDROCYANIC ACID
    • 氨基酸在酸性酸存在下的酸洗过程
    • US20160251302A1
    • 2016-09-01
    • US15031100
    • 2014-10-22
    • BASF SEJOSEF MEISSNER GMBH & CO. KG
    • SAMUEL NETORüdiger FRITZRenate HEMPELHolger ALLARDTYuan Shen DAIBarbara BECKERSebastian AHRENSJulia LESCHINSKIHenrich HERMANNMirko HAENDELJürgen PÖHLMANN
    • C07C201/16C02F1/26C02F1/20B01D11/04C02F3/00
    • C07C201/16B01D11/0488B01D11/0492B01D2011/002C02F1/20C02F1/26C02F3/00C02F2101/18C02F2103/36C07C205/06
    • 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.
    • 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。
    • 10. 发明授权
    • Process for the production of nitrobenzene by adiabatic nitration
    • 通过绝热硝化生产硝基苯的方法
    • US09284256B2
    • 2016-03-15
    • US14415794
    • 2013-07-23
    • Bayer MaterialScience AG
    • Thomas KnaufMichael Merkel
    • C07C201/00C07C201/08C07C201/16
    • C07C201/08C07C201/16C07C205/06
    • 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.
    • 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。