公开(公告)号：US09249083B2

公开(公告)日：2016-02-02

申请号：US13870506

申请日：2013-04-25

Applicant: BASF SE

Inventor： Samuel Neto ,  Ruediger Fritz ,  Renate Hempel ,  Holger Allardt ,  Barbara Becker ,  Julia Leschinski ,  Sebastian Ahrens ,  Heinrich Hermann ,  Mirko Haendel ,  Juergen Poehlmann

IPC: C07C205/00 ,  C07C201/00 ,  C07C205/06 ,  C07C201/06

CPC classification number: C07C205/06 ,  C07C201/06

Abstract: The invention relates to a process for scrubbing a crude mixture comprising dinitrotoluene, nitric acid, nitrogen oxides and sulfuric acid obtained in the nitration of toluene after the nitrating acid has been separated off, which comprises two scrubbing steps (SS-I) and (SS-II), wherein i) in a first scrubbing step (SS-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 (SS-I-1) of the first scrubbing step (SS-I) has a total acid content of from 20 to 40% by weight and a prescrubbed crude mixture is obtained, ii) in a second scrubbing step (SS-II), the prescrubbed crude mixture comprising dinitrotoluene is extracted with a scrubbing acid II in a scrub comprising at least one extraction stage, where the scrubbing acid discharged from the first extraction stage (SS-II-1) of the second scrubbing step (SS-II) has a pH of less than or equal to 4 and a mixture comprising dinitrotoluene which is essentially free of nitric acid, sulfuric acid and nitrogen oxides is obtained.

Abstract translation: 本发明涉及一种在分离出硝化酸后，除去包含二硝基甲苯，硝酸，氮氧化物和硫酸在硝化硝酸中得到的粗混合物的方法，该方法包括两个洗涤步骤（SS-I）和（SS -II），其中i）在第一洗涤步骤（SS-1）中，粗制混合物用包含硝酸，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，其中洗涤 从第一洗涤步骤（SS-I）的第一提取阶段（SS-I-1）排出的酸的总酸含量为20至40重量％，得到预混合的粗混合物，ii）在第二次 洗涤步骤（SS-II），包含二硝基甲苯的预先混合的粗混合物在洗涤中用擦洗酸II萃取，其包含至少一个提取阶段，其中从第一提取阶段（SS-II-1）排出的洗涤酸 第二洗涤步骤（SS- II）具有小于或等于4的pH，并且获得基本上不含硝酸，硫酸和氮氧化物的二硝基甲苯的混合物。

公开(公告)号：US08895783B2

公开(公告)日：2014-11-25

申请号：US13759466

申请日：2013-02-05

Applicant: BASF SE

Inventor： Andreas Raichle ,  Stefanie Haase ,  Holgar Braunsberg ,  Johannes Buettner ,  Ulrich Penzel ,  Samuel Neto

IPC: C07C209/00 ,  C07C209/36

CPC classification number: C07C209/36 ,  C07C211/47 ,  C07C211/50

Abstract: The present invention relates to a continuous process for preparing at least one aromatic amine by hydrogenation of at least one nitroaromatic by means of hydrogen, where a liquid phase comprising at least the aromatic amine and a gas phase comprising at least hydrogen are present, in the presence of a catalyst suspended in the liquid phase at a temperature of from 50 to 250° C. and a pressure of from 5 to 50 bar, wherein the pressure in the reactor is kept essentially constant by continuous adaptation of the amount of hydrogen fed to the reactor, the total amount of hydrogen fed to the reactor is monitored and the introduction of the at least one nitroaromatic is interrupted if the hydrogen uptake in the reactor is not at least 50 mol % of the amount of hydrogen required for stoichiometric reaction of the at least one nitroaromatic to form the at least one aromatic amine.

Abstract translation: 本发明涉及通过氢气至少一种硝基芳族化合物来制备至少一种芳族胺的连续方法，其中至少包含芳族胺的液相和至少包含氢的气相存在于 在50至250℃的温度和5至50巴的压力下悬浮在液相中的催化剂的存在，其中反应器中的压力通过连续适应供给到 监测反应器中进料到反应器中的氢气总量，如果反应器中的氢气吸收量不是化学计量反应所需的氢量的至少50摩尔％，则至少一种硝基芳族化合物的引入被中断 至少一种硝基芳族化合物以形成所述至少一种芳族胺。

公开(公告)号：US09688606B2

公开(公告)日：2017-06-27

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 ,  C07C205/06 ,  B01D11/04 ,  C02F1/20 ,  C02F1/26 ,  C02F3/00 ,  B01D11/00 ,  C02F101/18 ,  C02F103/36

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), whereini) 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.

公开(公告)号：US09284257B2

公开(公告)日：2016-03-15

申请号：US14653687

申请日：2013-12-10

Applicant: BASF SE ,  SHANGHAI BASF POLYURETHANE COMPANY LIMITED

Inventor： Yuanshen Dai ,  Da Peng Li ,  Pei Shi Jia ,  Zhan Cai ,  Samuel Neto

IPC: C07C205/00 ,  C07C201/08

CPC classification number: C07C201/08 ,  B01D17/0217 ,  C07C201/16 ,  C07C205/06

Abstract: Proposed is a separation method in a toluene to dinitrotoluene process, wherein said method with a first process step comprising feeding a toluene comprising first stream (1) and a nitric acid comprising second stream (2) into a first reactor (R1), reacting of the toluene comprising first stream (1) and the nitric acid comprising second stream (2) within the first reactor (R1) to a first reaction mixture (3), said first reaction mixture (3) comprising a first liquid/liquid mixed phase of an acid phase and an organic phase comprising mononitrotoluene, feeding the first reaction mixture (3) into a first separation device (S1), separating the first reaction mixture (3) within the first separation device (S1) into a first forward stream (4) having a flow direction to a second process step and a first backward stream (5) having a flow direction back to the first reactor (R1), said method having a second process step comprising feeding the first forward stream (4) into a second reactor (R2), feeding a nitric acid comprising third stream (6) and a sulfuric acid comprising fourth stream (7) into the second reactor (R2), reacting of the first forward stream (4), the nitric acid comprising third stream (6) and the sulfuric acid comprising fourth stream (7) within the second reactor (R2) to a second reaction mixture (8), said second reaction mixture (8) comprising a second liquid/liquid mixed acid phase and an organic phase comprising mononitrotoluene and dinitrotoluene, feeding the second reaction mixture (8) into a second separation device (S2), separating the second reaction mixture (8) within the second separation device (S2) into a second forward stream (9) having a flow direction to a process output and a second backward stream (10) having a flow direction back to the first reactor (R1), wherein fine separating of at least one of the streams (4, 5, 9, 10) after the first separation step (S1) and/or the second separation step (S2) in a coalescer is carried out.

公开(公告)号：US09115049B2

公开(公告)日：2015-08-25

申请号：US14045940

申请日：2013-10-04

Applicant: BASF SE

Inventor： Koenraad Vandewalle ,  Karen Vercruysse ,  Leo Denissen ,  Filip Deberdt ,  Hendrik De Winne ,  Bart Van De Voorde ,  Michael Reiser ,  Samuel Neto

IPC: C07C209/00 ,  C07C209/36 ,  C07C209/84

CPC classification number: C07C209/36 ,  C07C209/84 ,  C07C211/46

Abstract: A process for obtaining pure aniline contains catalytically hydrogenating nitrobenzene, to obtain a reaction mixture, separating the reaction mixture into a gas phase containing hydrogen and a liquid phase, liquid/liquid phase separating the liquid phase to obtain an aqueous phase and also crude aniline containing water as an organic phase, distillatively pre-purifying the crude aniline by removing the water via an overhead stream of a first distillation column to obtain a first bottom stream, feeding the first bottom stream as a feed stream to a pure column from which a pure aniline stream is taken off at the top and a second bottom stream containing high boilers is taken off, and passing the second bottom stream to incineration, by pumping the second bottom stream through heated pipelines and by adding methanol, ethanol, propanol, and/or acetone to the second bottom stream.

Abstract translation: 获得纯苯胺的方法含有催化氢化硝基苯，得到反应混合物，将反应混合物分离成含有氢和液相的气相，液/液相分离液相，得到含水相和粗苯胺 水作为有机相，通过经由第一蒸馏塔的塔顶流除去水来蒸馏预纯化粗苯胺，以获得第一底部料流，将第一底部料流作为进料流进料至纯的塔，纯纯 将苯胺流从顶部取出，取出含有高锅炉的第二塔底物流，并将第二塔底物流通过加热的管道，并通过加入甲醇，乙醇，丙醇和/或 丙酮到第二个底部流。