公开(公告)号：US20140039227A1

公开(公告)日：2014-02-06

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: C07C205/06

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：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。

公开(公告)号：US20190233364A1

公开(公告)日：2019-08-01

申请号：US16340593

申请日：2017-10-10

Applicant: BASF SE

Inventor： Armin LANGE DE OLIVEIRA ,  Barbara WUCHER ,  Christian BECHTOLD ,  Michael FRIKO ,  Renate HEMPEL

IPC: C07C209/36 ,  C07C211/50 ,  B01J23/89

CPC classification number: C07C209/36 ,  B01J23/892 ,  B01J2523/828 ,  B01J2523/847 ,  C07C209/82 ,  C07C211/50

Abstract: The present invention relates to a process for continuous hydrogenation of a nitro compound to the corresponding amine in a liquid reaction mixture comprising the nitro compound in the presence of a supported catalyst which comprises as the active component at least one element from groups 7 to 12 of the periodic table of the elements, wherein the hydrogenation is performed in the presence of at least one salt selected from the group consisting of the salts of the alkali metals, alkaline earth metals and of the rare earth metals and to a supported catalyst for continuous hydrogenation of a nitro compound to the corresponding amine in a liquid reaction mixture comprising the nitro compound which comprises as the active component at least one element from groups 7 to 12 of the periodic table of the elements and one salt of the alkali metals, alkaline earth metals or of the rare earth metals.

公开(公告)号：US20160194270A1

公开(公告)日：2016-07-07

申请号：US14916210

申请日：2014-09-01

Applicant: BASF SE

Inventor： Yuan Shen DAI ,  Katharina SPUHL ,  Renate HEMPEL

IPC: C07C201/16 ,  C07C201/08

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

Abstract: A process for the preparation of dintrotoluene which comprises (a) nitrating toluene with a nitrating acid, wherein said nitrating acid is a mixture of nitric acid and sulfuric acid, in one or more nitration steps, and separating the nitrating acid from the process stream thus formed, wherein a crude mixture comprising dinitrotoluene and a fraction of said nitrating acid dissolved therein is obtained, said crude mixture further comprising at least 50 ppm of HCN, and (b) washing the crude dinitrotoluene containing mixture in one or more washing steps, wherein, before the first washing step is carried out, the crude mixture is distilled and/or stripped to remove HCN therefrom, wherein a crude dinitrotoluene containing mixture which is essentially free of HCN is obtained.

Abstract translation: 一种制备二苯并芴的方法，其包括（a）在一个或多个硝化步骤中将硝酸与硝酸反应，其中所述硝酸是硝酸和硫酸的混合物，并将硝酸与工艺流分离，因此 形成，其中获得包含二硝基甲苯和所述硝酸的一部分溶解在其中的粗混合物，所述粗混合物还包含至少50ppm的HCN，和（b）在一个或多个洗涤步骤中洗涤含有二硝基甲苯的粗混合物，其中 ，在进行第一洗涤步骤之前，将粗混合物蒸馏和/或汽提以从其中除去HCN，其中获得基本上不含HCN的粗二硝基甲苯混合物。