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：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。