公开(公告)号：US09428441B2

公开(公告)日：2016-08-30

申请号：US14916210

申请日：2014-09-01

Applicant: BASF SE

Inventor： Yuan Shen Dai ,  Katharina Spuhl ,  Renate Hempel

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

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。

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.