公开(公告)号：US20160251302A1

公开(公告)日：2016-09-01

申请号：US15031100

申请日：2014-10-22

申请人： BASF SE ,  JOSEF MEISSNER GMBH & CO. KG

发明人： SAMUEL NETO ,  Rüdiger FRITZ ,  Renate HEMPEL ,  Holger ALLARDT ,  Yuan Shen DAI ,  Barbara BECKER ,  Sebastian AHRENS ,  Julia LESCHINSKI ,  Henrich HERMANN ,  Mirko HAENDEL ,  Jürgen PÖHLMANN

IPC分类号： C07C201/16 ,  C02F1/26 ,  C02F1/20 ,  B01D11/04 ,  C02F3/00

CPC分类号： C07C201/16 ,  B01D11/0488 ,  B01D11/0492 ,  B01D2011/002 ,  C02F1/20 ,  C02F1/26 ,  C02F3/00 ,  C02F2101/18 ,  C02F2103/36 ,  C07C205/06

摘要： 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.

摘要翻译： 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。