公开(公告)号：US12221402B2

公开(公告)日：2025-02-11

申请号：US17436293

申请日：2020-02-26

Applicant: BASF SE

Inventor： Barbara Becker ,  Thomas Heidemann ,  Regine Helga Bebensee ,  Eva Koch ,  Johann-Peter Melder ,  Hermann Luyken ,  Claudia Oezkozanoglu ,  Jens Kehrer

IPC: C07C209/16 ,  B01J21/04 ,  B01J23/89 ,  B01J37/00 ,  B01J37/02 ,  B01J37/03 ,  B01J37/04 ,  B01J37/08 ,  B01J37/16

Abstract: The present invention relates to a process for preparing alkanolamines and ethyleneamines in the liquid phase, by reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst which is obtained by reducing a catalyst precursor, wherein the preparation of the catalyst precursor comprises a step a) in which a catalyst precursor comprising one or more catalytically active components of Sn, Cu and Ni, and a step b) in which the catalyst precursor prepared in step a) is contacted with a soluble Re compound.

公开(公告)号：US09687838B2

公开(公告)日：2017-06-27

申请号：US14899444

申请日：2014-06-17

Applicant: BASF SE ,  DOW GLOBAL TECHNOLOGIES LLC

Inventor： Thomas Heidemann ,  Barbara Becker

IPC: C07C29/00 ,  B01J23/00 ,  B01J38/48 ,  B01J38/02 ,  B01J38/60 ,  B01J38/62 ,  B01J38/64 ,  B01J38/66 ,  B01J23/96 ,  C07C29/157 ,  B01J23/44 ,  C07C29/132

CPC classification number: B01J38/48 ,  B01J23/44 ,  B01J23/96 ,  B01J38/02 ,  B01J38/60 ,  B01J38/62 ,  B01J38/64 ,  B01J38/66 ,  C07C29/132 ,  C07C29/157 ,  Y02P20/584 ,  C07C31/205

Abstract: A process for the regeneration of a supported noble metal catalyst comprising contacting the catalyst with a liquid aqueous system at a temperature in the range of from 90 to 160° C., wherein the pH of the aqueous system is outside the range of from 6 to 8, separating the aqueous system from catalyst; and subjecting the catalyst to calcination.

公开(公告)号：US09914693B2

公开(公告)日：2018-03-13

申请号：US14771409

申请日：2014-02-12

Applicant: BASF SE

Inventor： Hermann Luyken ,  Stephanie Jaegli ,  Michael Lorenz ,  Gordon Brasche ,  Markus Jegelka ,  Barbara Becker ,  Robert Baumann ,  Johann-Peter Melder ,  Boris Buschhaus ,  Thomas Krug

IPC: C07C209/48 ,  C07C253/00 ,  C07C253/30 ,  C07C209/86 ,  C07C253/08

CPC classification number: C07C209/48 ,  C07C209/86 ,  C07C253/00 ,  C07C253/08 ,  C07C253/30 ,  C07C255/12 ,  C07C255/25 ,  C07C211/10

Abstract: The present invention relates to a process for preparing ethylenediamine (EDA), where the process comprises the steps a) to c). In step a), formaldehyde is reacted with hydrocyanic acid (HCN) to form formaldehyde cyanohydrin (FACH), where the hydrocyanic acid is completely free or largely free of sulfur dioxide (SO2). The FACH prepared in this way is reacted with ammonia (NH3) to form aminoacetonitrile (AAN) in step b), whereupon a hydrogenation of AAN in the presence of a catalyst to form EDA is carried out in step c).

公开(公告)号：US11214535B2

公开(公告)日：2022-01-04

申请号：US16619987

申请日：2018-05-24

Applicant: BASF SE

Inventor： Regine Helga Bebensee ,  Thomas Heidemann ,  Barbara Becker ,  Eva Koch ,  Hermann Luyken ,  Johann-Peter Melder

IPC: C07C215/08 ,  B01J23/46 ,  B01J23/75 ,  B01J8/24 ,  B01J8/18 ,  B01J21/02 ,  B01J21/06

Abstract: The invention relates to processes for preparing alkanolamines and ethyleneamines in the liquid phase, by reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst comprising one or more active metals selected from Sn and the elements of groups 8, 9, 10 and 11 of the Periodic Table of the Elements, wherein the amination catalyst is obtained by reductive calcination of a catalyst precursor. The catalyst precursor here is preferably prepared by contacting a conventional or catalytic support material with one or more soluble compounds of the active metals and optionally one or more soluble compounds of added catalyst elements. The present invention further relates to a process for preparing an amination catalyst comprising one or more active metals selected from Sn and the elements of groups 8, 9, 10 and 11 of the Periodic Table of the Elements, the amination catalyst being obtained by reductive calcination of a catalyst precursor, wherein the reactor in which the catalyst precursor is reductively calcined is connected to a denox plant, and to the use of a denox plant in the preparation of amination catalysts.

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：US11208373B2

公开(公告)日：2021-12-28

申请号：US16619976

申请日：2018-05-24

Applicant: BASF SE

Inventor： Thomas Heidemann ,  Barbara Becker ,  Eva Koch ,  Johann-Peter Melder ,  Hermann Luyken

IPC: C07C209/16 ,  B01J23/89 ,  B01J21/04 ,  B01J21/06 ,  B01J35/02 ,  B01J37/02 ,  B01J37/08

Abstract: The present invention relates to a process for preparing alkanolamines and/or ethyleneamines in the liquid phase, by reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst comprising Co, Ru and Sn.

公开(公告)号：US09828329B2

公开(公告)日：2017-11-28

申请号：US15125850

申请日：2015-03-11

Applicant: BASF SE

Inventor： Hermann Luyken ,  Stephanie Jaegli ,  Michael Lorenz ,  Gordon Brasche ,  Markus Jegelka ,  Barbara Becker ,  Robert Baumann ,  Johann-Peter Melder ,  Boris Buschhaus ,  Thomas Krug

IPC: C07C209/84

CPC classification number: C07C209/84 ,  C07C209/16 ,  C07C209/48 ,  C07C213/04 ,  C07C253/08 ,  C07C253/30 ,  C07C211/10 ,  C07C255/16 ,  C07C255/25 ,  C07C215/08

Abstract: The present invention relates to a process for purifying ethylenediamine (EDA) by distillation, wherein the process comprises the steps a) and b). In step a), a mixture (G1) comprising water, EDA and N-methylethylenediamine (N-MeEDA) is fed into a distillation apparatus (D1), and the major part of the water comprised in the mixture (G1) is separated off overhead at a pressure of greater than 4.8 bara. From the bottom of (D1), the water-enriched mixture (G2) is fed into a distillation apparatus (D2) in step b). At the top of (D2), the major part of the N-MeEDA is distilled off. The stream (S3) obtained from the bottom of (D2) comprises EDA, with the components water and N-MeEDA comprised in the mixture (G1) having been largely or completely removed. Further distillation steps can optionally be carried out in order to obtain pure EDA, for example when diethylenetriamine (DETA) is additionally comprised in the mixture (G1). If ammonia is additionally comprised in the mixture (G1), an ammonia removal is preferably additionally carried out before carrying out the step a) in the process of the invention.

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。