公开(公告)号：DE10344282A1

公开(公告)日：2005-04-21

申请号：DE10344282

申请日：2003-09-24

Applicant: BASF AG

Inventor： REUTEMANN WERNER ,  WEBER THEODOR ,  ROS KARL-HEINZ ,  JULIUS MANFRED

IPC: C07C209/86 ,  C07C211/04

Abstract: The invention relates to a method of avoiding corrosion in the separation of methylamine from a product stream ( 10 ) which is obtained in the preparation of methylamines by gas-phase reaction of methanol and ammonia and includes monomethylamine, dimethylamine, trimethylamine, ammonia and methanol as components, where ammonia is separated off by pure distillation in a first column ( 1 ), the remaining components of the product stream obtained as bottoms ( 12 ) are fed to a second column ( 2 ). Trimethylamine ( 14 ) is separated off in the second column ( 2 ) by extractive distillation with introduction of water. The further components of the product stream obtained as bottoms ( 15 ) from the second column ( 2 ) are fed to a third column ( 3 ), in which monomethylamine and dimethylamine are separated off at the top. The monomethylamine and dimethylamine are separated by distillation in a fourth column ( 4 ). To avoid corrosion alkali metal hydroxide is added to the second or third column ( 3 ).

公开(公告)号：DE102004058888A1

公开(公告)日：2006-06-08

申请号：DE102004058888

申请日：2004-12-06

Applicant: BASF AG

Inventor： GRAFMANS HORST ,  MAAS STEFFEN ,  WECK ALEXANDER ,  RUETTER HEINZ ,  SCHULZ MICHAEL ,  ROS KARL-HEINZ

IPC: C07C231/02 ,  C07C233/05

公开(公告)号：DE10004909A1

公开(公告)日：2001-08-09

申请号：DE10004909

申请日：2000-02-04

Applicant: BASF AG

Inventor： OHLBACH FRANK ,  MELDER JOHANN-PETER ,  ROS KARL-HEINZ ,  RUDLOFF MARTIN ,  LIEBE JOERG

IPC: C07B61/00 ,  C07D207/26 ,  C07D207/267

Abstract: N-Methyl-2-pyrrolidone (NMP) is prepared by preparing a mixture comprising monomethylamine, dimethylamine and trimethylamine and ammonia in a first process step by reacting ammonia with methanol at elevated temperature in the presence of a catalyst, separating 10 off the ammonia, reacting the mixture comprising the methylamines with gamma-butyrolactone (gamma-BL), in a molar ratio of monomethylamine to gamma-BL of at least 1 in a second process step at elevated temperature and superatmospheric pressure, separating NMP and unreacted methylamines from the reaction product and returning unreacted methylamines to the first process step for reaction with methanol and ammonia.

公开(公告)号：DE102004058887A1

公开(公告)日：2006-06-08

申请号：DE102004058887

申请日：2004-12-06

Applicant: BASF AG

Inventor： GRAFMANS HORST ,  MAAS STEFFEN ,  WECK ALEXANDER ,  RUETTER HEINZ ,  SCHULZ MICHAEL ,  ROS KARL-HEINZ

IPC: C07C231/02 ,  C07C233/05

Abstract: A process for preparing N,N-dimethylacetamide (DMAC) by continuously reacting methyl acetate (MeOAc) with dimethylamine (DMA) in the presence of a basic catalyst, wherein MeOAc is used in the form of a methanolic solution and in the range from 0.0002 to 0.09 mol of catalyst per mole of MeOAc, and performing the reaction at a temperature in the range from 90 to 140° C. and at an absolute pressure in the range from 10 to 30 bar.

公开(公告)号：DE10344283A1

公开(公告)日：2005-04-21

申请号：DE10344283

申请日：2003-09-24

Applicant: BASF AG

Inventor： REUTEMANN WERNER ,  WAMBSGANS ROLF ,  POPLOW FRANK ,  WEBER THEODOR ,  ROS KARL-HEINZ ,  JULIUS MANFRED

IPC: C07C209/16 ,  C07C211/04 ,  C07C209/24

Abstract: The invention relates to a process for preparing methylamines by gas-phase reaction of methanol and ammonia as starting materials at a pressure in the range from 15 to 30 bar in the presence of heterogeneous catalyst. The starting materials are vaporized in one or more heat exchangers (1, 2, 3), superheated to produce a feed gas stream and subsequently fed into a reactor (4), with the mixing of the starting materials being able to be carried out in the feed stream to one of the heat exchangers (1, 2, 3) or at any desired position in a heat exchanger (1, 2, 3). A product gas stream comprising monomethylamine, dimethylamine and trimethylamine and also reaction by-products is taken off from the reactor (4). To control the reactor inlet temperature of the starting materials to a temperature in the range from 360° C. to 370° C., all or some of the feed gas stream or the product gas stream is passed through an adjustable valve (5) in order to vary the pressure and thus the condensation temperature.

公开(公告)号：DE10011942A1

公开(公告)日：2001-09-13

申请号：DE10011942

申请日：2000-03-11

Applicant: BASF AG

Inventor： RUIDER GUENTHER ,  ROS KARL-HEINZ ,  MELDER JOHANN-PETER ,  SCHULZ GERHARD ,  GUTSCHOVEN FRANK ,  BUSKENS PHILIPP

IPC: C07C213/10 ,  C07C215/08 ,  C07C215/12 ,  C07C215/14

Abstract: Preparation of alkanolamines with improved color quality comprises (a) treating the alkanolamine (I) with an effective amount of phosphorous or hypophosphorous acid or its compounds for not less than 5 minutes at elevated temperature and then (b) distillation in the presence of an effective amount of one of these phosphorus compounds.

公开(公告)号：DE19855383A1

公开(公告)日：2000-06-08

申请号：DE19855383

申请日：1998-12-01

Applicant: BASF AG

Inventor： RUIDER GUENTHER ,  ROS KARL-HEINZ

IPC: C07C213/04 ,  C07C213/10 ,  C07C215/08 ,  C07C215/00

Abstract: The invention relates to a method for purifying triethanolamine which is produced by reacting aqueous ammonia with ethylene oxide in the liquid phase under pressure and at an increased temperature. To this end, excess ammonia, water and monoethanolamine are separated from the reaction product. The thus obtained crude product is reacted with ethylene oxide at temperatures of from 110 to 180 DEG C and is rectified in the presence of phosphorous or hypophosphorous acid or the compounds thereof.

公开(公告)号：DE102005052457A1

公开(公告)日：2007-05-10

申请号：DE102005052457

申请日：2005-11-03

Applicant: BASF AG

Inventor： ERNST MARTIN ,  OEHLENSCHLAEGER STEFFEN ,  KUHNKE FRANK ,  ROS KARL-HEINZ ,  DEEG ROLAND ,  MELDER JOHANN-PETER

IPC: C07C211/11 ,  C07C209/48

Abstract: The present invention relates to a process for the industrial preparation of a diamine starting from a corresponding alkenyl nitrile comprising at least one C—C double bond, which comprises the steps (a) reaction of the alkenyl nitrile with a corresponding monoamine in a first reactor so that the monoamine adds exothermically onto the at least one double bond to form an aminoalkyl nitrile, with the monoamine and water being charged initially and the alkenyl nitrile being fed in; (b) evaporation of unreacted alkenyl nitrile and monoamine to increase the concentration of the aminoalkyl nitrile product in the bottoms of the first reactor; (c) transfer of the aminoalkyl nitrile bottom product from step (b) to a second reactor; (d) batchwise catalytic hydrogenation of the aminoalkyl nitrile transferred in step (c) to the diamine in the second reactor, with each batch being obtained by initially charging a catalyst suitable for the hydrogenation of nitriles to amines and also water, the desired diamine and a base, introducing hydrogen into the second reactor and feeding in the aminoalkyl nitrile transferred in step (c); and (e) isolation of the diamine and, if appropriate, repetition of the steps (a) to (e). The invention further relates to an apparatus for preparing these diamines and the use of the apparatuses. A preferred diamine is 3-dimethylaminopropylamine (DMAPA).

公开(公告)号：DE102004058886A1

公开(公告)日：2006-06-08

申请号：DE102004058886

申请日：2004-12-06

Applicant: BASF AG

Inventor： GRAFMANS HORST ,  MAAS STEFFEN ,  WECK ALEXANDER ,  RUETTER HEINZ ,  SCHULZ MICHAEL ,  ROS KARL-HEINZ

IPC: C07C231/02 ,  C07C233/05

Abstract: A process for preparing N,N-dimethylacetamide (DMAC) by continuously reacting methyl acetate (MeOAc) with dimethylamine (DMA) in the presence of a basic catalyst, wherein MeOAc is used in the form of a methanolic solution which is obtained as a by-product in the preparation of polyTHF by transesterifying polyTHF diacetate with methanol.

公开(公告)号：DE102004023529A1

公开(公告)日：2005-12-08

申请号：DE102004023529

申请日：2004-05-13

Applicant: BASF AG

Inventor： HAESE FRANK ,  BOETTCHER ARND ,  STEIN BERND ,  REIF WOLFGANG ,  MELDER JOHANN-PETER ,  ROS KARL-HEINZ ,  RUETTER HEINZ ,  LIANG SHELUE ,  RITTINGER STEFAN

IPC: C07C209/16 ,  C07C209/26 ,  C07C211/06 ,  C07C211/08 ,  C07C211/35 ,  C07C213/02 ,  C07C217/08 ,  C07D295/02 ,  C07D295/027 ,  C07D295/03 ,  C07D295/088 ,  C07C217/42 ,  C07C215/08

Abstract: Process for the continuous preparation of an amine by reaction of a primary or secondary alcohol, aldehyde and/or ketone with hydrogen and a nitrogen compound selected from the group consisting of ammonia, primary and secondary amines at a temperature in the range from 60 to 300° C. in the presence of a copper-containing catalyst, wherein the catalytically active composition of the catalyst prior to reduction with hydrogen comprises from 20 to 85% by weight of aluminum oxide (Al 2 O 3 ), zirconium dioxide (ZrO 2 ), titanium dioxide (TiO 2 ) and/or silicon dioxide (SiO 2 ), from 1 to 70% by weight of oxygen-containing compounds of copper, calculated as CuO, from 0 to 50% by weight of oxygen-containing compounds of magnesium, calculated as MgO, oxygen-containing compounds of chromium, calculated as Cr 2 O 3 , oxygen-containing compounds of zinc, calculated as ZnO, oxygen-containing compounds of barium, calculated as BaO, and/or oxygen-containing compounds of calcium, calculated as CaO, and less than 30% by weight of oxygen-containing compounds of nickel, calculated as NiO, based on the oxygen-containing compounds of copper, calculated as CuO, and the reaction is carried out isothermally in the gas phase in a tube reactor.