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    Production of anhydrous formic acid involves hydrolysis of methyl formate followed by distillation, extraction with amide and further distillations, using the amide also as a foam suppressant in first distillation stage
    1.
    发明专利
    Production of anhydrous formic acid involves hydrolysis of methyl formate followed by distillation, extraction with amide and further distillations, using the amide also as a foam suppressant in first distillation stage 未知

    公开(公告)号：DE10002793A1

    公开(公告)日：2001-07-26

    申请号：DE10002793

    申请日：2000-01-24

    Applicant: BASF AG

    Inventor： AUER HEINZ ,  BESLING BERND ,  HAMMER HANS ,  HASSE HANS ,  SAUER FRIEDRICH ,  VICARI MAXIMILIAN ,  WAGNER GERHARD ,  ADRIAN TILL

    IPC: C07C51/56 ,  C07C51/09 ,  C07C51/44 ,  C07C51/48 ,  C07C53/02 ,  B01D19/04 ,  C07C233/05

    Abstract: In the production of anhydrous formic acid by hydrolysis of methyl formate followed by distillation, extraction of the bottom product with an amide extractant (I) and further distillation stages, a part-stream of (I) is taken out and fed into the first distillation column at a point between the inlet for the hydrolysis mixture and the methanol take-off point. A process for the production of (essentially) anhydrous formic acid (FA) involves: (i) hydrolysis of methyl formate (MF), (ii) removal of methanol and excess MF by distillation, (iii) liquid-liquid extraction of the bottom product with an amide of formula R (R )NC(O)R (I), (iv) distillation of the extract, (v) recycling the top product from (iv) (containing water and some FA) to the lower part of the distillation column used in stage (ii), (vi) separation of the bottom product from (iv) by distillation into anhydrous FA and extractant (I) and (vii) recycling (I) into the process from stage (vi). In this process, part of the extractant (I) is taken off and fed into the distillation unit for stage (ii) at a point above the inlet for the hydrolysis mixture and below the take-off point for methanol. R , R = alkyl, cycloalkyl, aryl or aralkyl, or R plus R plus the linking nitrogen may form a 5- or 6-membered heterocycle, with the proviso that only one of these groups is aryl; R = H or 1-4C alkyl. An Independent claim is also included for the apparatus used for this process, comprising a synthesis reactor (6), a hydrolysis reactor (1), a distillation column (2) for stage (ii), a distillation column (4) for stage (iv), an extraction unit (3), a distillation column (5) for stage (vi) and a connecting line (8) for transferring a part-stream of extractant (I) to distillation column (2).

    2.
    发明专利
    未知

    公开(公告)号：DE19728732A1

    公开(公告)日：1999-01-07

    申请号：DE19728732

    申请日：1997-07-04

    Applicant: BASF AG

    Inventor： BESLING BERND ,  KNAB JEAN WERNER ,  BROX WOLFGANG DR ,  LOHE BERND DR

    IPC: C07C7/148 ,  C07C11/09 ,  C07C7/04

    Abstract: The invention relates to a method for obtaining isobutene from conjugated hydrocarbons. Said method comprises the following steps; a) placing C4-hydrocarbon with a C3- or C4-primary alkanol; b) reacting isobutene in conjugated C4-hydrocarbons with C3- or C4-primary alkanol in the presence of a heterogeneous catalyst to obtain the corresponding isobutene-based tertiary ether; c) causing fractionation of the accumulated reaction mixture into non ethereal C4-hydrocarbons with a low boiling point and isobutene-based tertiary ether with a high boiling point by using a fractionating tower, said C4-hydrocarbons being removed by the head while the isobutene-based tertiary ether accumulated on the bottom is fed into a reactor; d) causing fission of said ether, thereby obtaining isobutene and the corresponding primary C3-C4-alkanol; e) distilling the blending resulting from step d) by using another fractionating tower, and removing the isobutene as an overhead. Step a) is carried out in an area (4C) containing the reaction ingredients in which the catalyst is placed to complete step b); the area (4C) is part of a fractionating tower (4); in said area (4C9 is effected a reaction fractionation; C3- or C4-alkanol is fed upstream from area (4C) of the fractionating tower (4), and the conjugated C4-hydrocarbons downstream from said area (4C).

    3.
    发明专利
    未知

    公开(公告)号：DE19703627A1

    公开(公告)日：1998-08-06

    申请号：DE19703627

    申请日：1997-01-31

    Applicant: BASF AG

    Inventor： BESLING BERND ,  HASSE HANS ,  PLUECKHAN JUERGEN DR ,  MAYER THOMAS ,  AUER HEINZ

    IPC: C07D301/32 ,  C07D303/04

    Abstract: In a pure ethylene oxide distillation process, an aqueous mixture containing ethylene oxide, formaldehyde and at least 5 % by weight water is supplied via an inlet to a distillation device with at least one distillation column at a height above the column bottom of at least 8 theoretical stages. The ethylene oxide is removed at the head of the column and a mixture is obtained at the bottom of the column with less than 5 % by weight ethylene oxide.

    5.
    发明专利
    未知

    公开(公告)号：DE10143424A1

    公开(公告)日：2003-03-20

    申请号：DE10143424

    申请日：2001-09-05

    Applicant: BASF AG

    Inventor： PESCHEL WERNER ,  HILDEBRANDT AXEL ,  BESLING BERND

    IPC: C07C213/04 ,  C07C215/08 ,  C07C215/12 ,  C07C215/10

    Abstract: Production of ethanolamines comprises reacting ammonia with ethylene oxide in the presence of water in a pressurized reactive distillation column equipped with a reboiler. The energy supply to the reboiler and the ammonia:ethylene oxide ratio in the feed stream are controlled so that the bottoms stream can be separated into an ammonia and water stream and a mono-, di- and triethanolamine stream. Production of mono-, di- and triethanolamine comprises liquid-phase reaction of ammonia with ethylene oxide in the presence of water in a pressurized reactive distillation column (I) equipped with a reboiler, where the mono:di:triethanolamine ratio is controlled by the energy supply to the reboiler and the ammonia content of the bottoms stream is controlled by the ammonia:ethylene oxide ratio in the feed stream so that the bottoms stream can be separated into an ammonia and water stream and a mono-, di- and triethanolamine stream in a single distillation column (II).

    8.
    发明专利
    未知

    公开(公告)号：DE10002795A1

    公开(公告)日：2001-08-02

    申请号：DE10002795

    申请日：2000-01-24

    Applicant: BASF AG

    Inventor： AUER HEINZ ,  BESLING BERND ,  HAMMER HANS ,  HASSE HANS ,  SAUER FRIEDRICH ,  VICARI MAXIMILIAN ,  WAGNER GERHARD ,  TILL ADRIAN

    IPC: C07C51/09 ,  C07C51/44 ,  C07C51/48 ,  C22C14/00 ,  C22C38/00 ,  C22C38/42 ,  C22C38/44 ,  C07C53/02 ,  C07C233/01 ,  B01J19/02

    Abstract: The invention concerns a device and a method for obtaining anhydrous or substantially anhydrous formic acid. Said device is partly or totally made of a zirconium-free material. A liquid material of general formula (I) is used as extracting agent, wherein radicals R and R represent alkyl, cycloalkyl, aryl or aralkyl groups or R and R together form with the N atom a heterocyclic five or six-membered ring and in which only one of the radicals is an aryl group and in which R stands for hydrogen or a C1-C4-alkyl group. The device comprises the following: (i) a synthesis reactor (6); (ii) a hydrolysis reactor (1); (iii) a first distillation device (2); (iv) a second distillation device (4); (v) an extraction device (3) and (vi) a third distillation device (5).

    Production of anhydrous formic acid involves hydrolysis of methyl formate, steam distillation, extraction with amide and further distillations, with prior use of steam for stripping aqueous extraction residue
    9.
    发明专利
    Production of anhydrous formic acid involves hydrolysis of methyl formate, steam distillation, extraction with amide and further distillations, with prior use of steam for stripping aqueous extraction residue 未知

    公开(公告)号：DE10002794A1

    公开(公告)日：2001-07-26

    申请号：DE10002794

    申请日：2000-01-24

    Applicant: BASF AG

    Inventor： ADRIAN TILL ,  AUER HEINZ ,  BESLING BERND ,  HAMMER HANS ,  HASSE HANS ,  SAUER FRIEDRICH ,  VICARI MAXIMILIAN

    IPC: B01J14/00 ,  C07C27/02 ,  C07C51/09 ,  C07C51/44 ,  C07C51/48 ,  C07C53/02 ,  C07C51/42 ,  C07C27/26 ,  C02F1/16

    Abstract: In the production of anhydrous formic acid by hydrolysis of methyl formate followed by steam distillation, extraction of the bottom product and further distillation stages, the steam used for steam distillation is used before this for stripping the aqueous phase which is discharged from the extraction stage. A process for the production of (essentially) anhydrous formic acid (FA) involves: (i) hydrolysis of methyl formate (MF), (ii) distillation of methanol and excess MF from the hydrolysis mixture with injection of steam into the bottom of the distillation column, (iii) liquid-liquid extraction of the bottom product with an extractant (I) for formic acid, some of the resulting aqueous phase being discharged as effluent, (iv) distillation of the extract, (v) recycling the top product from (iv) (containing water and some FA) to the lower part of the distillation column used in stage (ii), (vi) separation of the bottom product from (iv) into anhydrous FA and extractant (I) by distillation, and (vii) recycling (I) into the process from stage (vi). In this process, the steam injected in stage (ii) is used before this as waste water stripping steam to treat the aqueous phase discharged from stage (iii). An Independent claim is also included for the apparatus used for this process, comprising a synthesis reactor (6), a hydrolysis reactor (1), a distillation column (2) for stage (ii), a distillation column (4) for stage (iv), an extractor (3), a distillation column (5) for stage (vi) and a waste water stripper (10).

    Production of anhydrous formic acid by hydrolyzing methyl formate comprises introducing methanol-containing methyl formate into distillation column used to distil hydrolysis mixture
    10.
    发明专利
    Production of anhydrous formic acid by hydrolyzing methyl formate comprises introducing methanol-containing methyl formate into distillation column used to distil hydrolysis mixture 未知

    公开(公告)号：DE10002791A1

    公开(公告)日：2001-07-26

    申请号：DE10002791

    申请日：2000-01-24

    Applicant: BASF AG

    Inventor： ADRIAN TILL ,  AUER HEINZ ,  BESLING BERND ,  HAMMER HANS ,  HASSE HANS ,  SAUER FRIEDRICH ,  VICARI MAXIMILIAN

    IPC: C07C51/09 ,  C07C51/44 ,  C07C51/48 ,  C07C53/02 ,  C07C51/42

    Abstract: Production of anhydrous formic acid, by hydrolyzing methyl formate and distilling off methanol and unreacted methyl formate, before extracting formic acid with a selective solvent, comprises introducing methanol-containing methyl formate into the distillation column at a point between the methanol and methyl formate withdrawal points, and recycling the resulting methanol-depleted methyl formate to the hydrolysis step. Production of anhydrous formic acid comprises: (a) hydrolyzing methyl formate; (b) distilling the hydrolysis mixture to remove methanol and unreacted methyl formate; (c) introducing methanol-containing methyl formate into the distillation column at a point above the methanol withdrawal point and below the methyl formate withdrawal point; (d) recycling the methyl formate to step (a); (e) extracting formic acid from the distillation bottoms stream with a selective solvent; (f) distilling the extract to obtain a water-rich overhead stream and a bottoms stream comprising formic acid and solvent; (g) recycling the overhead stream to the bottom of the distillation column in step (b); (h) distilling the bottoms stream from step (f) to obtain an anhydrous formic acid stream and a solvent stream; and (i) recycling the solvent stream to step (e). An Independent claim is also included for apparatus for carrying out the process, comprising a synthesis reactor, a hydrolysis reactor, an extractor, and distillation columns for performing steps (b), (f) and (h).

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