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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
    24.
    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).

    Production of anhydrous formic acid involves hydrolysis of methyl formate followed by distillation, extraction with amide and further distillation stages, using the same extractant to wash useful products out of the off-gas
    29.
    发明专利
    Production of anhydrous formic acid involves hydrolysis of methyl formate followed by distillation, extraction with amide and further distillation stages, using the same extractant to wash useful products out of the off-gas 未知

    公开(公告)号：DE10002790A1

    公开(公告)日：2001-07-26

    申请号：DE10002790

    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 ,  B01J14/00 ,  C07C51/09 ,  C07C51/44 ,  C07C51/48 ,  C07C53/02 ,  C07C233/01

    Abstract: In the production of anhydrous formic acid (FA) by hydrolysis of methyl formate (MF) followed by distillation, extraction of the bottom product with an amide extractant (I) and further distillation stages, the off-gas streams containing MF and/or methanol and/or FA are washed with (I) which is then returned to the process along with these products in solution. 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. In this process, the off-gas streams containing MF and/or methanol and/or FA are washed with extractant (I), which is then returned to the process along with dissolved MF and/or methanol and/or FA. 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 system (2) for stage (ii), a distillation system (4) for stage (iv), an extraction unit (3), a distillation system (5) for stage (vi) and an off-gas scrubber (9).

    Manganese pentacarbonyl hydride and a process for its preparation
    30.
    发明专利
    Manganese pentacarbonyl hydride and a process for its preparation 未知

    公开(公告)号：GB855065A

    公开(公告)日：1960-11-30

    申请号：GB1862058

    申请日：1958-06-11

    Applicant: BASF AG

    Inventor： HIEBER WALTER ,  WAGNER GERHARD

    IPC: C01G45/04

    Abstract: Manganese pentacarbonyl hydride (Mn(CO)5).H is prepared by reacting manganese pentacarbonyl with an alcoholic solution of an alkali metal or alkaline earth metal hydroxide and treating the pentacarbonyl manganate thus formed with a non-oxidising inorganic or organic acid, an acid salt or other acid media whose aqueous solution contains hydrazin ions. Manganese pentacarbonyl is reacted suitably with an alcoholic solution of a hydroxide of Na, K, Li, Rb, or Cs or an alkaline earth metal, e.g. Ca or Ba and methanol, ethanol or propanol, preferably methanol. The resulting solution, containing a pentacarbonyl manganate, may be treated per se with the acid, acid salt or other acid media, or the pentacarbonyl manganate salt may be isolated by evaporation of the solvent and then treated to yield manganese pentacarbonyl hydride. Alternatively, the pentacarbonyl manganate solution may be treated with complexes containing large-volumed cations, e.g. tri-orthophenanthroline nickel (II) salts or stable cation complexes, e.g. (Cr(C6H6)2)+ or (Co(C5H5)2)+, and the resulting complex compound which precipitates being separated and treated with acid to yield the manganese pentacarbonyl. Reference is made to the reaction of the manganese pentacarbonyl hydride with diazo methane to yield a compound of the formula Mn(CO)5.CH3.

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