Classifications

• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
  • C07C209/82—Purification; Separation; Stabilisation; Use of additives
  • C07C209/84—Purification
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C2601/00—Systems containing only non-condensed rings
  • C07C2601/06—Systems containing only non-condensed rings with a five-membered ring
  • C07C2601/08—Systems containing only non-condensed rings with a five-membered ring the ring being saturated

Definitions

• the present invention relates to a process for separating 2-aminomethylcyclopentylamine (AMCPA) from a mixture comprising hexamethylenediamine and AMCPA.
• AMCPA 2-aminomethylcyclopentylamine
• HMI hexamethyleneimine
• DACH 1, 2-diaminocyclohexane
• AMCPA hexamethyleneimine
• the partial or complete hydrogenation of adiponitrile can be carried out by one of the known processes, for example by one of the processes described above in US Pat. No. 4,601,859, US Pat. No. 2,762,835, US Pat 416, DE-A 4 235 466, US-A 3 696 153, DE-A 9 500 222 or WO 92/21650 by generally containing the hydrogenation in the presence of nickel, cobalt, iron or ruthenium Performs catalysts.
• the catalysts can be used as.
• Supported catalysts or as unsupported catalysts can be used.
• aluminum oxide, silicon dioxide, titanium dioxide, magnesium oxide, activated carbon and spinels are suitable as catalyst supports.
• Raney nickel and Raney cobalt, for example, are suitable as full catalysts.
• the hydrogenation gives a mixture which contains hexamethylenediamine, AMCPA and optionally 6-aminocapronitrile and adiponitrile.
• the separation from a mixture containing hexamethylenediamine and AMCPA can be carried out in a manner known per se, preferably by distillation, for example according to DE-A 195 002 22 or German application 19 548 289.1, simultaneously or in succession, for example in a distillation column or in a side draw column Partition (Petlyuk column), so that the condensation temperature of the subsequent cleaning column in the AMCPA separation is generally higher and the condensation is facilitated.
• the low-boiling secondary component DACH if present, can advantageously be removed simultaneously with AMCPA, but the separation of DACH can also be carried out overhead in a separate column.
• low-boiling secondary components such as HMI, if present, are advantageously separated off completely or partially.
• the weight fraction of AMCPA, based on hexamethylenediamine is generally 10 to 10,000 ppm, in particular 100 to 1000 ppm, before the separation, the process according to the invention not being limited to these limits.
• the separation of AMCPA from the mixture is advantageously carried out by distillation at pressures of between 1 and 1100 mbar, preferably 1 to 500, which results in bottom temperatures in the range from 40 to 250 ° C.
• distillation columns which have a low pressure drop, preferably at most 1 mbar, in particular 0.5 mbar, per theoretical plate are particularly suitable.
• Packing columns are particularly suitable, preferably with ordered packing such as sheet metal packs, in particular wire mesh packs.
• water is added to the distillation mixture, with water contents of 0.01 to 10% by weight, in particular 0.1 to 5% by weight, based on the distillation mixture being preferred.
• the water can be added to the mixture before the distillation or during the distillation, for example into the column, preferably in the area below the feed, in particular in the bottom area.
• AMCPA and water are obtained as top product, generally, if hexamethylenediamine and AMCPA are present in the mixture, in a mixture with DACH and low-boiling components.
• the distillation can be carried out in several, such as 2 or 3 columns, advantageously in a single column.
• Hexamethylenediamine can be processed with dicarboxylic acids such as adipic acid into technically important polymers.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Applications Claiming Priority (3)

Publications (1)

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Family Applications (1)

Country Status (10)

Family Cites Families (5)

• 1997
  • 1997-02-07 DE DE19704618A patent/DE19704618A1/de not_active Withdrawn
• 1998
  • 1998-01-17 WO PCT/EP1998/000241 patent/WO1998034901A1/de not_active Application Discontinuation
  • 1998-01-17 EP EP98905307A patent/EP0960094A1/de not_active Withdrawn
  • 1998-01-17 JP JP53367398A patent/JP2001511163A/ja active Pending
  • 1998-01-17 CA CA002280830A patent/CA2280830A1/en not_active Abandoned
  • 1998-01-17 AU AU60947/98A patent/AU6094798A/en not_active Abandoned
  • 1998-01-17 BR BR9807188-2A patent/BR9807188A/pt not_active Application Discontinuation
  • 1998-01-17 KR KR1019997007153A patent/KR20000070888A/ko not_active Application Discontinuation
  • 1998-01-17 CN CN98803807A patent/CN1251567A/zh active Pending
  • 1998-02-05 AR ARP980100510A patent/AR011636A1/es unknown

Non-Patent Citations (1)

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