公开(公告)号：DE2651195A1

公开(公告)日：1978-05-18

申请号：DE2651195

申请日：1976-11-10

Applicant: BASF AG

Inventor： NEUBAUER GERALD DIPL CHEM DR ,  WAUW GERARD VAN ,  BEULLENS JOSEF

IPC: C07D201/16 ,  C01C1/242 ,  C01C1/248 ,  C01C1/24

Abstract: Recovery of large crystals of pure ammonium sulphate (I) from reaction mixts. obtd. by Beckmann rearrangement of cyclohexanone oxime (II) in H2SO4 or oleum to give caprolactam (III) comprises first neutralising the mixt. with NH3 at autogenous pressure and 80-125 degrees C. The crude lactam is sepd. and the residual soln. evapd. at 200-600 mm Hg, with cooling to 72-101 degrees C to crystallise (I). The crystals formed are sepd. and the mother liquor recycled to neutralisation. The concn. of (I) in the recycled mother liquor is insufficient to cause crystallisation during neutralisation. Pref. neutralisation is to pH 4.5-5, and the vapours from evaporation can be condensed and used to dilute the mother liquor. Alternatively they are used to concentrate either the hydroxylammonium sulphate solns. used to make (II) from cyclohexanone, or the (I) solns. obtd. by neutralising the oximation reaction mixt. (I) is a fertiliser. It is obtd. as larger crystals than in other processes, and these have lower moisture and esp. caprolactam contents. Utilisation of steam from the evaporator improves heat economy.

公开(公告)号：DE2819994A1

公开(公告)日：1979-11-22

申请号：DE2819994

申请日：1978-05-08

Applicant: BASF AG

Inventor： DECKER EMILE DE DIPL CHEM ,  NEUBAUER GERALD DIPL CHEM DR ,  PIJL PAUL ,  WAUWE GERARD VAN

IPC: B01D53/34 ,  B01D53/50 ,  B01D53/77 ,  C01B17/96 ,  C01C1/24 ,  C01D5/04 ,  C02F1/20 ,  C02F1/74 ,  C02C5/00

公开(公告)号：DE2840126A1

公开(公告)日：1980-03-27

申请号：DE2840126

申请日：1978-09-15

Applicant: BASF AG

Inventor： DEYCK FRANS VAN ,  HENS VICTOR ,  NEUBAUER GERALD DIPL CHEM DR

IPC: B01D53/047 ,  C01B2/30

Abstract: Purification of synthesis gas produced by steam reforming of hydrocarbons (esp.CH4) is carried out by scrubbing to remove most of the CO2, compressing, and removing residual CO2, hydrocarbons and H2O by contact with an adsorbent (e.g. mol. sieve) in adsorbers operating alternately in adsorption and regeneration phases. The improvement comprises passing part of the synthesis gas to a storage tank and recycling the stored gas into the synthesis gas circuit so as to maintain constant operating parameters in the downstream gas sepn. equipment. The stored gas can be used to restore the pressure in the absorbers after decompression in the regeneration phase, so that the purified gas leaving the adsorption unit remains constant in vol. and compsn.