THE PREPARATION OF 1, 6-HEXANEDIOL AND CAPROLACTONE

    公开(公告)号:MY118128A

    公开(公告)日:2004-09-30

    申请号:MYPI9700759

    申请日:1997-02-27

    Applicant: BASF AG

    Abstract: A PROCESS FOR PREPARING 1, 6-HEXANEDIOL AND e-CAPROLACTONE FROM A CARBOXYLIC ACID MIXTURE WHICH COMPRISES ADIPIC ACID, 6-HYDROXYCAPROIC ACID AND SMALL AMOUNTS OF 1,4-CYCLOHEXANEDIOLS AND WHICH IS OBTAINED AS BYPRODUCT OF THE OXIDATION OF CYCLOHEXANE TO CYCLOHEXANONE/CYCLOHEXANOL WITH OXYGEN OR OXYGEN-CONTAINING GASES BY WATER EXTRACTION OF THE REACTION MIXTURE, BY ESTERIFICATION AND HYDROGENATION OF A PART STREAM TO GIVE HEXANEDIOL AND CYCLIZATION OF 6-HYDROXYCAPROIC ESTER TO CAPROLACTONE, WHEREIN A) THE MONO- AND DICARBOXYLIC ACIDS PRESENT IN THE AQUEOUS REACTION MIXTURE ARE REACTED WITH A LOW MOLECULAR WEIGHT ALCOHOL TO GIVE THE CORRESPONDING CARBOXYLIC ESTERS, B) THE RESULTING ESTERIFICATION MIXTURE IS SUBJECTED TO A FIRST DISTILLATION STAGE TO REMOVE EXCESS ALCOHOL, WATER AND LOW BOILERS, C) A SECOND DISTILLATION STAGE IS CARRIED OUT ON THE BOTTOM PRODUCT FOR FRACTIONATION INTO AN ESTER FRACTION WHICH IS ESSENTIALLY FREE OF 1,4-CYCLOHEXANEDIOLS AND INTO A FRACTION WHICH COMPRISES AT LEAST THE GREATER PART OF THE 1,4-CYCLOHEXANEDIOLS, D) A THIRD DISTILLATION STAGE IS CARRIED OUT TO REMOVE FROM THE ESTER FRACTION AT LEAST PARTLY A STREAM WHICH ESSENTIALLY-COMPRISES 6-HYDROXYCAPROIC ESTER, E) THE ESTER FRACTION FROM (D), FROM WHICH 6-HYDROXYCAPROIC ESTER HAS BEEN AT LEAST PARTLY REMOVED, IS CATALYTICALLY HYDROGENATED AND THE HYDROGENATION PRODUCT IS DISTILLED IN A CONVENTIONAL MANNER TO ISOLATE 1,6-HEXANEDIOL AND F) THE STREAM WHICH ESSENTIALLY COMPRISES 6-HYDROXYCAPROIC ESTER IS HEATED TO ABOVE 200°C UNDER REDUCED PRESSURE, RESULTING IN CYCLIZATION OF 6-HYDROXYCAPROIC ESTER TO CAPROLACTONE, AND THE CYCLIZATION PRODUCT IS DISTILLED TO ISOLATE PURE e-CAPROLACTONE.

    24.
    发明专利
    未知

    公开(公告)号:AT266619T

    公开(公告)日:2004-05-15

    申请号:AT99944417

    申请日:1999-08-17

    Applicant: BASF AG

    Abstract: A process for catalytic hydrogenation of adiponitrile to hexamethylenediamine at elevated temperature and elevated pressure in the presence of catalysts based on elemental iron as catalytically active component and ammonia as solvent comprisesa) hydrogenating adiponitrile at from 70 to 220° C. and from 100 to 400 bar in the presence of catalysts based on elemental iron as catalytically active component and ammonia as solvent to obtain a mixture comprising adiponitrile,6-aminocapronitrile, hexamethylenediamine and high boilers until the sum total of the 6-aminocapronitrile concentration and the adiponitrile concentration is within the range from 1 to 50% by weight, based on the ammonia-free hydrogenation mixture,b) removing ammonia from the hydrogenation effluent,c) removing hexamethylenediamine from the remaining mixture,d) separating 6-aminocapronitrile and adiponitrile from high boilers individually or together, ande) returning 6-aminocapronitrile, adiponitrile or mixtures thereof into step a).

    25.
    发明专利
    未知

    公开(公告)号:ES2201127T3

    公开(公告)日:2004-03-16

    申请号:ES95942198

    申请日:1995-12-22

    Applicant: BASF AG

    Abstract: The invention concerns the simultaneous preparation of caprolactam and hexamethylene diamine from adipodinitrile, by the following steps: (a) the adipodinitrile is partially hydrogenated, producing a mixture substantially containing 6-aminocapronitrile, hexamethylene diamine, ammonia, adipodinitrile and hexamethylene imine (= "the mixture"); (b) the mixture obtained in step (a) is distilled, producing ammonia, as the forerunnings, and a residue I, in the presence of a compound A which is inert in the distillation conditions, the ammonia not being separated totally; (c) the residue I, substantially containing "the mixture", inert compound A and ammonia, the ammonia content being less than that of the mixture used in step (b), is subjected to a second distillation, producing a mixture of the inert compound A and ammonia, as the forerunnings, and a residue II; (d) the base II, substantially containing "the mixture" and inert compound A, is subjected to distillation in a third column, producing the inert compound A, as the forerunnings, and a residue III; (e) the base III, substantially containing "the mixture" and optionally an inert compound B, is subjected to distillation in a fourth column, producing forerunnings KP1, which substantially contain hexamethylene imine, optionally inert compound B and hexamethylene diamine, and a residue IV; (f) the forerunnings KP1 are subjected in a fifth column to distillation, producing forerunnings KP2, which substantially contain hexamethylene imine and optionally inert compound B, and a residue V, which substantially contains hexamethylene diamine with a degree of purity of at least 95 %, the forerunnings KP2 being fed to the third column or optionally only partially fed to the third column, and the rest being discarded; and (g) the residue IV, substantially containing 6-aminocapronitrile and adipodinitrile, is subjected in a sixth column to distillation, producing 6-aminocapronitrile with a degree of purity of at least 95 %, as forerunnings, and adiponitrile in the residue. The resultant 6-aminocapronitrile is cyclized to form caprolactam.

    METHOD OF CONTINUOUSLY PURIFING CRUDE CAPROLAKTAM OBTAINED FROM 6-AMINOCAPRONITRILE

    公开(公告)号:PL186443B1

    公开(公告)日:2004-01-30

    申请号:PL32116295

    申请日:1995-12-22

    Applicant: BASF AG

    Abstract: Crude capronitrile is purified by hydrogenation, subsequent treatment in an acidic medium and subsequent distillation in an alkaline medium, by a process in which (a) 6-aminocapronitrile is converted into crude caprolactam by reaction with water, (b) high boilers and low boilers are separated off from the crude caprolactam from step (a), (c) the crude caprolactam from step (b) is treated with hydrogen at from 50 DEG to 150 DEG C. and from 1.5 to 250 bar in the presence of a hydrogenation catalyst and, if desired, of a solvent to give a mixture A, (d1) mixture A in a solvent is passed, at from 30 DEG to 80 DEG C. and from 1 to 5 bar, over an ion exchanger containing terminal acid groups to give a mixture B1, or (d2) mixture A is distilled in the presence of sulfuric acid, any solvent present being removed before the addition of the sulfuric acid, to give a mixture B2, and (e) mixture B1 or mixture B2 is distilled in the presence of a base to give pure caprolactam.

    28.
    发明专利
    未知

    公开(公告)号:ES2198013T3

    公开(公告)日:2004-01-16

    申请号:ES97951227

    申请日:1997-11-18

    Applicant: BASF AG

    Abstract: Polytetrahydrofuran, tetrahydrofuran copolymers, diesters or monoesters of these polymers are prepared by polymerizing tetrahydrofuran in the presence of at least one telogen and/or comonomer on a heterogeneous carrier catalyst which contains on an oxidic carrier material as active mass a catalytically active amount of at least one oxygenous molybdenum and/or tungsten compound and, when the precursor compounds of the active mass have been applied to the carrier material precursor, has been calcined at temperatures of between 500° C. and 1000° C. The catalyst used contains a promotor which comprises at least one element or a compound of an element of the 2nd, 3rd including the lanthanides, 5th, 6th, 7th, 8th or 14th group of the periodic system of elements.

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