Simultaneous separation process of 6-aminocapronitrile and hexamethylenediamine

    公开(公告)号:CZ289878B6

    公开(公告)日:2002-04-17

    申请号:CZ20012583

    申请日:2001-07-13

    Applicant: BASF AG

    Abstract: Simultaneous prepn of caprolactam and hexamethylene diamine (HMD) from adipo-dinitrile (ADN) comprises (a) partial hydrogenation of (I) to a mixt. of ADN; HMD, 6-amino-capronitrile (ACN) ammonia and hexamethylenimine (HMI); (b) distillation in a first column at 10-30 br and 60-220 deg C in the presence of an inert substance (A) that boils at 60-220 deg C at 18 bar, to remove most of the ammonia at the head, leaving a residue; (c) distillation in a second column of the residue which contains ADN, HMD, ACN, HMI, (A) and residual NH3) at 100-220 deg C and 2-15 bar, under conditions different from those in the first column, giving at column head temp. of at least 20 deg C and a sump. temp. of 220 deg C max, to remove the NH3 and some (A), leaving a residue; (d) distillation in a third column, of the residue (which contains ADN, HMD, ACN, HMI and (A) at 10-220 deg C and 0.1-2 bar, (opt. in the presence of an inert substance (B) that boils at 50-220 deg C at 0.3 bar) to remove (A) for return to the second column, leaving a residue; (e) distillation in a fourth column, of the residue (which contains ADN, HMD, ACN, HMI and opt. (B)) at 100-220 deg C and 10-500 mbar to give a head fraction KPI (contg. HMD, HMI and opt. (B) and a residue (R4); (f) distillation of KPI in a fifth column at 100-220 deg C and 50-2000 mbar, to give a head fraction KP2 (contg. HMI and opt. (B)) which is returned to column 3 or partly returned and partly removed, and a residue comprising 95% HMD; and (g) the residue (R4) from the fourth column, contg. ACN and (I), is distilled in a sixth column at 100-220 deg C and 1-500 mbar to give a head product contg. 95% ACN and a residue (R2) contg. ADN); (h) cyclising. Also claimed is a process for the simultaneous separation of HDM and ACN for (M) by steps (b)-(g).

    Process for the continuous preparation of pure 5-formyl valeric acid esters

    公开(公告)号:CZ292036B6

    公开(公告)日:2003-07-16

    申请号:CZ34698

    申请日:1996-07-26

    Applicant: BASF AG

    Abstract: 5-Formyl valeric acid esters are prepared in a yield of not less than 90 percent by distillation of a formyl valeric ester mixture of 5-formyl valeric acid ester and either 3- or 4-formyl valeric acid ester or a mixture of 3- and 4-formyl valeric acid esters, wherein the ester radicals of the respective formyl valeric acid esters are identical, wherein the 3- or 4-formyl valeric acid esters or a mixture thereof are separated from the 5-formyl valeric acid ester in a distillation column at a pressure in the range from 2.10e2 to 1.10e4 Pa (from 2 to 100 mbar) and a temperature of not above 150 degC (measured as the temperature at the bottom of the column) and the esters used are the corresponding methyl or ethyl esters, whereby the purity of the 5-formyl valeric acid ester is not less than 98 percent and, as impurity, 4-formyl valeric acid ester is present in an amount of not more than 100 ppm.

    Process for simultaneously preparing caprolactam and hexamethylenediamine

    公开(公告)号:CZ289886B6

    公开(公告)日:2002-04-17

    申请号:CZ202797

    申请日:1995-12-22

    Applicant: BASF AG

    Abstract: Disclosed is a process for simultaneously preparing caprolactam and hexamethylenediamine from adiponitrile. The invented preparation process is characterized by (a) partial hydrogenation of adiponitrile, (b) subjecting the obtained mixture to distillation to obtain a portion of ammonia as a top product and a heavy fraction I, whereby distillation is carried out in the presence of an inert compound A, (c) subjecting the heavy fraction I to a second distillation to obtain a mixture of the inert compound A and ammonia as a top product and a heavy fraction II, (d) subjecting the heavy fraction II to another distillation to obtain the inert compound A as a top product and a heavy fraction III, whereby the distillation is optionally carried out in the presence of a compound B, (e) subjecting the heavy fraction to distillation to obtain a top product KP1 and a heavy fraction IV, (f) subjecting the KP1 top to distillation to obtain a top product KP2 and a heavy fraction V, whereby the se KP2 top product is supplied at least partially to a third column and the residue is discharged, and (g) subjecting the heavy fraction IV to distillation in order to obtain 6-aminocapronitrile as a top product with adiponitrile at the column bottom, and so obtained 6-aminocapronitrile is then recycled to caprolactam.

    PROCESS OF CONTINUOUS OBTAINING PURE ESTERS OF 5-FORMYLOVALERIC ACID

    公开(公告)号:CZ34698A3

    公开(公告)日:1998-07-15

    申请号:CZ34698

    申请日:1996-07-26

    Applicant: BASF AG

    Abstract: PCT No. PCT/EP96/03290 Sec. 371 Date Jan. 27, 1998 Sec. 102(e) Date Jan. 27, 1998 PCT Filed Jul. 26, 1996 PCT Pub. No. WO97/06126 PCT Pub. Date Feb. 20, 19975-Formylvaleric esters are prepared in a yield of not less than 90% by distillation of a formylvaleric ester mixture of 5-formylvaleric ester and either 3- or 4-formylvaleric ester or a mixture of 3- and 4-formylvaleric esters, where the ester radicals of the respective formylvaleric esters are identical, wherein the 3- or 4-formylvaleric ester or a mixture thereof is separated from the 5-formylvaleric ester in a distillation column at a pressure in the range from 2 to 100 mbar and a temperature of not above 150 DEG C. (measured as the temperature at the bottom of the column) and the esters used are the corresponding methyl or ethyl esters, where the purity of the 5-formylvaleric ester is not less than 98% and, as impurity, 4-formylvaleric ester is present in an amount of not more than 100 ppm.

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