Continuous preparation of poly:amide(s) from omega-amino:alkyl nitrile and water

    公开(公告)号:DE19635077A1

    公开(公告)日:1998-03-05

    申请号:DE19635077

    申请日:1996-08-30

    Applicant: BASF AG

    Abstract: A continuous multi-step process for the preparation of polyamides by reacting an w-aminoalkyl nitrile with water at high temperature and pressure, comprises (1) heating an w-aminoalkyl nitrile in an excess amount of water at 250-350 deg C and 4-30 MPa, the temperature and pressure being chosen to give a single-phase liquid reaction mixture, in which at least 95 mol.% nitrile groups are converted to form a first reaction product (I); (2) heating (I) at 220-300 deg C and 1-7 MPa, so that the pressure is at least 0.5 MPa less than that in step (1), whilst separating the gas and liquid phases to form a second reaction product (II); (3) heating (II) at 220-300 deg C and 10-300 kPa in a first sub-step (3a), then in a second sub-step (3b) the gas phase is separated from the liquid phase and then in a third sub-step (c) the relative viscosity (measured at 25 deg C and a concentration of 1 g polymer per 100 ml sulphuric acid (96 wt.%)) of the polyamide is altered to a value of 1.6-3.5 by selecting the appropriate temperature and dwell time, whilst in the final sub-step (3d) the third reaction product (III) is isolated by standard techniques and optionally processed.

    3.
    发明专利
    未知

    公开(公告)号:DE19962573A1

    公开(公告)日:2001-07-05

    申请号:DE19962573

    申请日:1999-12-23

    Applicant: BASF AG

    Abstract: The invention relates to a method for the production of polyamides from amino nitriles and water, (1) by reacting aminonitriles with water at a temperature of 180 - 350 DEG C and a pressure of 30 - 120 bar adjusted in such a way that in addition to a liquid phase, a gaseous phase is also present in the first reaction step; (2) relaxation of the reaction mixture obtained in the first reaction step via an evaporator zone or adiabatically with removal of water and ammonia in a second reaction step and (3) post-condensation in the second reaction step at a pressure 0.1 mbar to 5 bar at a temperature of 230 - 320 DEG C.

    4.
    发明专利
    未知

    公开(公告)号:DE19804033A1

    公开(公告)日:1999-08-05

    申请号:DE19804033

    申请日:1998-02-02

    Applicant: BASF AG

    Abstract: The invention relates to a continuous method for producing a polyamide by reacting at least one aminonitrile with water, comprising the following steps: (1) reaction of at least one aminonitrile with water at a temperature of between 90 and 400 DEG C and a pressure of between 0.1 and 15 x 10 Pa in a tubular flow reactor containing packing material of a Bronsted acid catalyst selected from beta zeolite, sheet silicate or titanium dioxide packing materials, as well as metallic packing materials, which yields a reaction mixture; (2) further reaction of the reaction mixture at a temperature of between 150 and 400 DEG C and a pressure which is lower than the pressure in step 1, where the temperature and pressure are selected such that a first gaseous phase and a first liquid or a first solid phase or a mixture of a first solid and a first liquid phase is obtained, and the first gaseous phase is separated from the first liquid or first solid phase or the mixture of the first liquid and first solid phase; and (3) addition of the first liquid or first solid phase or the mixture of first liquid and first solid phase to a gaseous or liquid phase containing water, at a temperature of between 150 and 370 DEG C and a pressure of between 0.1 and 30 x 10 Pa, resulting in a product mixture.

    Improved production of polyamide from amino-nitrile and water

    公开(公告)号:DE19709390A1

    公开(公告)日:1998-09-10

    申请号:DE19709390

    申请日:1997-03-07

    Applicant: BASF AG

    Abstract: Production of a polyamide from an aminonitrile (AN) and water comprises the combination of steps (1), (2) and (3) or (1), (2), (3) and (4) or (1), (2) and (4) where step (1) involves reacting the AN and water at 100-360 deg C/0.1-35 x 10 Pa; step (2) involves reacting the product of step (1) at 150-400 deg C and a pressure below that in (1) to give a first gas phase and a first liquid and/or solid phase and then separating the phases; step (3) involves reacting the first liquid and/or solid phase with a water-containing gas- or liquid-phase at 150-360 deg C to give a product mixture; and step (4) involves post-condensation of the step (3) product at 200-350 deg C and at a pressure below that in (3) to give a second water- and ammonia-containing gas phase and a second liquid and/or solid phase containing the polyamide. The polyamides prepared using the above combinations of steps are claimed per se. Preferably steps (1) - (4) are effected continuously with recycling of the gas phase obtained in each step to a prior step and with the temperature and pressure in steps (1) and/or (3) such that the gas phase is separated off. Step (1) is such that the conversion of the AN nitrile groups is at least 95 mol.% and a chain extender and/or branching agent may be present. The AN is an 8-13C aminoalkylarylnitrile or an w-aminoalkylnitrile with a 4-12C alkylene group, especially a mixture of (by wt.) 50-99.99% 6-aminocapronitrile; 0.01-50% 4-10C aliphatic- alpha ,w-, 8-12C aromatic- or 5-8C cycloalkane-dicarboxylic acid; 0-50% 4-10C alpha ,w-diamine; 0-50% 2-12C alpha ,w-dinitrile; and 0-50% 5-12C alpha ,w-amino acid or lactam.

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