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    Pure higher (meth)acrylate ester preparation in high yield, for use as monomer, by carrying out esterification by adding reaction components to refluxing azeotrope-forming solvent in reactor with rotating evaporator
    53.
    发明专利
    Pure higher (meth)acrylate ester preparation in high yield, for use as monomer, by carrying out esterification by adding reaction components to refluxing azeotrope-forming solvent in reactor with rotating evaporator 未知

    公开(公告)号：DE10152680A1

    公开(公告)日：2003-05-08

    申请号：DE10152680

    申请日：2001-10-19

    Applicant: BASF AG

    Inventor： MARTIN FRIEDRICH-GEORG ,  NESTLER GERHARD ,  SCHROEDER JUERGEN

    IPC: C07C51/50 ,  C07C67/08 ,  C07C67/48 ,  C07C69/54

    Abstract: Preparation of higher (meth)acrylate esters, by reacting (meth)acrylic acid with an alcohol in presence of acid catalyst(s), polymerization inhibitor(s) and a solvent forming an azeotrope with water is effected in a reactor with a rotating evaporator by heating to the boiling point (b.pt.) of the lowest boiling component, commencing rotation and dosing the remaining components. Preparation of higher (meth)acrylate esters (I), by reacting (meth)acrylic acid (II) with an alcohol (III) in presence of acid catalyst(s) (AC), polymerization inhibitor(s) (PI) and a solvent (SV) forming an azeotrope with water, distilling off the azeotrope and condensing to form aqueous and organic phases, is effected in a reactor with a rotating evaporator in presence of at least 10 wt. % SV based on the reaction mixture. At least part of SV and optionally at least of part of AC and/or PI is heated in the reactor to the b.pt. of the lowest boiling component, rotation is commenced and (II), (III) and if necessary the remainder of SV, AC and/or PI are supplied (together or separately). In variants, the components initially added to the reactor also include at least part of (II) and/or (III), provided that the presence of at least part of AC and at least part of PI is essential (rather than optional) if (II) is present. An Independent claim is included for reaction mixtures (A) comprising mainly trimethylol propane triacrylate (Ia) or alkoxylated trimethylol propane triacrylate (Ib), obtained by heating at least 10 wt. % SV (based on acrylic acid (IIa) and trimethylol propane (IIIa) or alkoxylated trimethylol propane (IIIb)) in a reactor with a rotating evaporator and supplying (IIa) and (IIIa/b) in ratio 3.3-4.5:1 (the necessary amount of AC being added before dosing of (IIa) and (IIIa/b)), adjusting the temperature to 70-110 deg C, reacting for less than 20 hours, optionally washing, neutralizing, optionally washing, and removing SV by distillation and stripping until the content of (A) is less than 0.5 wt. %.

    56.
    发明专利
    未知

    公开(公告)号：DE59900932D1

    公开(公告)日：2002-04-11

    申请号：DE59900932

    申请日：1999-03-24

    Applicant: BASF AG

    Inventor： NESTLER GERHARD ,  SCHROEDER JUERGEN ,  BOLZ GERHARD

    IPC: C07C51/21 ,  C07C51/25 ,  C07C51/44 ,  C07C57/05 ,  C07C57/07 ,  C07C67/08 ,  C07C69/54

    Abstract: A process for preparing acrylic acid and/or acrylates, which comprises stage A with or without stages B and C:A: cooling a gaseous reaction mixture which comprises acrylic acid and is obtained in the gas-phase oxidation to prepare acrylic acid, using an inert high-boiling solvent, to give a gaseous mixture comprising acrylic acid;B: separating the gaseous mixture comprising acrylic acid to give a low-boiling fraction, a crude acrylic acid, and a bottom product, andC: esterifying the crude acrylic acid obtained in stage B by means of one or more alkanols to give an esterification mixture comprising one or more acrylates and one or more acetic esters.

    PROCESS FOR PREPARING N-SUBSTITUTED PYRAZOLES
    57.
    发明专利
    PROCESS FOR PREPARING N-SUBSTITUTED PYRAZOLES 未知

    公开(公告)号：BG63304B1

    公开(公告)日：2001-09-28

    申请号：BG10190897

    申请日：1997-09-24

    Applicant: BASF AG

    Inventor： MERKELE HANS R ,  FRETSCHNER ERICH ,  SCHROEDER JUERGEN

    IPC: C07D231/12 ,  C07D521/00

    Abstract: A process is disclosed for preparing N-substituted pyrazoles having the general formula in which R1 stands for C1 to C12 alkyl or C7 to C20 phenylalkyl, and R2, R3, R4 represent independently from each other hydrogen, C1 to C12 alkyl, C7 to C20 phenylalkyl or optionally substituted aryl residues, by reacting pyrazoles having the general formula 10 claims in which R2, R3 and R4 have above-said meanings, with an alcohol having the general formula R1-O-H, in which R1 has above-said meanings, at temperatures from 50 to 400oC in the presence of a catalyst. The reaction of pyrazole (II) with compound (III) is carried out in a molar ratio from 0.001:1 to 1: 1 in the liquid phase at a slight negative pressure up to an over pressure of 250 bars. Acids. their alkyl esters and/or their anhydrides are used as catalysts in a molar ratio from 0.0001: 1 to 0.5: 1 in relation to pyrazole (II). 10 claims

    Fractional condensation of acrylic acid-containing oxidation gas with acrylic acid oligomer drawn off and cracked to give acrylic acid which is fed to the quenching liquid circuit
    60.
    发明专利
    Fractional condensation of acrylic acid-containing oxidation gas with acrylic acid oligomer drawn off and cracked to give acrylic acid which is fed to the quenching liquid circuit 未知

    公开(公告)号：DE19924533A1

    公开(公告)日：2000-11-30

    申请号：DE19924533

    申请日：1999-05-28

    Applicant: BASF AG

    Inventor： SCHROEDER JUERGEN ,  NESTLER GERHARD ,  MUELLER-ENGEL KLAUS JOACHIM

    IPC: C07C51/44 ,  C07C51/487 ,  C07C57/05 ,  C07C57/07

    Abstract: The working up of acrylic acid-containing gas obtained by partial oxidation is such that the acrylic acid oligomers and/or high boilers obtained in the fractional condensation of the gas are drawn off from the fractionation column and are cracked to give acrylic acid which is then condensed and recycled to the flow circuit for quenching liquid. Production of acrylic acid by high temperature, heterogenically-catalysed partial oxidation of propane or propylene and/or acrolein with molecular O2 comprises: (i) directly cooling the acrylic acid-containing gas with a quenching liquid (I), with the non-condensed (I) being fed back (optionally over an indirectly cooling heat-exchanger (8)) to the circuit and partly removed (9); and (ii) letting the cooled gas flow up through a column (10) with e.g. bubble plates (5) etc so that it is fractionally condensed such that crude acrylic acid is drawn-off in a side outlet (12) and acrylic acid oligomer-containing sump liquid (4) and/or heavy boilers (6) are drawn off at or near the sump and used as the quenching liquid (I). The novel feature is that the drawing-off device for (I) leads to a vessel in which the oligomers are cracked at high temperature to give acrylic acid which is then condensed and recycled to the flow circuit for quenching liquid (I).

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