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

    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

    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. %.

    24.
    发明专利
    未知

    公开(公告)号:BR9808158A

    公开(公告)日:2000-03-28

    申请号:BR9808158

    申请日:1998-03-05

    Applicant: BASF AG

    Abstract: The invention relates to a method for extracting an aqueous solution containing (meth)acrylic acid. Said solution is brought into contact with a solution containing at least one extracting agent which can be converted into (meth)acrylic acid and forms a miscibility gap with the aqueous solution to produce an organic phase containing (meth)acrylic acid and extraction agent and an aqueous phase.

    25.
    发明专利
    未知

    公开(公告)号:ID21820A

    公开(公告)日:1999-07-29

    申请号:ID990084

    申请日:1997-09-18

    Applicant: BASF AG

    Abstract: In the preparation of esters of acrylic or methacrylic acid by esterification with alcohols, the interfering deposits formed on the apparatus parts by relatively high molecular weight by-products can be avoided, removed or lessened by allowing a liquid partly or wholly consisting of the alcohol used for the esterification to act on the deposits, fouled apparatus parts or on the surfaces of the apparatus parts on which deposits are easily formed, with preference being given to wetting the deposits or surfaces using suitable nozzles or cleaning sprayers.

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