Preparing alkyl ester of (meth)acrylic acid comprises supplying (meth)acrylic acid, alkanol and catalyst to reaction zone, adding discharged mixture to rectification unit, supplying a partial flow of sump stream and isolating streams

    公开(公告)号:DE102005010587A1

    公开(公告)日:2006-06-08

    申请号:DE102005010587

    申请日:2005-03-08

    Applicant: BASF AG

    Abstract: Continuous preparation of alkyl ester of (meth)acrylic acid (A) comprises supplying (meth)acrylic acid, 1-5C alkanol and acid esterifying catalyst (a) to a reaction zone (5,6); adding the discharged reaction mixture to a rectification unit (I); isolating the alkyl ester of (meth)acrylic acid containing in main stream (23) and a sump stream (22); supplying a partial flow of the sump stream; and isolating the separated sump stream (40). Continuous preparation of alkyl ester of (meth)acrylic acid (A) comprises reacting (meth)acrylic acid and 1-5C alkanol in homogeneous, liquid, solvent-free phase with increased temperature and in presence of a acid esterifying catalyst, where (meth)acrylic acid, alkanol and acid esterified catalyst are supplied to a reaction zone (5,6) (that water formed during a retention time are separated rectificative as a component of a alkanol comprising mixture in one of the reaction zone mounted rectification unit (III), in which obtained distillate is isolated in a alkanol containing organic and a water containing aqueous phase, the organic phase is led back into (III) and the aqueous phase is removed, and a reaction mixture (21) is discharged from the reaction zone); initiating the mixture into a rectification unit (I) and the alkyl ester of (meth)acrylic acid containing in main stream (23) and a sump stream (22) are isolated under addition of water; supplying a partial flow of the sump stream (22) from (I) of a residue column unit (IV) comprising a column boiler (61) and recycling into a main stream (29) in (I) and isolating the separated sump stream (40); where (IV) comprises a rectification column (62) in addition to the column boiler, and the ascending vapors from the column boiler are initiated into the rectification column, and resulting liquid at the lowest stage of the rectifying column is led into the column boiler, where the rectification column is operated in a manner, such that the water content of the resulting liquid at the lowest stage is smaller than 0.1 wt.%.

    Thermal separation process for the separation of at least one (meth)acrylic monomer enriched material stream comprises use of a device having separate volume elements and defined residence time

    公开(公告)号:DE10332758A1

    公开(公告)日:2004-05-27

    申请号:DE10332758

    申请日:2003-07-17

    Applicant: BASF AG

    Abstract: A thermal separation process for the separation of at least one (meth)acrylic monomer enriched material stream from a (meth)acrylic monomer containing mixture comprises use of a device having separate volume elements in which the liquid temperature does not differ by more than 2 degreesC and the total residence time is no greater than 20 hours. A thermal separation process for the separation of at least one (meth)acrylic monomer enriched material stream from a (meth)acrylic monomer containing mixture, comprising the continuous stationary operation of at least one thermal separation device comprising at least one separating chamber optionally containing inserts to which at least one (meth)acrylic monomer containing stream is removed whereby the material stream that is fed to the separator chamber contains x wt.% of components that are different to (meth)acrylic monomers; the material stream having the highest content by weight of (meth)acrylic monomers that is removed from the separator chamber contains y wt.% of components that are different to (meth)acrylic monomers whereby the ratio x:y is at least 5; the separator chamber, excluding inlets and outlets is bordered by a solid phase, comprises at least one recirculating heat exchanger and has a liquid phase filled total volume of at least 1 m3 whereby the temperature of the liquid phase is at least 80 degreesC; and is characterized by subdivision of the separating cavity into n individual volume elements whereby the highest and lowest temperature in the liquid phase within the separate volume elements does not differ by more than 2 degreesC; the total residence time is as defined by equation (1) and is no greater than 20 hours. tges = integral(i=1 to n) msi/mi x 2A (1) To = 100 degreesC; Ti = the arithmetic mean value of the highest and lowest temperature in i volume elements; msi = the total mass of (meth)acrylic monomers in i volume elements containing liquid phase; mi = the total liquid phase mass flow from i volume element. The total amount of liquid phase contained within dead-volume elements is not greater than 5 wt.% of the total liquid phase within the separator chamber.

    Method for the production of at least one partial propylene oxidation and/or ammoxidation product

    公开(公告)号:ZA200503358B

    公开(公告)日:2006-07-26

    申请号:ZA200503358

    申请日:2005-04-26

    Applicant: BASF AG

    Abstract: Preparation of at least one partial oxidation and/or ammoxidation product of propylene involves subjecting crude propylene (prepared by dehydrogenation or oxydehydrogenation in the presence and/or absence of oxygen) in the presence of unconverted propane as a constituent of a gas mixture 2 which comprises a total 4C-hydrocarbon content of at most 3 vol.%, to a heterogeneously catalyzed gas phase partial oxidation and/or ammoxidation. Preparation of at least one partial oxidation and/or ammoxidation product of propylene involves: (a) subjecting crude propane in the presence of and/or absence of oxygen to a homogeneously and/or a heterogeneously catalyzed dehydrogenation and/or oxydehydrogenation to obtain a propane- and propylene-containing gas mixture 1; (b) optionally removing and/or converting to other compounds a portion of the constituents other than propane and propylene contained in the gas mixture 1 to obtain a gas mixture 1' comprising propane and propylene and also compounds other than oxygen, propane and propylene; and (c) subjecting gas mixture 1 and/or gas mixture 1' as a constituent of a gas mixture 2 to a heterogeneously catalyzed gas phase partial oxidation and/or partial gas phase ammoxidation of propylene contained in gas mixture 1 and/or 1'. The total content of 4C-hydrocarbons of gas mixture 2 is at most 3 vol.%.

    15.
    发明专利
    未知

    公开(公告)号:DE50302480D1

    公开(公告)日:2006-04-27

    申请号:DE50302480

    申请日:2003-05-02

    Applicant: BASF AG

    Abstract: A process prepares an aqueous alkali metal acrylate solution by distillatively removing acrylic acid from a mixture as vapors and taking up the vapors immediately from the gas phase into an aqueous alkali solution.

    Heterogeneously catalyzed partial gas phase oxidation of propene to acrylic acid, useful for the production of adhesive, comprises use of a gas phase mixture having a molar ratio of oxygen to propene of 1.5-2.5

    公开(公告)号:DE10313209A1

    公开(公告)日:2004-03-04

    申请号:DE10313209

    申请日:2003-03-25

    Applicant: BASF AG

    Abstract: A process for the heterogeneously catalyzed partial gas phase oxidation of propene to acrylic acid by passage of a gas phase mixture comprising 6-15 vol.% propene, 4-20 vol. % water and no greater than 10 vol. % of other components as well as molecular oxygen such that the molar ratio of oxygen to propene is 1.5-2.5 and the residual amount to 100 vol.% comprises molecular nitrogen though a first reaction stage. A process for the heterogeneously catalyzed partial gas phase oxidation of propene to acrylic acid by passage of a gas phase mixture (I) comprising propene, molecular oxygen and at least one inert gas having a molar ratio of oxygen to propene of at least 1. The process involves a first reaction stage at elevated temperature having a fixed catalyst bed of ring shaped catalyst having a multimetal oxide active material of formula (1). The catalyst has a volume specific activity in the flow direction of the mixture (I) which is either constant or at least increases once and the active mass composition does not change over the bed packing such that the conversion of propene is at last 90 mol.% in a single pass with a selectivity to acrolein and acrylic acid of at least 90 mol.% with direct or indirect cooling of the product mixture leaving the first reaction stage. Optional addition of molecular oxygen and/or inert gas and the product mixture comprising acrolein, molecular oxygen and at least one inert gas having a molar ratio of oxygen to acrolein of at least 0.5 is passed through a second reaction stage comprising a second fixed bed catalyst packing comprising ring shaped packing whose active mass comprises a multimetal oxide of formula (2). Multimetal oxide (2) whose volume specific activity in the direction of flow at least increases once and whose composition does not alter over the second reaction stage such that the single-pass conversion of acrolein is at least 90 mol.% and the selectivity of both reaction stages to the formation of acrylic acid (with respect to reacted propene) is at least 80 mol.% is characterized in that the reaction mixture (I) comprises 6-15 vol.% propene, 4-20 vol.% water and no greater than 10 vol. % of other components that are not propene, water, oxygen or nitrogen, as well as molecular oxygen such that the molar ratio of oxygen to propene is 1.5-2.5 and the residual amount to 100 vol.% comprises molecular nitrogen. Mo12X1aX2bX3cX4dX5eOn (1) Mo12VfX6gX7hOm (2) X1 = Bi, Co or Ni; X2 = W or Nb; X3 = Fe or Cr; X4 = K, Cs or Sr; X5 = Si, Al or Zr; X6 = W or Nb; X7 = Sb, Cu, Ni or Fe; a = 5-10; b = 0-4; c = 2-5; d = 0.02-0.15; e = 0.5-4; f = 1-5; g = 1-2; h = 1-4; m, n = number of O atoms dependent upon the valency and number of elements.

    20.
    发明专利
    未知

    公开(公告)号:AT356794T

    公开(公告)日:2007-04-15

    申请号:AT02774555

    申请日:2002-09-03

    Applicant: BASF AG

    Abstract: (Meth)acrylates are prepared by reacting (meth)acrylic acid with an alcohol in the presence of at least one acidic catalyst and at least one polymerization inhibitor in a reaction zone b) consisting of at least one reactor b1) having at least one connected distillation unit b2), by a process in which in reactor b1), the temperature is brought to from 120 to 150° C. and the desired (meth)acrylic acid: alcohol stoichiometry is established, the distillate of the distillation unit b2) is treated with a wash liquid (wash step c)), the discharge from the wash step c) is separated into at least one organic phase c1) and at least two aqueous phases c2) and c3), the organic phase c1) is passed partly as reflux into the distillation unit b2) and partly, without further scrubbing, into a purification b) of the (meth)acrylate by distillation and the aqueous phases c2) and c3) are passed at least partly into an alcohol recovery d).

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