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    PRODUCTION OF CRYSTALLINE SOLID FROM GLYCINE-N,N-DIACETIC DERIVATIVE HAVING SUFFICIENTLY LOW HYGROSCOPIC PROPERTY
    1.
    发明专利
    PRODUCTION OF CRYSTALLINE SOLID FROM GLYCINE-N,N-DIACETIC DERIVATIVE HAVING SUFFICIENTLY LOW HYGROSCOPIC PROPERTY 失效

    公开(公告)号：JPH10175929A

    公开(公告)日：1998-06-30

    申请号：JP32491397

    申请日：1997-11-26

    Applicant: BASF AG

    Inventor： SCHOENHERR MICHAEL DR ,  RAULS MATTHIAS DR ,  ASCHERL HERMANN ,  LETZELTER THOMAS ,  BAUMANN DIETER ,  POTTHOFF-KARL BIRGIT DR

    IPC: C11D1/04 ,  C07C227/42 ,  C07C229/16 ,  C07C229/24

    Abstract: PROBLEM TO BE SOLVED: To obtain a crystalline solid of the subject compound substantially not containing an additive and having virtually sufficiently low hygroscopic property. SOLUTION: This crystalline solid constituted of a glycine-N,N-diacetic acid derivative represented by formula I [R is a 1-30C alkyl or a 2-30C alkenyl, a group of formula II (A is a 1-12C alkylene bridge, etc.; M is H or an alkali metal, etc.), etc.] is produced by distilling away water content of an aqueous solution of (A) glycine-N,N-diacetic acid derivative I [R is a 1-20C alkyl or a group of formula II, etc.] as a starting substance. Crystallization is carried out by adding a crystalline component A in an amount of 0.001-50wt.%, preferably 0.01-10wt.% based on an amount of the component A in a starting substance as a nucleus for crystallization and the crystallization temperature is controlled to 10-100 deg.C, especially 40-80 deg.C. The resultant crystalline solid has a purity of 70-99.9%, especially 80-99.5% based on total amount of solid.

    PRODUCTION OF GUANIDINE DERIVATIVE
    2.
    发明专利
    PRODUCTION OF GUANIDINE DERIVATIVE 失效

    公开(公告)号：JP2000191625A

    公开(公告)日：2000-07-11

    申请号：JP36247499

    申请日：1999-12-21

    Applicant: BASF AG

    Inventor： KESSEL KNUT ,  KLUGE MICHAEL DR ,  GREINDL THOMAS DR ,  BOGENSTAETTER THOMAS DR ,  SCHERR GUENTER DR ,  RAULS MATTHIAS DR ,  VAN GELDER RICHARD

    IPC: C07C277/08 ,  C07C279/14 ,  C07C303/22 ,  C07C309/15 ,  C07F9/38

    Abstract: PROBLEM TO BE SOLVED: To readily obtain a guanidine derivative in a high purity, high yield and narrow particle size distribution by reacting O-alkyl isourea salt with a specific amine in the presence of a seed crystal of a guanidine derivative. SOLUTION: This guanidine derivative (A) is expressed by formula I [R1 is a 1-8C alkylene or a 5-10C bifunctional alicyclic group; R2 is H or a 1-8C alkyl; Z is COOR3, SO2R3 (R3 is H, an alkali metal or the like) or the like] and is obtained by reacting (B) an O-alkyl isourea salt of formula II (R5 is a 1-8C alkyl; X- is 1 equivalent of anion) with (C) an amine of formula III in the presence of (D) a seed crystal of a guanidine of formula I. Preferably, the reaction is performed in a reaction chamber in which the components B and C are continuously introduced and thereafter the crystal of the component D is continuously taken out.

    PRODUCTION OF PURE TRIETHYLENEDIAMINE SOLUTION
    3.
    发明专利
    PRODUCTION OF PURE TRIETHYLENEDIAMINE SOLUTION 失效

    公开(公告)号：JP2001064281A

    公开(公告)日：2001-03-13

    申请号：JP2000221322

    申请日：2000-07-21

    Applicant: BASF AG

    Inventor： RIECHERS HARTMUT ,  HOEHN ARTHUR ,  SIMON JOACHIM ,  LANG ORTMUND ,  SCHOENMAKERS HARTMUT ,  RAULS MATTHIAS DR ,  CLAERBOUT KOEN

    IPC: C07D471/08 ,  C07D487/08

    Abstract: PROBLEM TO BE SOLVED: To provide an effective and economical method for producing pure triethylenediamine(TEDA) and its solution. SOLUTION: This method for producing pure triethylenediamine solution comprises evaporating triethylenediamine and introducing the gas state triethylenediamine into a liquid solvent. The gaseous triethylendiamine is obtained from the top of a column or its side discharging port. Further, the pure triethylenediamine solution is produced by following the above method and then crystallizing the triethylenediamine from the solution. The liquid solvent is selected from the group consisting of cyclic or non-cyclic hydrocarbons, chlorinated aliphatic hydrocarbons, aromatic hydrocarbons, alcohols, ketones, aliphatic carboxylic acid esters, aliphatic nitriles and ethers.

    4.
    发明专利
    未知

    公开(公告)号：AT202075T

    公开(公告)日：2001-06-15

    申请号：AT97119147

    申请日：1997-11-03

    Applicant: BASF AG

    Inventor： SCHOENHERR MICHAEL DR ,  RAULS MATTHIAS DR ,  ASCHERL HERMANN ,  LETZELTER THOMAS ,  BAUMANN DIETER ,  POTTHOFF-KARL BIRGIT DR

    IPC: C11D1/04 ,  C07C227/42 ,  C07C229/16 ,  C07C229/24

    Abstract: A method for the preparation of a crystalline solid comprising a glycine-N,N-diacetic acid derivative of formula (I) with a very low hygroscopicity, comprises fixing the water content of the starting material containing (I) at 10-30 wt.% and then carrying out crystallisation: MOOC-CH(R)-N(CH2COOM)2 (I) R = 1-30C alkyl or 2-30C alkenyl (both optionally containing 1-5 OH, formyl, 1-4C alkoxy(carbonyl) or phenoxy groups and/or optionally containing up to 5 non-adjacent O atoms in the chain), alkoxylate groups of formula (II), phenyl-(1-20 C)-alkyl (optionally containing up to 3 1-4C alkyl, OH, carboxyl, sulpho or 1-4C alkoxycarbonyl ring substituents), 5- or 6-membered optionally benzalated heterocyclic ring containing up to 3 N, O or S atoms (optionally containing up to 3 1-4C alkyl, OH, carboxyl, sulpho or 1-4C alkoxycarbonyl substituents) or a group of formula (III): -(CH2)k-O-(A O)m-(A O)n-Y (II) -A-CH(COOM)-N(CH2COOM)2 (III) A , A = 2-4C 1,2-alkylene; Y = H, 1-12C alkyl, phenyl or 1-4C alkoxycarbonyl; k = 1-3; m, n = 0-50; A = 1-12C alkylene or single bond; and M = H, alkali(ne earth) metal or optionally substituted ammonium, with the provision that m+n = at least 4.

    7.
    发明专利
    未知

    公开(公告)号：ES2160992T3

    公开(公告)日：2001-11-16

    申请号：ES98104396

    申请日：1998-03-11

    Applicant: BASF AG

    Inventor： SCHLAFER DIETER DR ,  MAUSS MICHAEL DR ,  RAULS MATTHIAS DR ,  BAUMANN DIETER

    IPC: C01D1/30

    Abstract: Production of crystalline NaOH . 3.5H2O, involves crystallising NaOH.3.5H2O from an aqueous NaOH solution oversaturated with NaOH . 3.5H2O, and removing the crystals using a mechanical solid/liquid separator. The solid/liquid separation occurs under conditions in which crystalline NaOH.3.5H2O can be liberated from the lye residues; the NaCl content of the crystalline NaOH . 3.5H2O being ≤ 100 mg per kg.

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