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    PROCESS FOR PURIFYING AND RECOVERING THE CONTAMINATED CATALYST SOLUTION ARISING IN THE CARBONYLATION OF METHANOL AND/OR METHYL ACETATE AND/OR DIMETHYL ETHER
    33.
    发明专利
    PROCESS FOR PURIFYING AND RECOVERING THE CONTAMINATED CATALYST SOLUTION ARISING IN THE CARBONYLATION OF METHANOL AND/OR METHYL ACETATE AND/OR DIMETHYL ETHER 未知

    公开(公告)号：CA2012567C

    公开(公告)日：1994-08-30

    申请号：CA2012567

    申请日：1990-03-20

    Applicant: HOECHST AG

    Inventor： ERPENBACH HEINZ ,  LORK WINFRIED ,  WEFERLING NORBERT ,  PRINZ PETER

    IPC: B01J38/00 ,  B01J31/40 ,  C07B61/00 ,  C07C27/00 ,  C07C51/12 ,  C07C51/42 ,  C07C51/48 ,  C07C51/56 ,  C07C51/573 ,  C07C53/08 ,  C07C53/12 ,  C07C67/36 ,  C07C67/37 ,  C07C67/48 ,  C07C67/58 ,  C07C69/16 ,  B01J38/50

    Abstract: In the process for purifying and recovering the contaminated catalyst solution arising in the carbonylation of methanol and/or methyl acetate and/or dimethyl ether and containing carbonyl complexes of rhodium, quaternary organophosphorus compounds as organic promoters, undistillable organic impurities as well as acetic acid, acetic anhydride and ethylidene diacetate, the carbonyl complex of rhodium as well as acetic acid, acetic anhydride and ethylidene diacetate are extracted from the contaminated catalyst solution by means of a tri-C3- to C8-alkylphosphane and the trialkylphosphane phase is separated from the promoter phase freed of rhodium and containing the organic impurities; the trialkylphosphane phase is separated into the volatile constituents acetic acid, acetic anhydride and ethylidene diacetate as well as trialkylphosphane and the rhodium carbonyl complex remaining as the residue and the recovered trialkylphosphane is used for further extraction; the contaminated promoter phase, freed of the rhodium carbonyl complex, is freed of the organic impurities by extraction with dialkyl ethers, carboxylic acid esters or hydrocarbons and, after the extractant phase has been separated off, recombined with the recovered acetic acid/acetic anhydride and ethylidene diacetate mixture and with the rhodium carbonyl complex and recycled to the carbonylation reactor; finally, the impurities remaining as the residue from a distillation of the extractant phase which has been separated off are removed from the system.

    PROCESS FOR THE PREPARATION OF TERTIARY PHOSPHINES
    34.
    发明专利
    PROCESS FOR THE PREPARATION OF TERTIARY PHOSPHINES 未知

    公开(公告)号：GB2262284A

    公开(公告)日：1993-06-16

    申请号：GB9225936

    申请日：1992-12-11

    Applicant: HOECHST AG

    Inventor： STELZER OTHMAR ,  LANGHANS KLAUS PETER ,  WEFERLING NORBERT

    IPC: C07F9/50 ,  C07F9/58

    Abstract: Tertiary phosphines of the formula R'PR2 or R2P-[CH2]3-PR2 in which R is an aryl, pyridyl or arylsulfonic acid group and R' is an aryl, arylsulfonic acid or n-butyl group, are prepared by reading phosphines of the formula HnPR"3-n or H2P-[CH2]3-PH2 in which R" is hydrogen or an n-butyl, aryl or pyridyl group and n is 1 or 2 with a halogen compound of the formula X-R, in which R has the abovememtioned meaning and X is fluorine, chlorine or bromine, in the presence of powdered potassium hydroxide and dimethyl sulfoxide and/or dimethoxyethane at temperatures between 0 and 100 DEG C, at least 1 mol of potassium hydroxide being used per mol of halogen compound.

    PROCESS FOR MAKING CHLOROPHOSPHINES AND THIOPHOSPHINIC ACID CHLORIDES, AND NOVEL 9-CHLORO-9- THIOXO-9-PHOSPHABICYCLONONANES
    40.
    发明专利
    PROCESS FOR MAKING CHLOROPHOSPHINES AND THIOPHOSPHINIC ACID CHLORIDES, AND NOVEL 9-CHLORO-9- THIOXO-9-PHOSPHABICYCLONONANES 未知

    公开(公告)号：CA1283664C

    公开(公告)日：1991-04-30

    申请号：CA518448

    申请日：1986-09-18

    Applicant: HOECHST AG

    Inventor： WEFERLING NORBERT ,  KLOSE WERNER

    IPC: C07F9/34 ,  C07F9/52 ,  C07F9/6568 ,  C07F9/28

    Abstract: PROCESS FOR MAKING CHLOROPHOSPHINES AND THIOPHOSPHINIC ACID CHLORIDES, AND NOVEL 9-CHLORO-9-THIOXO-9-PHOSPHABI- CYCLONONANES Chlorophosphines or thiophosphinic acid chlorides of the general formulae RPCl2, R2PCl or R2P(=S)Cl are made from feed materials selected from hydrogen-functional primary or secondary phosphines or secondary phosphine sulfides, where R stands for identical or different, linear or branched, substituted or unsubstituted alkyl radicals having from 1 - 16 carbon atoms, aryl radicals, aralkyl radicals or alkylaryl radicals having from 6 - 9 carbon atoms or cycloalkyl radicals having from 5 - 10 carbon atoms. To this end, the feed materials are reacted with phosphorus pentachloride, or with chlorine gas in the presence of phosphorus trichloride at temperatures within the range -78 to +145.degree.C. It is possible for two radicals R to be linked together by one or two substituted or unsubstituted hydrocarbon chains having from 1 - 4 carbon atoms.

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