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    SEPARATION OF PRODUCT GAS MIXTURE OF CATALYTIC SYNTHESIS OF METHYLMERCAPTAN
    1.
    发明专利
    SEPARATION OF PRODUCT GAS MIXTURE OF CATALYTIC SYNTHESIS OF METHYLMERCAPTAN 失效

    公开(公告)号：JPH10195041A

    公开(公告)日：1998-07-28

    申请号：JP35662297

    申请日：1997-12-25

    Applicant: DEGUSSA

    Inventor： HOFEN WILLI ,  BOECK WOLFGANG DR ,  RAUTENBERG STEPHAN DR ,  SAUER JOERG DR ,  ARNTZ DIETRICH DR ,  GOEDECKE RALF DR ,  TAUGNER WOLFGANG ,  SONNENSCHEIN RAYMUND DR

    IPC: C07C319/02 ,  C07C319/28 ,  C07C321/04

    Abstract: PROBLEM TO BE SOLVED: To separate methylmercaptan, etc., in high purity and obtain a synthetic intermediate for methionine, etc., by treating a specific product gas mixture under specific conditions. SOLUTION: (i) A product gas stream is separated into an aqueous condensate 33 containing methanol and water, an organic condensate 34 containing hydrogen sulfide, methylmercaptan and dimethylsulfide and a residual gas stream 35 containing hydrogen sulfide and methylmercaptan by particle dondensation at two stages and (ii) methylmercaptan and dimethysulfide are absorbed from the residual gas stream 35 by first cleaning and (iii) hydrogen sulfide is absorbed from a released gas stream 36 by a second cleaning using methanol and (iv) hydrogen sulfide is separated from residual component of product gas mixture 27 produced in distillate fraction as a crude product of gas and (v) the crude product is distilled to separate the crude product into methylmercaptan, dimethylsulfide, dimethyl ether, polysulfide, methanol and water component.

    CONTINUOUS PRODUCTION OF METHYLMERCAPTAN
    2.
    发明专利
    CONTINUOUS PRODUCTION OF METHYLMERCAPTAN 失效

    公开(公告)号：JPH10195040A

    公开(公告)日：1998-07-28

    申请号：JP35662197

    申请日：1997-12-25

    Applicant: DEGUSSA

    Inventor： HOFEN WILLI ,  BOECK WOLFGANG DR ,  RAUTENBERG STEPHAN DR ,  SAUER JOERG DR ,  ARNTZ DIETRICH DR ,  GOEDECKE RALF DR ,  TAUGNER WOLFGANG ,  SONNENSCHEIN RAYMUND DR

    IPC: B01J21/04 ,  B01J23/30 ,  C07B61/00 ,  C07C319/08 ,  C07C321/04

    Abstract: PROBLEM TO BE SOLVED: To provide a continuous method for producing methylmercaptan useful as a synthetic intermediate for methionine, etc., capable of reducing operation energy cost by treating specific starting substance mixture under specify conditions. SOLUTION: Hydrogen sulfide-newly produced gas 20 is compressed until an intermediate pressure under addition of liquid methanol and circulated hydrogen sulfide gas is mixed with the newly produced gas and the mixture is compressed to operation pressure and further, methanol is fed to compressed gas mixture in the form of methanol vapor 24 to produce a starting substance mixture 25 having 1.1-3 molar ratio of hydrogen sulfide to methanol and the starting substance gas mixture is heated to 150-200 deg.C preheating temperature and further, the starting substance gas mixture 25 is thermally exchanged with reaction heat generated in a catalyst bed to heat the gas mixture to reaction temperature and methanol and hydrogen sulfide are reacted with the gas mixture in contact with a catalyst bed to provide methylmercaptan. It is preferable to inject excess liquid methanol and circulate unvaporized content.

    5.
    发明专利
    未知

    公开(公告)号：DE4235295A1

    公开(公告)日：1994-04-21

    申请号：DE4235295

    申请日：1992-10-20

    Applicant: DEGUSSA

    Inventor： HASSEBERG HANS-ALBRECHT DR ,  HUTHMACHER KLAUS DR ,  RAUTENBERG STEPHAN DR ,  PETSCH HEINRICH ,  WEIGEL HORST

    IPC: C07C319/20 ,  C07C323/58

    Abstract: The direct saponification of methionine nitrile obtained from methylmercaptopropionaldehyde, prussic acid and ammonia gives low yields, catalyst and educt losses and unwanted side-products. The aim of the invention is therefore to provide a method which can be carried out without isolating the intermediate products, in particular continuously, and with low losses. The ketone used is recovered in high yields after amide saponification since this liberates the ketone from side-products. In order to recover the ammonia, it is necessary for the ammonia to be substantially freed of ketone, the mixture of ammonia, ketone and water obtained being separated under pressure in a separation column. When the amide is saponified at >/= 160 DEG C, amide concentrations of less than 25 % by wt. are preferred. Methionine nitrile is produced by treatment with at least 4 equivalents of >/= 50 % by wt. ammonia at between 40 and 80 DEG C for between 5 and 60 min. Cyanide residues are destroyed by heating to over 150 DEG C. Methionine is of particular use as a feedstuff, in particular in aqueous solution.

    8.
    发明专利
    未知

    公开(公告)号：ES2154873T3

    公开(公告)日：2001-04-16

    申请号：ES97121628

    申请日：1997-12-09

    Applicant: DEGUSSA

    Inventor： HOFEN WILLI ,  BOCK WOLFGANG DR ,  RAUTENBERG STEPHAN DR ,  SAUER JORG DR ,  ARNTZ DIETRICH DR ,  GOEDECKE RALF DR

    IPC: B01J21/04 ,  B01J23/30 ,  C07B61/00 ,  C07C319/08 ,  C07C321/04

    Abstract: A process for the continuous production of methyl-mercaptan (I) comprises (i) reacting a mixture of methanol and hydrogen sulphide (H2S) in the vapour phase at 300-500 degrees C and 5-15 bar on an alumina-based catalyst bed and (ii) separating (I) from the gas mixture obtained by absorption and distillation, with recycling of unreacted methanol and H2S, removal of inert gas and waste water, and replacement of used methanol and H2S. The starting gas mixture is obtained by (a) compressing fresh H2S to an intermediate pressure (P1) with addition of liquid methanol, (b) adding the recycled H2S and compressing the mixture to operating pressure (P2), (c) adding more methanol in the form of vapour to give a compressed mixture with a mol ratio of (H2S):(methanol) = 1.1-3, (d) preheating the gas mixture to 150-200 degrees C, (e) heating to reaction temperature using the heat of reaction released on the catalyst and (f) reaction on the catalyst bed.

    9.
    发明专利
    未知

    公开(公告)号：DE19654515C1

    公开(公告)日：1998-10-01

    申请号：DE19654515

    申请日：1996-12-27

    Applicant: DEGUSSA

    Inventor： HOFEN WILLI ,  BOECK WOLFGANG DR ,  RAUTENBERG STEPHAN DR ,  SAUER JOERG DR ,  ARNTZ DIETRICH DR ,  GOEDECKE RALF DR ,  TAUGNER WOLFGANG ,  SONNENSCHEIN RAYMUND DR

    IPC: B01J21/04 ,  B01J23/30 ,  C07B61/00 ,  C07C319/08 ,  C07C321/04

    Abstract: A process for the continuous production of methyl-mercaptan (I) comprises (i) reacting a mixture of methanol and hydrogen sulphide (H2S) in the vapour phase at 300-500 degrees C and 5-15 bar on an alumina-based catalyst bed and (ii) separating (I) from the gas mixture obtained by absorption and distillation, with recycling of unreacted methanol and H2S, removal of inert gas and waste water, and replacement of used methanol and H2S. The starting gas mixture is obtained by (a) compressing fresh H2S to an intermediate pressure (P1) with addition of liquid methanol, (b) adding the recycled H2S and compressing the mixture to operating pressure (P2), (c) adding more methanol in the form of vapour to give a compressed mixture with a mol ratio of (H2S):(methanol) = 1.1-3, (d) preheating the gas mixture to 150-200 degrees C, (e) heating to reaction temperature using the heat of reaction released on the catalyst and (f) reaction on the catalyst bed.

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