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    PRODUCTION OF 2-HYDROXYALKYL (METH)ACRYLATE
    81.
    发明专利
    PRODUCTION OF 2-HYDROXYALKYL (METH)ACRYLATE 失效

    公开(公告)号：JPS6327457A

    公开(公告)日：1988-02-05

    申请号：JP16967686

    申请日：1986-07-21

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KANBARA YOSHIHIKO ,  ASANO SHIRO ,  ISOZAKI WATARU ,  ASAO KOICHI ,  FUKADA ISAO

    IPC: C07C69/54 ,  C07C67/26 ,  C07C67/54

    Abstract: PURPOSE:To easily obtain the titled vinyl monomer compound on a commercial base, by reacting acrylic acid, etc., with an alkylene oxide in the presence of a catalyst and a nitric acid (salt) as a polymerization inhibitor using a reactor made of a stainless steel for commercial production apparatus. CONSTITUTION:The objective compound can be produced by reacting acrylic acid or methacrylic acid with an alkylene oxide in the presence of a catalyst such as quaternary ammonium salt and nitric acid or nitric acid salt as a polymerization inhibitor using a reaction apparatus and distillation apparatus made of stainless steel and distilling and refining the liquid obtained by the above synthetic reaction. The apparatus used in the above reaction is partly or wholly made of a stainless steel, preferably an austenitic steel such as SUS-304, 316, etc., from the viewpoint of availability and processability. The amount of the nitric acid or nitric acid salt added as a polymerization inhibitor is preferably 50-500ppm based on 2-hydroxyalkyl (meth)acrylate.

    PRODUCTION OF (METH)ACRYLAMIDE
    82.
    发明专利
    PRODUCTION OF (METH)ACRYLAMIDE 失效

    公开(公告)号：JPS61221160A

    公开(公告)日：1986-10-01

    申请号：JP6083085

    申请日：1985-03-27

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： ASANO SHIRO ,  TOKUNAGA MAREO ,  KANBARA YOSHIHIKO

    IPC: C07B61/00 ,  B01J25/00 ,  C07C67/00 ,  C07C231/00 ,  C07C231/06 ,  C07C233/09

    Abstract: PURPOSE:To produce (meth)acrylamide economically, suppressing the production of by-products, by hydrating (meth)acrylonitrile in the presence of a mixed catalyst produced by the simultaneous development and regeneration of a Raney- copper catalyst. CONSTITUTION:Acrylamide or methacrylamide is produced by hydrating acrylonitrile or methacrylonitrile at 70-150 deg.C, preferably 90-140 deg.C using a liquid-phase suspension bed of a Raneycopper catalyst. The Raney-copper catalyst is produced by developing a Raney-copper alloy with an aqueous solution of a basic compound such as sodium hydroxide, dissolving the soluble component (e.g. aluminum) from the alloy, and removing the dissolved compound and the most part of the excessive basic compound by washing with water, etc. A mixed catalyst can be produced by developing the Raney-copper alloy while mixing with the catalyst used for a long period. The used catalyst can be regenerated simultaneously to the development of the alloy.

    PRODUCTION OF ACRYLAMIDE
    86.
    发明专利
    PRODUCTION OF ACRYLAMIDE 失效

    公开(公告)号：JPS63203654A

    公开(公告)日：1988-08-23

    申请号：JP3348587

    申请日：1987-02-18

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KANBARA YOSHIHIKO ,  ASANO SHIRO ,  ISOZAKI WATARU ,  ASAO KOICHI

    IPC: C07B61/00 ,  C07C67/00 ,  C07C231/00 ,  C07C231/06 ,  C07C233/09

    Abstract: PURPOSE:To produce acrylamide preventing the lowering of catalytic activity with time, deterioration of filterability of catalyst and lowering of quality of produced monomer, by reacting acrylonitrile with water in the presence of a copper-based catalyst, nitric acid radical and (meth)acrylic acid radical. CONSTITUTION:Acrylonitrile is reacted with water in the presence of suspended copper-based catalyst at 50-200 deg.C, preferably 70-130 deg.C. The reaction is carried out by adding 5-50ppm of nitric acid or nitric acid radical in terms of nitric acid radical based on the raw material liquid and adding (meth)acrylic acid radical in a manner that 6-20 times equivalent of the (meth)acrylic acid radical based on the nitric acid radical is constantly present in the reaction liquid. The reactor used in the reaction is an inner filter-type reactor having a catalyst filter in the reaction zone. The amounts of various impurities can be reduced and the amount of expensive copper-based catalyst can be decreased to less than half of the conventional process.

    PRODUCTION OF PYRUVIC ACID OR PYRUVIC ACID ESTER
    87.
    发明专利
    PRODUCTION OF PYRUVIC ACID OR PYRUVIC ACID ESTER 失效

    公开(公告)号：JPS63126840A

    公开(公告)日：1988-05-30

    申请号：JP27280786

    申请日：1986-11-18

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： ARASHIBA NOBUMASA ,  ASANO SHIRO ,  ONO KYOKO

    IPC: C07C67/313 ,  B01J23/44 ,  C07B61/00 ,  C07C51/373 ,  C07C59/19 ,  C07C69/716

    Abstract: PURPOSE:To easily obtain the titled compound from a raw material available at a low cost, in two steps in high yield using an industrially valuable process, by oxidizing methacrylic acid or its ester with ozone and hydrogenating the reaction product using a palladium catalyst at a specific temperature. CONSTITUTION:Methacrylic acid or a methacrylic acid ester is dissolved in an alcohol solvent such as methanol to a concentration of 0.1-40wt%. The solution is oxidized with preferably 1.05-1.5mol of ozone based on 1mol of the methacrylic acid or its ester and the obtained reaction liquid is hydrogenated at

    PRODUCTION OF GLYOXYLIC ACID
    88.
    发明专利
    PRODUCTION OF GLYOXYLIC ACID 失效

    公开(公告)号：JPS6383043A

    公开(公告)日：1988-04-13

    申请号：JP22500486

    申请日：1986-09-25

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： ARASHIBA NOBUMASA ,  ASANO SHIRO ,  SAKAMOTO TOSHIHIKO

    IPC: B01J27/053 ,  B01J23/74 ,  B01J23/745 ,  B01J27/00 ,  C07B61/00 ,  C07C51/285 ,  C07C59/153

    Abstract: PURPOSE:To obtain the titled compound useful as an intermediate for various chemicals such as drug modulator, cosmetic, etc., from glyoxal as a raw material, to improve selectivity, by separately adding an aqueous solution of hydrogen peroxide and ferrous ion to a reaction mixture. CONSTITUTION:An aqueous solution of hydrogen peroxide and ferrous ion are separately added to glyoxal of raw material, which is oxidized to give the aimed compound. 5-60wt% aqueous solution of hydrogen peroxide is preferably used and preferably the aqueous solution of hydrogen peroxide as an oxidizing agent is added to glyoxal. Ferrous sulfate, etc., are used as the ferrous ion and preferably added continuously or intermittently during the reaction process. The amount of the ferrous ion used is >=about 0.01mol, preferably about 0.5mol based on 1mol glyoxal. The reaction is preferably carried out at 0-30 deg.C while preventing the reaction system from coming into contact with a gas phase containing molecular oxygen such as air, etc.

    PRODUCTION OF GLYOXYLIC ACID
    89.
    发明专利
    PRODUCTION OF GLYOXYLIC ACID 失效

    公开(公告)号：JPS62298552A

    公开(公告)日：1987-12-25

    申请号：JP13921186

    申请日：1986-06-17

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： ARASHIBA NOBUMASA ,  ASANO SHIRO ,  ONO KYOKO

    IPC: C07C59/153 ,  C07C51/00 ,  C07C51/34 ,  C07C67/00

    Abstract: PURPOSE:In oxidizing maleic acid with ozone in an alcoholic solvent, reducing the resultant substance in the presence of a catalyst and hydrolyzing, to obtain the titled compound useful as an intermediate for various chemical products such as drug modifier, agricultural chemicals, etc., in high yield, by carrying out the reduction reaction under specific hydrogen partial pressure. CONSTITUTION:Maleic acid is oxidized with ozone in an alcoholic solvent such as methyl alcohol, etc. Then, the resultant substance is reduced in the presence of a hydrogenating catalyst at hydrogen partial pressure of >=3.0kg/cm (pressure particularly has no upper limitation; however, too high-pressure pressurizing with hydrogen is not required) absolute pressure at

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