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    PRODUCTION OF NITROUS ESTER
    252.
    发明专利
    PRODUCTION OF NITROUS ESTER 失效

    公开(公告)号：JPH11189570A

    公开(公告)日：1999-07-13

    申请号：JP29795198

    申请日：1998-10-20

    Applicant: UBE INDUSTRIES

    Inventor： NISHIHIRA KEIGO ,  TANAKA HIDEJI ,  YOSHIDA SHINICHI

    IPC: C07C201/04 ,  C07C203/00

    Abstract: PROBLEM TO BE SOLVED: To provide a method for stably producing a nitrous ester by effectively removing heat of reaction by specifying the amount of an alcohol and the circulation amount or the like of a bottom liquid when the alcohol is reacted with nitrogen oxide in a distillation reaction column by a specific method. SOLUTION: This method for producing a nitrous ester comprising flowing down an alcohol liquid from an upper part region 2 to a lower part region 3 while supplying the alcohol liquid from an alcohol liquid-supplying line 6 to a distillation reaction column 1, taking out the bottom liquid of the distillation reaction column 1 from the bottom part 4, cooling the taken out bottom liquid by a cooler 8, recycling the cooled bottom liquid by a recycling pipe 9 so as to be flown down from the lower part 3, on the other hand, supplying a feedstock gas containing nitrogen oxide from a feedstock gas-supplying line 5 to bring the nitrogen oxide into contact with the alcohol in the distillation reaction column 1 in a countercurrent state to carry out a gas-liquid catalytic reaction to provide nitrous ester comprises regulating so that the recycling amount of the bottom liquid may be 50-300 times as much as the weight of the total supplied alcohol, the total amount of the total supplied alcohol and the alcohol amount in the bottom liquid may be 20-150 mol per 1 mol nitrogen oxide, and the alcohol concentration in the bottom liquid at the bottom part 4 may be 15-60 wt.%.

    PRODUCTION OF HIGH-PURITY ALKYL ESTER OF NITROUS ACID
    253.
    发明专利
    PRODUCTION OF HIGH-PURITY ALKYL ESTER OF NITROUS ACID 失效

    公开(公告)号：JPH04202160A

    公开(公告)日：1992-07-22

    申请号：JP33010690

    申请日：1990-11-30

    Applicant: UBE INDUSTRIES

    Inventor： NISHIHIRA KEIGO ,  TANAKA HIDEJI ,  KODAMA KUNIOKI

    IPC: C07C201/04 ,  C07C203/00

    Abstract: PURPOSE:To suppress formation of impurities and to obtain the title high-purity compound simply, inexpensively and in high yield by reacting a nitrite with an aliphatic monohydric alcohol while adjusting pH of the reaction solution with nitric acid instead of sulfuric acid. CONSTITUTION:4-6C aliphatic monofunctional alcohol is blended with an aqueous solution of an alkali metal salt (preferably sodium salt) of nitrous acid and maintained at 0-30 deg.C, preferably 0-15 deg.C while stirring. An aqueous solution of nitric acid is dripped to the mixed solution until the pH value of the water phase of the prepared reaction solution becomes 1-3. After the water phase of the prepared reaction solution is separated and removed, the organic phase is washed with water until the washed solution becomes pH >=4.

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