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    172.
    发明专利
    未知

    公开(公告)号：FR1386935A

    公开(公告)日：1965-01-22

    申请号：FR969337

    申请日：1964-04-01

    Applicant: TOYO RAYON CO LTD

    IPC: C07D201/10

    173.
    发明专利
    未知

    公开(公告)号：BE651498A

    公开(公告)日：1964-12-01

    申请号：BE651498

    申请日：1964-08-06

    IPC: C07D201/10

    Improvements in the production of epsilon-caprolactam
    174.
    发明专利
    Improvements in the production of epsilon-caprolactam 未知

    公开(公告)号：GB942968A

    公开(公告)日：1963-11-27

    申请号：GB846462

    申请日：1962-03-05

    Applicant: ALLIED CHEM

    IPC: C07D201/10

    Abstract: Caprolactam is prepared from a crude, oily hydrochloride of cyclohexanone oxime containing between 1.5 and 2 mols of hydrogen chloride per mol of oxime by stripping hydrogen chloride and volatile impurities from the crude hydrochloride in the presence of a saturated hydrocarbon liquid boiling between 65 DEG C. and 150 DEG C. at atmospheric pressure until between 1 and 1.5 mols of hydrogen chloride per mol of oxime remains and the resulting hydrochloride is crystallisable as a free flowing slurry in the remaining hydrocarbon at 15 DEG to 50 DEG C., cooling and crystallising to a free flowing slurry, mixing with sulphuric acid in a molecular ratio of 1:1 at a temperature at which hydrogen chloride is evolved, separating off the solution of oxime in sulphuric acid and subjecting the oxime to conditions of temperature and time, and a further catalyst if desired, such that Beckmann re-arrangement occurs. Concentrated sulphuric acid is preferably used and is added to the hydrochloride at a temperature between 15 DEG and 45 DEG C., and effecting the Beckmann re-arrangement at 80 DEG to 200 DEG C. The oxime hydrochloride may be obtained by reacting nitrosyl chloride with cyclohexane in the presence of actinic light.

    176.
    发明专利
    未知

    公开(公告)号：FR1319834A

    公开(公告)日：1963-03-01

    申请号：FR894569

    申请日：1962-04-16

    Applicant: STAMICARBON

    IPC: C07D201/10

    Method of producing nitroso compounds or oximes
    177.
    发明专利
    Method of producing nitroso compounds or oximes 未知

    公开(公告)号：GB903680A

    公开(公告)日：1962-08-15

    申请号：GB2520660

    申请日：1960-07-19

    Applicant: TOYO RAYON CO LTD

    IPC: C07D201/10

    Abstract: A method of producing a nitroso compound or an oxime comprises reacting a nitrosation agent with an alkane or cycloalkane containing 5-10 carbon atoms while irradiating with actinic light where sulphuric acid of above 4% W/W concentration is caused to flow over the surface of the reactor through which the light passes and with which the reaction mixture makes contact. In a preferred embodiment the reaction is carried out continuously in apparatus shown in section in the Figure in which the hydrocarbon enters the reaction zone 7 through 16 and the nitrosation agent e.g. a mixture of NOCl and HCl or a mixture of NO and Cl2, through 5. Sulphuric acid, preferably of at least 90% concentration flows over the reactor surface 4 from a reservoir 15 and a sulphuric acid solution of the product collects at 11 and is withdrawn at 12. The source of actinic light 1 and the reactor are surrounded by cooling jackets. The flow of sulphuric acid is said to allow the reaction to proceed continuously without the transmission of active light being impeded by adherence of products and by-products to the reactor wall. Examples describe the preparation of cyclohexanone oxime and dipropyl ketoxime. e -Caprolactam may be obtained by heating a sulphuric acid solution of cyclohexanone oxime obtained by this process to effect Beckmann rearrangement.

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