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    Apparatus for the continuous carrying out heterogeneous catalytic reaction in liquid phase
    1.
    发明授权
    Apparatus for the continuous carrying out heterogeneous catalytic reaction in liquid phase 失效
    连续在液相中进行异构催化反应的装置

    公开(公告)号：US3901660A

    公开(公告)日：1975-08-26

    申请号：US41139073

    申请日：1973-10-31

    Applicant: HOECHST AG

    Inventor： OHORODNIK ALEXANDER ,  SENNEWALD KURT ,  HUNDECK JOACHIM ,  STUTZKE PAUL

    IPC: B01J8/00 ,  B01J8/18 ,  B01J8/22 ,  C07C51/377 ,  C07C53/16

    CPC classification number: B01J8/228 ,  B01J8/006 ,  B01J8/1836 ,  B01J2208/00176 ,  C07C51/377 ,  C07C53/16

    Abstract: Heterogeneous catalytic reactions are carried out continuously in liquid phase. A substantially uniform suspension of liquid starting material and fine particulate catalyst together with resulting reaction product is continuously conveyed upwardly in a reaction zone by the introduction, in accordance with the principle of an airlift pump, of a gas or vaporous material near the bottom of the reaction zone, and recycled downwardly through a reflux line to the bottom of the reaction zone. The path of liquid material through the reflux line is interrupted by an injector system situated in a closed catalyst-separating zone containing reaction product. Following establishment of the reaction equilibrium, starting material is continuously supplied near the bottom of the reaction zone and crude but catalyst-free reaction product continuously removed near the head of the catalyst-separating zone. Reaction product which is to be removed is caused to travel through the catalyst-separating zone with the injector system therein towards the reaction product outlet at a velocity smaller than the sedimentation velocity of the catalyst under the prevailing operational conditions.

    Process for the manufacture of acrylic acid esters
    2.
    发明授权
    Process for the manufacture of acrylic acid esters 失效
    制备丙烯酸酯的方法

    公开(公告)号：US3882167A

    公开(公告)日：1975-05-06

    申请号：US36386373

    申请日：1973-05-25

    Applicant: HOECHST AG

    Inventor： LOHMAR ELMAR ,  OHORODNIK ALEXANDER ,  GEHRMANN KLAUS ,  STUTZKE PAUL

    IPC: C07C69/54 ,  B01J8/22 ,  B01J19/18 ,  C07C67/08

    CPC classification number: B01J19/1862 ,  B01J8/228 ,  B01J2219/00094 ,  B01J2219/00101 ,  C07C67/08 ,  Y10S203/06 ,  C07C69/54

    Abstract: Improved process permitting heterogeneous catalytic reactions to be carried out continuously in liquid phase, wherein a suspension of liquid starting material and fine particulate catalyst together with resulting reaction product is continuously conveyed upwardly in a reaction zone, in accordance with the principle underlying an airlift pump, by the introduction of a gas into, near the bottom of, the reaction zone, and recycled downwardly through a by-pass reflux line to the bottom of the reaction zone, the recycled liquid material passing through an injector system interrupting its flow, the said system being situated in the bypass reflux line in a closed catalyst-separating zone containing reaction product; wherein, following establishment of the reaction equilibrium, starting material is continuously supplied to the reaction zone and crude, catalyst-free reaction product is removed near the head of the catalyst-separating zone; wherein reaction product, which is to be removed from the catalystseparating zone, is caused to flow upwardly through the catalystseparating zone with the injector system therein towards the reaction product outlet at velocity smaller than the sedimentation velocity of the catalyst in the catalyst-separating zone under the operational conditions prevailing. The improved process is more particularly used for esterifying arcylic acid in contact with an acid ion exchanger as a catalyst, at elevated temperature and under pressures substantially between 0.01 and 1 atmosphere absolute. To this end, the reaction zone is continuously supplied with a starting mixture of acrylic acid and an alkanol having between 4 and 6 carbon atoms; an inert gas is introduced into, near the bottom of, the reaction zone; the resulting suspension is heated to boiling; an azeotropic mixture of water originating from the esterification, alkanol and/or ester, is distilled off in a distillation zone placed directly above the head of the reaction zone; the azeotropic mixture is condensed and separated into a specifically lighter, predominantly organic phase and into a specifically heavier, predominantly aqueous phase, the organic phase being recycled to the head of the distillation zone and/or to the reaction zone; and resulting crude alkyl acrylate is removed near the head of the catalyst-separating zone.

    Abstract translation: 改进的方法允许在液相中连续进行非均相催化反应，其中根据空气提升泵的原理，液体原料和细颗粒催化剂的悬浮液与所得反应产物一起在反应区中向上连续输送， 通过将气体引入到反应区的底部附近，并通过旁路回流管向下循环到反应区的底部，再循环的液体材料通过一个中断其流动的喷射器系统，所述的 系统位于包含反应产物的封闭催化剂分离区中的旁路回流管线中; 其中，在建立反应平衡之后，将原料连续地供应到反应区，在催化剂分离区的头部附近除去粗的无催化剂的反应产物; 其中将从催化剂分离区除去的反应产物通过其中的注射器系统向上流过催化剂分离区，其速度小于催化剂中催化剂的沉降速度朝向反应产物出口 分区在现行的运行条件下。

    3.
    发明专利
    未知

    公开(公告)号：CH620448A5

    公开(公告)日：1980-11-28

    申请号：CH804876

    申请日：1976-06-23

    Applicant: HOECHST AG

    Inventor： OHORODNIK ALEXANDER DR ,  LOHMAR ELMAR DR ,  GEHRMANN KLAUS DR ,  STUTZKE PAUL

    IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  C07F9/28

    Abstract: Continuous production of 2,5-dioxo-1-oxa-2-phospholanes of the general formula from a beta-halogenoformyl-ethyl phosphinic acid halide of the general formula R1XP(O)-CHR2-CHR3-CO-X in which formula R1 stands for an alkyl radical having 1, 2, 3 or 4 carbon atoms, or a phenyl radical, R2 and R3 each stands for hydrogen or CH3, and X stands for chlorine or bromine, by reacting the said acid halide with acetic anhydride. The phospho lanes are produced by introducing, into a heatable circulation reactor, an initial quantity of the desired 2,5-dioxo-1-oxa-2-phospholane and circulating it therein at a temperature of 110 DEG to 190 DEG C; separately preheating the respective beta-halogenoformyl-ethyl phosphonic acid halide and acetic anhydride starting materials to a temperature of 60 DEG to 160 DEG C; mixing these starting materials together and continuously adding the resulting mixture to the material circulated in the reactor, the mixture being introduced into the lower third of the reactor; distilling off resulting acetyl halide near the head of the circulation reactor, a pressure difference 0.1 to 5 bar, being established between the point of introduction of the mixture of starting materials and the overflow level in the circulation reactor, and the material being kept circulating by the evaporating acetyl halide; and removing the resulting desired 2,5-dioxo-1-oxa-2-phospholane from the reactor at a location which is below that at which the acetyl halide is distilled off.

    6.
    发明专利
    未知

    公开(公告)号：DE2648005A1

    公开(公告)日：1978-04-27

    申请号：DE2648005

    申请日：1976-10-23

    Applicant: HOECHST AG

    Inventor： AUER EBERHARD DIPL CHEM DR ,  OHORODNIK ALEXANDER DIPL CHEM ,  STUTZKE PAUL

    IPC: C07F9/30

    Abstract: Production of N-substituted 2-carbamoyl phosphinic acids of the general formula: (I) in which R1 stands for an alkyl group having 1 to 4 carbon atoms or an aryl group; R2 and R3 stand independently of each other for an alkyl group having 1 to 4 carbon atoms, an aryl group or a hydrogen atom; R4 stands for an alkyl group having 1 to 18 carbon atoms, an aryl group or a hydrogen atom; and R5 stands for an alkyl group having 1 to 18 carbon atoms or an aryl group. More specifically, a 2-chloroformyl phosphinic acid chloride of the general formula (II) is reacted at 120 DEG to 170 DEG C with an amine of the general formula (III) and resulting N-substituted 2-carbamoyl phosphinic acid chloride of the general formula (IV) the latter compound being obtained while hydrogen chloride is split off, is hydrolyzed with water.

    PRODUCTION OF N-SUBSTITUTED 2-CARBAMOYL PHOSPHINIC ACIDS
    8.
    发明专利
    PRODUCTION OF N-SUBSTITUTED 2-CARBAMOYL PHOSPHINIC ACIDS 未知

    公开(公告)号：CA1081708A

    公开(公告)日：1980-07-15

    申请号：CA288992

    申请日：1977-10-19

    Applicant: HOECHST AG

    Inventor： AUER EBERHARD ,  OHORODNIK ALEXANDER ,  STUTZKE PAUL

    IPC: C07F9/30

    Abstract: PRODUCTION OF N-SUBSTITUTED 2-CARBAMOYL PHOSPHINIC ACIDS. Production of N-substituted 2-carbamoyl phosphinic acids of the general formula: (I) in which R1 stands for an alkyl group having 1 to 4 carbon atoms or an aryl group; R2 and R3 stand independently of each other for an alkyl group having 1 to 4 carbon atoms, an aryl group- or a hydrogen atom; R4 stands for an alkyl group having 1 to 18 carbon atoms, an aryl group or a hydrogen atom; and R5 stands for an alkyl group having 1 to 18 carbon atoms or an aryl group. More specifically, a 2-chloroformyl phosphinic acid chloride of the general formula (II) is reacted at 120 to 170.degree.C with an amine of the general formula (III) and resulting N-substituted 2-carbamoyl phosphinic acid chloride of the general formula (IV) the latter compound being obtained while hydrogen chloride is split off, is hydrolyzed with water.

    CONTINUOUS PRODUCTION OF 2,5-DIOXO-1-OXA-2-PHOSPHOLANES
    9.
    发明专利
    CONTINUOUS PRODUCTION OF 2,5-DIOXO-1-OXA-2-PHOSPHOLANES 未知

    公开(公告)号：CA1055959A

    公开(公告)日：1979-06-05

    申请号：CA256710

    申请日：1976-07-09

    Applicant: HOECHST AG

    Inventor： OHORODNIK ALEXANDER ,  LOHMAR ELMAR ,  GEHRMANN KLAUS ,  STUTZKE PAUL

    IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  C07F9/40

    Abstract: CONTINUOUS PRODUCTION OF 2,5-DIOXO-1-OXA-2-PHOSPHOLANES. Continuous production of 2,5-dioxo-1-oxa-2-phospholanes of the general formula from a beta-halogenoformyl-ethyl phosphinic acid halide of the general formula R1XP(O)-CHR2-CHR3-CO-X in which formulae R1 stands for an alkyl radical having 1, 2, 3 or 4 carbon atoms, or a phenyl radical, R2 and R3 each stands for hydrogen or CH3, and X stands for chlorine or bromine, by reacting the said acid halide with acetic anhydride. The phospholanes are produced by introducing, into a heatable circulation reactor, an initial quantity of the desired 2,5-dioxo-1-oxa-2-phospholane and circulating it therein at a temperature of 110 to 190.degree.C; separately preheating the respective betahalogenoformyl-ethyl phosphinic acid halide and acetic anhydride starting materials to a temperature of 60 to 160.degree.C; mixing these starting materials together and continuously adding the resulting mixture to the material circulated in the reactor, the mixture being introduced into the lower third of the reactor; distilling off resulting acetyl halide near the head of the circulation reactor, a pressure difference of 0.1 to 5 bar, being established between the point of introduction of the mixture of starting materials and the overflow level in the circulation reactor, and the material being kept circulating by the evaporating acetyl halide; and removing the resulting desired 2,5-dioxo-1-oxa-2-phospholane from the reactor at a location which is below that at which the acetyl halide is distilled off.

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