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    Preparation and recovery of N-hydrocarbylthiophosphoric triamides or N-hydrocarbylphosphoric triamides
    9.
    发明授权
    Preparation and recovery of N-hydrocarbylthiophosphoric triamides or N-hydrocarbylphosphoric triamides 失效
    N-烃基硫代磷酸三酰胺或N-烃基磷酸三酰胺的制备和回收

    公开(公告)号：US5883297A

    公开(公告)日：1999-03-16

    申请号：US58367

    申请日：1998-04-09

    申请人： Gerald M. Sulzer ,  Chi Hung Cheng ,  W. Dirk Klobucar ,  Charles H. Kolich

    发明人： Gerald M. Sulzer ,  Chi Hung Cheng ,  W. Dirk Klobucar ,  Charles H. Kolich

    IPC分类号： C01C1/16 ,  C07F9/02 ,  C07F9/22 ,  C07F9/26

    CPC分类号： C01C1/164 ,  C07F9/025 ,  C07F9/224 ,  C07F9/26

    摘要： A reaction mixture containing N-hydrocarbylthiophosphoric triamide or N-hydrocarbylphosphoric triamide ("Triamide") is formed by reacting ammonia with N-hydrocarbylaminothiophosphoryl dichloride or N-hydrocarbylaminophosphoryl dichloride in a liquid organic medium, in proportions of at least 16 moles of ammonia per mole of such dichloride and that keep in solution the ammonium chloride co-product formed in the reaction. The temperature of the reaction mixture is kept high enough to keep ammonium chloride-ammonia complex from forming a solid phase in the reaction mixture, but low enough to avoid significant reduction in Triamide yield. The reaction mixture is then caused/allowed to separate into an inorganic phase comprising ammonia, ammonium chloride and co-product thiophosphoric triamide or phosphoric triamide, and an organic phase comprising Triamide, liquid organic medium, dissolved ammonia and, usually, phosphorus impurities. These phases are separated from each other. The ammonia is removed from the organic phase to leave a concentrated solution of Triamide in residual liquid organic medium usually also containing phosphorus impurities. The Triamide is separated or recovered from this residual mixture by continuously introducing a stream of the liquid mixture into a wiped film evaporator operating at a temperature of about 60.degree.-140.degree. C., and at a pressure that avoids solids formation on the heating surface of the wiped film evaporator, and continuously collecting the Triamide product. Triamides are urease inhibitors for use with urea-based fertilizers.

    摘要翻译： 通过使氨与N-烃基氨基硫代磷酰基二氯化物或N-烃基氨基磷酰基二氯化物在液体有机介质中反应，按每摩尔至少16摩尔氨的比例形成含有N-烃基硫代磷酰三胺或N-烃基磷酸三酰胺（“三酰胺”）的反应混合物 的这种二氯化物，并保持溶液中形成的氯化铵副产物在反应中。 反应混合物的温度保持足够高以保持氯化铵 - 氨络合物在反应混合物中形成固相，但足够低以避免三酰胺产率的显着降低。 然后使反应混合物分离成包含氨，氯化铵和副产物硫代磷酸三酰胺或磷酸三酰胺的无机相，以及包含三酰胺，液体有机介质，溶解氨和通常为磷杂质的有机相。 这些阶段相互分离。 从有机相中除去氨，留下通常也含有磷杂质的残留液体有机介质中的三酰胺浓缩溶液。 通过将液体混合物流连续地引入到在约60-140℃的温度下操作的擦拭膜蒸发器中并且在避免在加热表面上形成固体的压力下将三酰胺分离或回收 的擦拭膜蒸发器，并连续收集三酰胺产物。 三酰胺是用于尿素肥料的尿素酶抑制剂。

    Preparation of N-hydrocarbylthiophosphoric triamides
    10.
    发明授权
    Preparation of N-hydrocarbylthiophosphoric triamides 失效
    N-烃基硫代磷酸三酰胺的制备

    公开(公告)号：US5770771A

    公开(公告)日：1998-06-23

    申请号：US786396

    申请日：1997-01-21

    申请人： Gerald M. Sulzer ,  Chi Hung Cheng ,  W. Dirk Klobucar ,  Charles H. Kolich

    发明人： Gerald M. Sulzer ,  Chi Hung Cheng ,  W. Dirk Klobucar ,  Charles H. Kolich

    IPC分类号： C01C1/16 ,  C07F9/02 ,  C07F9/22 ,  C07F9/26

    CPC分类号： C01C1/164 ,  C07F9/025 ,  C07F9/224 ,  C07F9/26

    摘要： Continuously fed to and mixed in a first reactor are (i) a preformed mixture of primary hydrocarbyl monoamine, tertiary amine and liquid inert organic solvent, and (ii) thiophosphoryl chloride while removing heat of reaction to maintain the reaction temperature in the range of about -20.degree. C. to about +50.degree. C. A reaction mixture containing N-hydrocarbylaminothiophosphoryl dichloride is formed. Ammonia and an effluent stream from the first reactor are continuously fed to and mixed in a second reactor in proportions of at least about 16 moles, of ammonia per mole of N-hydrocarbylaminothiophosphoryl dichloride that produce a reaction mixture containing N-hydrocarbylthiophosphoric triamide, and that keep in solution ammonium chloride co-product formed in the reaction. Heat of reaction is removed so that the temperature is high enough to keep ammonium chloride-ammonia complex from forming a solid phase in this reaction mixture, but low enough to avoid significant reduction in yield of N-hydrocarbylthiophosphoric triamide being formed. Effluent is withdrawn from the second reactor so as to maintain a substantially constant volume of reaction mixture in the second reactor. The process eliminates a difficult filtration of the co-product ammonium chloride formed in the second reaction. Also, it possible to accomplish this in a continuous process, with improved efficiency in large scale production of the N-hydrocarbylthiophosphoric triamides. Moreover, the ammonium chloride can be readily converted in the process to an industrially useful liquid co-product mixture.

    摘要翻译： 连续进料并混合在第一反应器中的是（i）主要烃基单胺，叔胺和液体惰性有机溶剂的预制混合物，和（ii）硫代磷酰氯，同时除去反应热，将反应温度保持在约 -20℃至约+ 50℃。形成含有N-烃基氨基硫代磷酰基二氯化物的反应混合物。 将氨和来自第一反应器的流出物流连续地进料至第二反应器中，其比例为至少约16摩尔，每摩尔N-烃基氨基硫代磷酰二氯的氨，其产生含有N-烃基硫代磷酰三酰胺的反应混合物，并且 保持反应中形成的溶液中氯化铵共同产物。 去除反应热，使得温度足够高以使氯化铵 - 氨络合物在该反应混合物中形成固相，但足够低以避免形成的N-烃基硫代磷酰三酰胺的产率显着降低。 将废水从第二反应器中排出，以便在第二反应器中维持反应混合物体积基本恒定。 该方法消除了在第二反应中形成的副产物氯化铵的难以过滤。 此外，可以在连续的方法中实现这一点，提高N-烃基硫代磷酸三酰胺的大规模生产的效率。 此外，氯化铵可以在工艺中容易地转化成工业上有用的液体共产物混合物。