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    Process for producing benzophenone-azine
    1.
    发明授权
    Process for producing benzophenone-azine 失效
    二苯甲酮吖嗪的制备方法

    公开(公告)号：US4751326A

    公开(公告)日：1988-06-14

    申请号：US684419

    申请日：1984-12-20

    申请人： Takanari Nawata ,  Shuzabu Sakaguchi ,  Toshiaki Kohzaki ,  Osamu Aoki ,  Norio Takeda ,  Masafumi Shimpo

    发明人： Takanari Nawata ,  Shuzabu Sakaguchi ,  Toshiaki Kohzaki ,  Osamu Aoki ,  Norio Takeda ,  Masafumi Shimpo

    IPC分类号： C07B61/00 ,  B01J27/00 ,  B01J27/32 ,  C07C67/00 ,  C07C241/00 ,  C07C251/88 ,  C07C109/04

    CPC分类号： C07C251/88 ,  B01J27/32 ,  Y02P20/584

    摘要： An improved process for producing benzophenone-azine in which a catalyst can be removed, recovered and recycled is disclosed. The process comprises the steps of:(a) oxidizing benzophenone-imine with molecular oxygen in the presence of cuprous chloride catalyst to produce an oxidation reaction mixture containing benzophenone-azine;(b) contacting the oxidation reaction mixture obtained in step (a) with an aqueous solution containing ammonium chloride and hydrochloric acid to decompose the remaining benzophenone-imine substantially without causing decomposition of the produced benzophenone-azine and simultaneously to extract the catalyst from the oxidation reaction mixture;(c) separating the oxidation reaction mixture containing benzophenone-azine after the extraction in step (b) to recover benzophenone-azine as a solution;(d) neutralizing the catalyst-containing aqueous solution separated after the extraction step (b) with ammonia and then contacting the neutralized catalyst-containing aqueous solution with benzophenone-imine to extract the catalyst into benzophenone-imine; and(e) separating the benzophenone-imine solution containing the catalyst obtained after extraction in step (d) from the aqueous layer and recycling said solution to step (a) to reuse as a catalyst for step (a), without isolating the catalyst from said benzophenone-imine solution.

    摘要翻译： 公开了可以除去，回收和回收催化剂的二苯甲酮 - 吖嗪的改进方法。 该方法包括以下步骤：（a）在氯化亚铜催化剂存在下用分子氧氧化二苯甲酮 - 亚胺以产生含有二苯甲酮 - 吖嗪的氧化反应混合物; （b）将步骤（a）中获得的氧化反应混合物与含有氯化铵和盐酸的水溶液接触，基本上分解剩余的二苯甲酮 - 亚胺，而不会引起生成的二苯甲酮 - 吖嗪的分解，同时从催化剂中提取催化剂 反应混合物; （c）在步骤（b）中提取后分离含有二苯甲酮 - 吖嗪的氧化反应混合物，以二苯甲酮 - 吖嗪为溶液回收; （d）用氨中和提取步骤（b）后分离的含催化剂的水溶液，然后使中和的含有催化剂的水溶液与二苯甲酮 - 亚胺接触，将催化剂萃取到二苯甲酮 - 亚胺中; 和（e）将步骤（d）中提取后得到的含有催化剂的二苯甲酮 - 亚胺溶液从水层中分离出来，并将所述溶液再循环到步骤（a）中以再利用作为步骤（a）的催化剂，而不将催化剂从 称二苯甲酮 - 亚胺溶液。

    Process for preparing benzophenone-azines
    2.
    发明授权
    Process for preparing benzophenone-azines 失效
    制备二苯甲酮吖嗪的方法

    公开(公告)号：US4727190A

    公开(公告)日：1988-02-23

    申请号：US918656

    申请日：1986-10-14

    申请人： Takanari Nawata ,  Shuzabu Sakaguchi ,  Toshiaki Kohzaki ,  Osamu Aoki ,  Norio Takeda ,  Yoshiyuki Aoki ,  Masafumi Shimpo

    发明人： Takanari Nawata ,  Shuzabu Sakaguchi ,  Toshiaki Kohzaki ,  Osamu Aoki ,  Norio Takeda ,  Yoshiyuki Aoki ,  Masafumi Shimpo

    IPC分类号： C09B17/00 ,  B01J27/122 ,  C01B21/16 ,  C07B61/00 ,  C07C249/16 ,  C07C251/88 ,  C07C109/16

    CPC分类号： C07C251/88 ,  C01B21/16

    摘要： A process for continuously preparing benzophenone-azines comprising oxidizing benzophenone-imines with molecular oxygen or a molecular oxygen-containing gas in the presence of a copper halide catalyst is disclosed. The oxidation reaction is carried out in a multistage system under an oxygen partial pressure gradually decreasing from the former stage to the latter stage and at a conversion gradually decreasing from the former stage to the latter stage, while controlling the conversion so that the molar ratio of the benzophenone-imines to the copper halide in the final stage be maintained at 1 or more. By the process, the continuous reaction can stably be performed at a high conversion of the benzophenone-imines without involving insolubilization and sedimentation of the catalyst.

    摘要翻译： 公开了一种连续制备二苯甲酮吖嗪的方法，包括在卤化铜催化剂存在下用分子氧或含分子氧气体氧化二苯甲酮 - 亚胺。 氧化反应在多级体系​​中，在从前一阶段到后一阶段逐渐降低的氧分压下进行，并且转化率从前一阶段逐渐降低到后一阶段，同时控制转化率，使得 在最后阶段将二苯甲酮 - 亚胺与卤化铜保持在1以上。 通过该方法，连续反应可以稳定地在二苯甲酮 - 亚胺的高转化率下进行，而不会引起催化剂的不溶解和沉淀。

    Process for preparing hydrazine hydrohalogenide
    4.
    发明授权
    Process for preparing hydrazine hydrohalogenide 失效
    制备氢卤化肼的方法

    公开(公告)号：US4628119A

    公开(公告)日：1986-12-09

    申请号：US702553

    申请日：1985-02-19

    申请人： Takanari Nawata ,  Shuzabu Sakaguchi ,  Osamu Aoki

    发明人： Takanari Nawata ,  Shuzabu Sakaguchi ,  Osamu Aoki

    IPC分类号： B01J23/00 ,  B01J27/122 ,  C01B21/16 ,  C07C109/04

    CPC分类号： C07C251/88 ,  C01B21/16 ,  Y02P20/584

    摘要： A process for preparing hydrazine hydrohalogenide is disclosed. The process comprises the steps of:(a) oxidizing benzophenone-imines with molecular oxygen in the presence of a copper halide catalyst to produce benzophenone-azines;(b) contacting the oxidation reaction mixture with an aqueous solution containing a hydrohalogenic acid thereby hydrolyzing the benzophenone-azines to produce a hydrazine hydrohalogenide and, simultaneously, extracting and removing the catalyst with the hydrohalogenic acid-containing aqueous solution to obtain an aqueous solution containing the hydrazine hydrohalogenide and the catalyst;(c) separating the aqueous solution and adjusting the solution to a pH of from 3 to 7 with an alkali;(d) contacting the aqueous solution with benzophenone-imines to extract the catalyst;(e) separating the catalyst-containing benzophenone-imines solution from the aqueous solution containing the hydrazine hydrohalogenide to recover the hydrazine hydrohalogenide and to recycle the catalyst-containing benzophenone-imines solution to step (a).The process is advantageous in that the catalyst is easily recovered for reuse.

    摘要翻译： 公开了一种制备氢卤酸肼的方法。 该方法包括以下步骤：（a）在卤化铜催化剂存在下用分子氧氧化二苯甲酮 - 亚胺，生成二苯甲酮 - 吖嗪; （b）使氧化反应混合物与含有氢卤酸的水溶液接触，从而水解二苯甲酮 - 吖嗪以产生氢卤酸肼，同时用含氢卤酸的水溶液萃取和除去催化剂，得到含有 肼氢卤化物和催化剂; （c）用碱分离水溶液并将溶液调节至3至7的pH; （d）使该水溶液与二苯甲酮 - 亚胺接触以提取催化剂; （e）从含有氢卤化肼的水溶液中分离含催化剂的二苯甲酮 - 亚胺溶液以回收氢卤酸肼，并将含有催化剂的二苯甲酮 - 亚胺溶液再循环到步骤（a）。 该方法的优点在于催化剂容易回收再利用。