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    Isolation of polycarbonate with carbon dioxide
    1.
    发明授权
    Isolation of polycarbonate with carbon dioxide 失效
    用二氧化碳分离聚碳酸酯

    公开(公告)号：US5250658A

    公开(公告)日：1993-10-05

    申请号：US940566

    申请日：1992-09-04

    申请人： Hanns-Ingolf Paul ,  Rolf Treckmann ,  Gunther Weymans ,  Jurgen Kirsch ,  Wolfgang Herrig

    发明人： Hanns-Ingolf Paul ,  Rolf Treckmann ,  Gunther Weymans ,  Jurgen Kirsch ,  Wolfgang Herrig

    IPC分类号： C08G64/40 ,  C08J3/14

    CPC分类号： C08J3/14 ,  C08G64/403 ,  C08J2369/00

    摘要： According to the invention, a special process for isolating polycarbonate from methylene chloride at temperatures of 30.degree. to 80.degree. C. in the form of a powder with residual solvent contents below 5% by weight is started up as a continuous process by starting up in a two-component nozzle, in which CO.sub.2 -containing fluid and the polymer solution are continuously combined, with a large excess of CO.sub.2 and then allowing the polycarbonate/methylene chloride/CO.sub.2 fluid system to pass through the gel-forming range of the polycarbonate/methylene chloride/CO.sub.2 phase diagram with continuous reduction of the CO.sub.2 throughput to a ratio of CO.sub.2 to organic solution of 4:1 to 2:1. The process started up in this way has a particularly long useful life.

    摘要翻译： 根据本发明，通过以30重量％〜80℃的温度从二氯甲烷中分离残留溶剂含量低于5重量％的粉末形式的特殊方法作为连续方法开始，通过在 将含有CO 2的流体和聚合物溶液连续组合的双组分喷嘴与大量过量的CO 2混合，然后使聚碳酸酯/二氯甲烷/ CO 2流体系统通过聚碳酸酯/ 二氧化氯/ CO2相图，将CO 2通量的持续降低至4：1至2：1的CO 2与有机溶液的比例。 以这种方式启动的过程具有特别长的使用寿命。

    Process for isolating polycarbonates with CO.sub.2 under pressure
    2.
    发明授权
    Process for isolating polycarbonates with CO.sub.2 under pressure 失效
    在压力下用二氧化碳分离聚碳酸酯的方法

    公开(公告)号：US5221731A

    公开(公告)日：1993-06-22

    申请号：US888942

    申请日：1992-05-26

    申请人： Gunther Weymans ,  Jurgen Kirsch ,  Wolfgang Herrig ,  Hanns-Ingolf Paul ,  Rolf Treckmann

    发明人： Gunther Weymans ,  Jurgen Kirsch ,  Wolfgang Herrig ,  Hanns-Ingolf Paul ,  Rolf Treckmann

    IPC分类号： C08G64/40 ,  C08J3/14

    CPC分类号： C08G64/403

    摘要： A continuous process for the isolation of polycarbonates from a solution of polycarbonate in methylene chloride at temperatures of 30.degree. to 80.degree. C. is disclosed. The process which yields polycarbonate in powder form having residual solvent content of less than 5% by weight, is characterized in that it entails the following steps:a) obtaining a solution of polycarbonate in methylene chloride containing 10 to 40 percent polycarbonate, said percent being relative to the total weight of the polycarbonate solution,b) mixing into said solution under pressures of 10 to 50 bar and at temperatures of 30.degree. to 50.degree. C. a fluid containing carbon dioxide resulting in a non-gelling polycarbonate/methylene/chloride/dioxide pressurized system, in which between 10 and 12% CO.sub.2 are dissolved,c) mixing said pressurized system in a two-component nozzle with additional fluid containing carbon dioxide under a pressure of 50 to 300 bar and at temperatures of 40.degree. to 150.degree. C., to cause rapid precipitation of polycarbonate in the form of solid particles, the quantitative ratio of CO.sub.2 to solution being between 1.0 and 15, preferably between 2.5 and 8.0,f) separating methylene chloride and carbon dioxide gases in a compressor/condenser system.The process is further characterized in that a time interval of at least 0.1 second separates step b) and step c), and in that the input of the fluid containing carbon dioxide is controlled to prevent gelatin in step b) and in that the pressurized system is above the gelation range in step c).

    摘要翻译： 公开了一种在聚碳酸酯从二氯甲烷溶液中分离聚碳酸酯的连续方法，其温度为30℃至80℃。 产生具有小于5重量％的残留溶剂含量的粉末形式的聚碳酸酯的方法的特征在于其需要以下步骤：a）获得聚碳酸酯在含有10-40％聚碳酸酯的二氯甲烷中的溶液，所述百分比为 相对于聚碳酸酯溶液的总重量，b）在10至50巴的压力和30至50℃的温度下将所述溶液混合到含有二氧化碳的流体中，得到非胶凝聚碳酸酯/亚甲基/氯化物 二氧化碳加压系统，其中溶解有10至12％的二氧化碳，c）将所述加压系统混合在双组分喷嘴中，在50至300巴的压力和40至150℃的温度下将含有二氧化碳的另外的流体混合 为了引起固体颗粒形式的聚碳酸酯的快速沉淀，CO 2与溶液的定量比在1.0和15之间，优选在2.5和8.0之间，f）sepa 在压缩机/冷凝器系统中评估二氯甲烷和二氧化碳气体。 该方法的特征还在于，至少0.1秒的时间间隔分离步骤b）和步骤c），并且控制含二氧化碳的流体的输入以防止步骤b）中的明胶，并且加压系统 在步骤c）中的凝胶化范围之上。

    Process for the production of polycarbonate
    4.
    发明授权
    Process for the production of polycarbonate 失效
    聚碳酸酯生产工艺

    公开(公告)号：US5258484A

    公开(公告)日：1993-11-02

    申请号：US902356

    申请日：1992-06-19

    申请人： Reinhard Schomacker ,  Uwe Hucks ,  Gunther Weymans ,  Wolfgang Herrig ,  Jurgen Kirsch

    发明人： Reinhard Schomacker ,  Uwe Hucks ,  Gunther Weymans ,  Wolfgang Herrig ,  Jurgen Kirsch

    IPC分类号： C08G64/22 ,  C08G64/24

    CPC分类号： C08G64/24

    摘要： A process for the continuous production of a thermoplastic aromatic polycarbonate is disclosed. Accordingly, in a reactor system which includes a tube reactor and a tank equipped with a stirrer, there are reacted a preheated dialkali diphenolate aqueous solution with gaseous phosgene in CH.sub.2 Cl.sub.2 and/or in chlorobenzene solution containing excess phosgene, in a mixer to form a mixed emulsion. The emulsion is then transported at least partly against the force of gravity into the tube reactor to facilitate a polycondensation reaction and in which after a residence time of at least 10 seconds and without dissipation of the heat of reaction there is added a chain terminator. The heat of reaction is dissipated in said tank and aqueous sodium hydroxide and catalyst are added to complete the reaction. The process according to the invention leads to high yields of phosgene.

    摘要翻译： 公开了连续生产热塑性芳族聚碳酸酯的方法。 因此，在包括管式反应器和装有搅拌器的罐的反应器系统中，在混合器中使预热的二元醇二酚盐水溶液与气态光气在CH 2 Cl 2中和/或含有过量光气的氯苯溶液中反应，形成混合 乳液。 然后将乳液至少部分地抵抗重力输送到管式反应器中以促进缩聚反应，并且其中在至少10秒的停留时间之后并且不消耗反应热量时，添加了链终止剂。 在所述槽中消散反应热，加入氢氧化钠水溶液和催化剂以完成反应。 根据本发明的方法导致高产率的光气。

    Process for the production of polycarbonate of constant viscosity
    5.
    发明授权
    Process for the production of polycarbonate of constant viscosity 失效
    用于生产恒定粘度的聚碳酸酯的方法

    公开(公告)号：US5412060A

    公开(公告)日：1995-05-02

    申请号：US189382

    申请日：1994-01-31

    申请人： Claus Wulff ,  Uwe Hucks ,  Rolf Bachmann ,  Gunther Weymans ,  Jurgen Kadelka ,  Wolfgang Herrig

    发明人： Claus Wulff ,  Uwe Hucks ,  Rolf Bachmann ,  Gunther Weymans ,  Jurgen Kadelka ,  Wolfgang Herrig

    IPC分类号： C08G64/24 ,  C08G64/00

    CPC分类号： C08G64/24

    摘要： The invention relates to a process for the production of polycarbonates by the two-phase interfacial method in which deviations between measured and estimated variables are continuously minimized by means of a suitably selected observer or filter system on the basis of a process model with an empirical Mark-Houwink relation adapted to the process. The variables estimated by the observer/filter are converted into control variables which are used to set input streams of the production process. Product quality is kept constant, changes in load or set values are quickly intercepted and even disturbances not readily accessible to measurement are taken into account by the process control.

    摘要翻译： 本发明涉及通过两相界面方法生产聚碳酸酯的方法，其中通过适当选择的观察者或过滤系统，在经验标记的过程模型的基础上，将测量值和估计变量之间的偏差连续最小化 -Houwink关系适应过程。 由观察者/过滤器估计的变量被转换为用于设置生产过程的输入流的控制变量。 产品质量保持不变，负载或设定值的变化被快速截断，并且通过过程控制考虑到测量中不容易获得的均匀干扰。

    Isolation of poly(ester)carbonates from methylene chloride using carbon dioxide fluid
    6.
    发明授权
    Isolation of poly(ester)carbonates from methylene chloride using carbon dioxide fluid 失效
    使用二氧化碳流体从甲基氯化物中分离聚（酯）碳酸酯

    公开(公告)号：US5248763A

    公开(公告)日：1993-09-28

    申请号：US932471

    申请日：1992-08-20

    申请人： Jurgen Kirsch ,  Gunther Weymans ,  Dieter Freitag

    发明人： Jurgen Kirsch ,  Gunther Weymans ,  Dieter Freitag

    IPC分类号： C08G63/64 ,  C08G63/88 ,  C08G63/90 ,  C08G64/40 ,  C08J3/14

    CPC分类号： C08G63/64 ,  C08G64/403

    摘要： A process for isolating a poly(ester)carbonate resin from its methylene chloride solution is disclosed. The process entails combining a solution which contains 5 to 30% by weight resin with carbon dioxide fluid in a two-component nozzle under pressures of 90 to 180 bar and at temperatures of 50.degree. to 75.degree. C., while maintaining in said the two-component nozzle a back-pressure of 85 to 150 bar, and introducing the resin into a separation vessel with retention of dust particles. Importantly, the relative quantities of carbon dioxide fluid and polymer solution used in the two-component nozzle are between 10 and 3 parts carbon dioxide fluid per one part of polymer solution, and the carbon dioxide fluid contains 10 to 1000 ppm methylene chloride. The process avoids blockage of said nozzle.

    摘要翻译： 公开了一种从其二氯甲烷溶液中分离聚（酯）碳酸酯树脂的方法。 该方法需要在90至180巴的压力和50至75℃的温度下将含有5至30重量％树脂的溶液与双组分喷嘴中的二氧化碳流体混合，同时保持在所述两个 - 组件喷嘴的背压为85至150巴，并将树脂引入分离容器中并保持灰尘颗粒。 重要的是，双组分喷嘴中使用的二氧化碳流体和聚合物溶液的相对数量为每一部分聚合物溶液为10-3份二氧化碳流体，二氧化碳流体含有10至1000ppm二氯甲烷。 该过程避免了所述喷嘴的堵塞。

    Process for the separation of multicomponent systems containing intermediate boiling substances in separating columns with side discharge
    9.
    发明授权
    Process for the separation of multicomponent systems containing intermediate boiling substances in separating columns with side discharge 失效
    在具有侧向排放的分隔柱中分离含有中间体沸腾物质的多组分体系的方法

    公开(公告)号：US5244544A

    公开(公告)日：1993-09-14

    申请号：US880815

    申请日：1992-05-08

    申请人： Lothar Lang ,  Franz F. Rhiel ,  Gunther Weymans

    发明人： Lothar Lang ,  Franz F. Rhiel ,  Gunther Weymans

    IPC分类号： B01D3/42

    CPC分类号： B01D3/4238 ,  Y10S203/19 ,  Y10S203/20

    摘要： A process for the separation of multicomponent systems containing intermediate boiling substances in separating separating columns with side discharge, the temperatures T.sub.u and T.sub.o above and below the side discharge are measured on the column or inside the column and the temperature difference T.sub.u -T.sub.o is used for controlling the side discharge. The control is carried out by constantly controlling one of the two temperatures T.sub.u or T.sub.o by the output of the evaporator or the discharge from the sump or the reflux or the removal of distillate or the reflux ratio.

    摘要翻译： 在分离具有侧面放电的分离柱的分离塔中分离含有中间沸点物质的多组分体系的方法，在柱上或柱内测量在侧面排出物上方和下方的温度Tu和To，并且将温度差Tu-To用于 控制侧面放电。 控制是通过恒定地控制蒸发器的输出或从贮槽的排放或回流或馏出物的去除或回流比来控制两个温度Tu或To中的一个温度。