CN1303887A - 硅氧烷组合物的连续生产方法 - Google Patents

硅氧烷组合物的连续生产方法 Download PDF

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CN1303887A
CN1303887A CN00136485A CN00136485A CN1303887A CN 1303887 A CN1303887 A CN 1303887A CN 00136485 A CN00136485 A CN 00136485A CN 00136485 A CN00136485 A CN 00136485A CN 1303887 A CN1303887 A CN 1303887A
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section
composition
continuous annular
parts
mixing machine
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CN1162471C (zh
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R·德恩
J·波法德
N·辛格
A·L·塔特
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General Electric Co
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General Electric Co
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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)

Abstract

通过在连续环状料层混合机中形成预混物并连续将这种预混物排放至配料装置中进行配料以形成填充的可热硫化的硅氧烷组合物,可将高含量的处理过的煅制二氧化硅、加工流体和高分子量的硅氧烷聚合物连续配制成均匀的用二氧化硅填充的可热硫化的硅氧烷组合物。

Description

硅氧烷组合物的连续生产方法
本发明涉及一种可热硫化的硅氧烷组合物的连续生产方法。
可热硫化的硅氧烷组合物包含一种高粘度的硅氧烷聚合物、一种无机增强填料和各种有助于加工或使组合物具有所需的最终性能的各种添加剂。可向组合物中加入硫化剂并进行热硫化以制造硅氧烷橡胶模制件，如垫圈、医用管材和计算机键垫。
通常，可热硫化的硅氧烷组合物是采用间歇涅合机如高强度密闭式混炼机或低强度双臂胶浆混合机，将高粘度的聚二有机基硅氧烷、无机填料和添加剂涅合生产的。在该方法中，聚二有机基硅氧烷、无机填料和处理剂和添加剂进行间歇混合直至获得所需的性能。在US专利5,198,171(Kasahara等)中，聚二有机基硅氧烷、无机填料和处理剂的预浓缩物是通过高速机械剪切混合机形成的。形成的预混物再在同向双螺杆挤出机中进行配料。这种预混物在第一步中形成，其中，25℃时的粘度为1×106cP或更大的聚二有机基、硅氧烷、无机填料和处理剂在高速机械剪切机中混合以提供一种可流动的颗粒混合物，其中，每一种成分均以基本均匀的分散微细的状态存在。然后，将这种可流动的颗粒混合物以恒定的进料速度加至涅合和挤出机中，该装置具有两个以相同方向转动的螺杆。
间歇方法要求较长的混合时间和大量的能量。在工业化规模的分批生产中，不均匀的剪切和外延的应力会导致填料按大小分布不均匀，并导致在性能上的变化。在不同时间加工的胶料可产生不同的物理性能。间歇方法需要较多的人力、能耗和资本，所生产的物料的适合度仅能达到最低限度。
在US专利5,409,978(Hamada等)中，聚二有机基硅氧烷、无机填料和处理剂的预浓缩物在约200-300℃下在同向旋转连续双螺杆挤出机中形成。然后，将这种预浓缩物在反转的双螺杆挤出机中于150-300℃下进行配料和热处理。但是，这种需要两个挤出机的方法成本较高并需要较大的加工面积。
采用上述方法，生产量受到限制。因此，仍希望开发一种改善生产量并适合作为低成本方法的方法，所述低成本方法可由填料、添加剂和聚合物有效地利用单个挤出机连续和均匀地生产低粘度和高粘度全范围的硅氧烷弹性体。
本发明提供了一种对高含量填料、加工流体和硅氧烷聚合物进行配料以生产具有所需增强性能和挥发物含量的、均匀填充的可热硫化硅氧烷组合物的方法。本发明的方法包括连续将填料与硅氧烷聚合物加至高速混合段以形成自由流动的颗粒状浓缩物。这种浓缩物连续从混合段中排放至用于进一步加工的配料装置中。
另一方面，本发明涉及一种形成填料与硅氧烷聚合物的预混物的方法。在该方法中，填料与硅氧烷组合物在连续环状料层混合机中进行混合，从混合机中排出填充后的硅氧烷聚合物预混物。
另一方面，本发明涉及一种对填充后的可热硫化硅氧烷组合物进行配料的方法，其中，填料与硅氧烷聚合物在高速连续混合机中进行混合以形成一种预混物，部件末端速度(element tip speed)为约3m/s至约100m/s。然后，将这种预混物排放至下一个加工装置中。
另一方面，本发明涉及一种连续环状料层混合机，其具有一系列的部分，所述部分至少包含以下的三个部分，含有向前推进的(forward pitched)混合部件的第一部分，含有中立或向前推进的切割部件的第二部分和含有向后推进(rearward pitched)的混合部件的第三部分。
另一方面，本发明涉及一种配料装置，其包含第一段连续环状料层混合机(annular layer mixer)和包含与第一段相连的挤出机的至少一个后续段，以允许连续从第一段向第二段排出加工后的物料。
图1是连续可热硫化硅氧烷组合物配料方法和装置的示意图；
图2是连续可热硫化硅氧烷组合物配料方法和装置的示意图；
图3为连续环状料层混合机的侧面断面图；
图4和图5为混合部件的示意图；
图6为说明部件齿节的示意图；
图7为通过图3中A-A线的示意图；
图8为通过图3中B-B线的示意图；和
图9为测定部件齿节的参考范围。
班伯里混炼机或胶浆(dough)混合机公知可用于对填料与硅氧烷聚合物进行间歇配料。配料操作有两个不同的步骤；第一步涉及用聚合物将填料润湿，而第二步涉及将附聚物打碎并将填料均匀分散于聚合物中。将填料充分分散于聚合物中是非常重要的。任何较大的未分散的附聚物均将导致机械性能变差，这是因为其会造成引发裂缝的故障。
在间歇或连续过程中，处理剂可与硅氧烷聚合物一起在加入填料时进行分散或在加入填料之前进行分散。在这些过程中，在硅氧烷聚合物与存在的游离的未反应的硅烷醇基团间会产生很大的界面力。处理剂必须扩散通过大部分高分子量硅氧烷聚合物并穿透刚性的硅氧烷聚合物/填料界面以使填料得到处理。必须增加混合强度以克服较大的界面力并允许处理剂穿透接近硅烷醇基团。混合强度增加会引起物料温度不希望发生的增加。
按照本发明，硅氧烷和填料的自由流动的颗粒浓缩物在高速混合段中连续形成。该浓缩物连续从混合段中排放至用于进一步加工的配料装置中。混合段可包含连续环状料层混合机。连续环状料层混合机包含一个圆筒形混合槽，其中，被混合的物料沿着螺旋形通道沿着槽的轴被推进，为与圆筒形混合机壁相邻接的环的形式。典型的连续环状料层混合机公开于US专利5,018,673(Erich等)中，该文献描述了一种混合机，其包含基本上水平设置的圆筒形外壳，其一端设有用于连续供应物料的供料管，另一端设有连续排出物料的排料管。圆筒形外壳包封了一个混合装置，其与外壳同轴安装。混合装置在可高速下进行驱动。该装置包含混合部件，其基本上由装置径向凸出到外壳内壁的附近。混合机包括一个引入区，其与供料管连接，和润湿区，其设置在引入区的轴向输送方向的下游。混合机也包括设置在润湿区中用于使液体进入形成物料环形式的部件。环被螺旋输送并在外壳的内壁上移动通过混合机。混合机还包含分离簇集物的部件。该部件包括多个切割部件，其设置在相对于混合装置的轴的径向平面上，并在外壳的整个周缘附近相互间以相等的环状间距来排列。
在本发明的实施方案中，采用连续环状料层混合机作为预混段以在大量填料中产生未固化的硅氧烷聚合物的微细分散体。然后，使这种物料在挤出机中于压缩、拉伸和剪切流动场中进行相转换，成为配料状态，而干的填料呈少数相。填料的第一段增密导致在挤出机中更短的混合时间，从而显著改善生产能力。
可用于本发明的无机填料可以是任何用于与硅氧烷聚合物共混物中的无机填料。无机填料的实例包括增强二氧化硅如煅制二氧化硅或沉淀二氧化硅或用有机硅化合物进行过表面处理的二氧化硅，所述有机硅化合物例如为有机聚硅氧烷、有机烷氧基硅烷、有机氯硅烷或六有机二硅氮烷。填料可以是硅藻土、微细的石英、氧化铝、二氧化钛、氧化铁、氧化铈、氢氧化铈、氧化镁、氧化锌、碳酸钙、硅酸锆、碳黑或群青。可采用单独一种填料或填料组合用来增强硅氧烷聚合物。
以100重量份硅氧烷聚合物计，填料的用量为约5至约200重量份，优选约10至约100重量份，更优选约20至约60重量份。
在填料表面上残余的硅烷醇基团可控制在二氧化硅与硅氧烷聚合物链中羟基或氧基团间的氢键强度。在填料中的高浓度残余硅烷醇会造成最后制品在贮藏期间的“结构化(structuring)”或“皱片硬化(crepe hardening)”。这种作用导致难于在贮藏一段时间后对材料进行加工。如果在填料中的硅烷醇官能基团的浓度太高，则可加入处理剂以减少基团至所需的浓度。硅烷醇反应物处理剂可发生反应而减少可利用的基团的浓度至约8至约2羟基基团/填料的(纳米)2，优选约7至约3羟基基团/填料的(纳米)2。表面处理过的二氧化硅是本发明优选的填料，以每100重量份硅氧烷聚合物计，其用量为约10至约100重量份，优选约20至约60重量份。
处理剂可混入填料中以减少填料硅烷醇基团，从而改善填料的分配能力和/或减少硅氧烷橡胶老化所需的时间，并防止蠕变硬化和/或调节可塑性。处理剂可为一种有机硅烷、低粘度聚硅氧烷或硅氧烷树脂，其具有1-6个碳原子的烷氧基和/或硅烷醇基团。具体实例包括：二苯基-硅烷二醇、二甲基硅烷二醇、甲基三乙氧基硅烷和苯基三甲氧基硅烷。低粘度聚硅氧烷可包含一种或多种选自甲基、苯基、乙烯基和3,3,3-三氟丙基的有机基团。在25℃下聚硅氧烷的粘度为约1至约300cp，优选约5至约100cp。以每100重量份填料计，处理剂的加入量为0.1至100重量份，优选0.5至约50重量份，更优选约1.0至约20重量份。优选的硅烷醇-反应物处理剂包括硅烷醇-终端的聚二甲基硅氧烷、八甲基环四硅氧烷(D4)和六甲基二硅氮烷(HMDZ)。
用于本发明组合物中的硅氧烷聚合物可由式Ⅰ的重复单元表示：
其中，R1每次出现独立地表示C1-C4烷基或C2-C4亚烷基，R2每次出现独立地表示C1-C4烷基、C1-C4卤代烷基或C2-C4亚烷基；R3每次出现独立地表示H、C1-C10烷基、C2-C4亚烷基、C4-C6环烷基、OH或C1-C4卤代烷基；n表示整数1,000至20,000。
另一个优选的组合物包含硅氧烷聚合物，其中，R1每次出现独立地表示CH3或CH=CH2；R2每次出现独立地表示CH3、CH=CH2或CH2CH2CF3；R3每次出现独立地表示CH3、CH=CH2、OH或CH2CH2CF3；n表示整数约4,000至约10,000。
另一个实施方案提供了一种组合物，其中，以硅氧烷聚合物为基准计，硅氧烷聚合物的乙烯基含量为约0.05wt％至约0.5wt％。
可热硫化的硅氧烷组合物也可包含其它添加剂，如耐热改善剂如金属的氧化物、氢氧化物和脂肪酸盐、硫化返原抑制剂、阻燃剂如铂化合物、防脱色剂、增塑剂如硅油、内脱模剂如金属皂、颜料和染料。
通过以下附图和详述，本发明的特征将更为明显，这些非限定实例说明本发明的实施方案。
图1图示说明了本发明的方法。
在图1中，本发明的装置10包含高速混合段12和挤出机段14。高速混合段12可表示连续环状料层混合机，并可表示单一混合机或设置为顺序操作的多个混合机。挤出机段14可为一个或多个同向旋转啮合双螺杆挤出机、反转双螺杆挤出机或单螺杆挤出机。优选挤出机段14为同向旋转啮合双螺杆挤出机或单螺杆往复式挤出机。当挤出机段包括多个挤出机时，它们可顺序连接或串联。
在本发明的方法中，填料装于减量(loss-in-weight)进料机16中，并与硅氧烷聚合物20和处理剂22一起加至混合段12中。
在混合段12中，向聚合物、填料和处理剂施以高速、高强度力，以产生自由流动的粉末预混物24。
需要适宜的末端速度(tip speed)和停留时间以将物料打碎，并用聚合物覆盖填料并用处理剂润湿物料。物料在约3m/s至约100m/s的部件末端速度下混合以形成预混物。优选部件的末端速度为约10m/s至约80m/s，更优选约15m/s至约60m/s。物料需要一段停留时间以通过混合机。当采用单个的混合机时，停留时间可为约3秒至约5分钟。对于单个的混合机来说，停留时间可为约5秒至约1分钟，优选约20秒至约45秒。混合段12可包含多个混合机。当顺序采用两个混合机时，对两个混合机来说，停留时间可为约5秒至约10分钟，或停留时间可为约10秒至约5分钟，或优选20秒至约3分钟。混合段12可产生一种堆积密度为约0.3至约0.6，或约0.35至约0.55，甚至0.36至约0.48的产物。
有利地，该预混物24可用于连续过程(如本发明所述)或可贮藏并分布开以在以后使用。在图1中，将预混物24加至挤出机段14中，在此，其与添加剂26配料并脱除挥发性成分，产生可热硫化的硅氧烷聚合物组合物30。
图2说明了本发明的另一个实施方案。图2的装置50包括连续环状料层高速混合机52和顺序设置的第二混合机54。可采用两个或多个混合机来增加停留时间以提供更均匀的预混物。图2的装置包括挤出机56，其顺序连接至混合机52、54的下游和随后的挤出机58。
在图2所述的过程中，减量进料机60将填料62计量加入第一混合机52中，以与聚合物62和处理剂66混合。将来自混合机52的产物68加至混合机54中，在此，产生自由流动的粉末预混物70，再将其加至挤出机56中，在此，再加入附加的处理剂72以进行进一步的处理。附加的聚合物可在此步骤中加入(未示出)以制成低硬度(durometer)材料。在此步骤中加入加工助剂和其它添加剂74以产生一种产物76，将其排放至挤出机58中进行脱挥发性成分处理78。挤出机58产生一种可热硫化的硅氧烷聚合物组合物80备用。
图3至8显示了一个连续环状料层混合机以及相关的部件。
图4和5为可以被安装在能在本发明中使用的混合机中的加工部件的示意图。图3为连续环状料层混合机102的侧面断面图，显示出图4和5的部件的布置。
在图3中，混合机102包括具有纵向中心轴106的圆筒形外壳104。该外壳104在横向端部处由端壁108、110密封着。轴106从外壳104的两个端部穿过伸出并且由端壁108、110密封。进料口112设在外壳104的顶部以基本成切线地通向外壳104的内部，并且排料口114设在外壳104的下端，基本成切线地与外壳104内部相通并且从外壳104的内部通向外面。
在混合机102的轴106上设有各种样式的加工部件。图4显示出在图3中的连续环状料层混合机102内部从转动轴106延伸并从轴106径向伸出的混合部件116。如沿着轴106的纵向轴线看以及如图7和8所示，这些混合部件116在轴向上成90°间隔排列。混合部件116包括从底座120伸出而终止在末端扇形端头122的杆118。图示的混合部件116垂直于底座120伸出一个倾斜的叶片型头122。该部件116以一个端头倾斜角安装在底座120中以提供相对增强的输送(推进的)功能或逆向混合功能，视情况而定。下文叙述部件的各种齿节和其功能，参照图6～9。
图5显示出在混合机102内部从底座126中伸出并且从轴106上径向定位的切割部件124。该切割部件124包括杆128，该杆端部130向外张开并且在132向里倾斜以在其远端136处形成切割边134。所示该部件124是垂直延伸的。该部件124可以以一个切割边的倾斜角进行安装以便控制输送和返混功能，如参照图6和图9所述的一样。如图8所示，沿轴106纵轴线看，该部件124以90°间隔轴向排列。
图6为这些部件的示意图，显示出相对于混合机轴106的部件齿节。图6显示出混合机106的第一引入部分138(第一部分)，其中设有沿着轴向输送方向142安装有端头的混合部件140。填料/处理剂/硅氧烷聚合物材料通过如图3所示的在第一部分138处的进料口112被送进混合机106，并且通过混合部件140沿着轴向输送方向142进行加速和启动。图6所示为沿混合机轴106的纵向轴线152所限定的轴线看过去的部件端头122和136的齿节，此处齿节角度由图9所限定。在90°和小于180°之间倾斜的部件具有输送功能，而在0°和小于90°之间倾斜的部件具有保持功能。混合部件140延伸靠近外壳104的内壁以避免死区，如图7所示，这些混合部件140围绕着轴106的圆周彼此相隔约90°。
这些混合部件140的输送方向设定成与由图9的坐标轴146所定义的垂线成约138°，其中横坐标148与混合机轴的纵向轴线150一致，并且纵坐标152垂直于轴线150。输送部件140的转动会产生了一个离心力，该离心力在部件140的径向外端将材料抛成环状。然后部件140的齿节使得控制成环状的材料成螺旋形向前穿过混合机102内部。
混合机102的第二部分154包括切割部件156，该部件与垂线成一个约118°的输送方向角。这些切割部件156如图9所示与输送部件140一起围绕着轴106在圆周上彼此间隔约90°，并且靠着外壳104的内壁延伸以避免死区。部件156用来分离物料团以加速填料变湿。
第三部分158包括向后推进的输送部件160以提供返混并增加停留时间。
在本发明的一个实施例中，连续的环状料层混合机102顺序包括至少一个含混合部件的第一部分、一个含切割部件的第二部分以及含混合部件的第三部分。除了特定的混合或切割部件之外，这些部分可以包括其它部件。例如，第二部分可包括切割和混合部件。第一部分可以包括向前推进的部件，第二部分可以包括向前和中立部件，并且第三部分可以包括用于增加停留时间的向后推进部件。连续环状料层混合机102的全部部件可以包括约5到约80％的第一部分部件，约10到约85％的第二部分部件和约0到约75％的第三部分部件；优选约10到约65％的第一部分部件，约10到约65％的第二部分部件和约10到约75％的第三部分部件；或者优选约15到约55％的第一部分部件，约10到约45％的第二部分部件和约20到约65％的第三部分部件。
图6所示为本发明的一个实施方案，其中连续环状料层混合机102顺序包括一个含向前推进的混合部件140的第一部分138、一个合向前推进的切割部件156的第二部分154以及合向后推进的混合部件160的第三部分158。如图6所示，混合机102终止于一个含向前推进的切割部件164继之以一个用于喷射预混合料的中立部件168的第四部分162。第二部分154还可以包括一个向前推进的混合部件166。
按照本发明，在连续环状料层混合机中的预混合在大量填料中产生未固化的聚合物的微细分散体。然后，将这种物料在挤出机中于压缩、拉伸和剪切流动场中进行相转换，成为配料状态，而干的填料为少数相。填料在环状料层混合机中的增密导致更短的掺入时间，从而显著改善生产能力。
从以下的详细讨论中，本发明的这些和其它特性将更为明显，这种非限定性实例说明了本发明的优选实施方案。在实施例中，预混物的质量由堆积密度、BET表面积、溶液和干粉末粒径表征。预混物物料通过扫描电子显微镜、透射式电子显微镜和抗压试验检测。
实施例1
Drais KTT连续环状料层混合机设有如表1所述的部件构造。
                  表1
部件号/说明     角度*     说明
1               139    向前输送和混合部件
2               136    向前输送和混合部件
3               139    向前输送和混合部件
4               135    向前输送和混合部件
5               119    向前输送和切割部件
6               117    向前输送和切割部件
7               122    向前输送和混合部件
8                62    向后混合部件
9                68    向后混合部件
10               71    向后混合部件
11               70    向后混合部件
12               70    向后混合部件
13               69    向后混合部件
14               69    向后混合部件
15               67    向后混合部件
16                  67    向后混合部件
17                 124    向前输送和切割部件
18                 185    中立切割部件
由图9的坐标轴146限定的垂线所成的角度(°)。
通过Doering泵(p=240 psi)，以40磅/小时的速度将硅橡胶加入混合机中，通过减量Acrisson进料机以60磅/小时的速度加入预处理过的煅制二氧化硅。两种进料均在室温下进行。混合机在安培数15.5-16.5下于3000rpm下进行操作。排出温度从81°F增至89°F，壳体温度保持在约73°F。制备七个具有0.40-0.42的堆积密度的样品。
实施例2
用63份的煅制二氧化硅和100份的聚合物胶重复实例1的Drais混合步骤。将来自Drais混合步骤的的产物立即加至班伯里混炼机中，在此，其与2.5份的甲氧基终端的流体处理剂、2.5份的硅烷醇流体处理剂/加工助剂和0.8份的乙烯基甲氧基硅烷交联剂进行配料，然后再用1.2份的催化剂于350°F下硫化10分钟，并在450°F下进行后烘烤。表2提供了对75 Duorometer产物所获得的物理性质。
实施例3
作为比较，将填料和聚合物直接加至班伯里混炼机中，并与实施例2所述相同的物料进行配料，相同的方式进行硫化。表2提供了对75 Duorometer产物所获得的物理性质。
                    表2
性质/实施例        2      3
肖氏A硬度          72     76
伸长率             395    366
100％模量          322    355
拉伸强度           1277   1302
撕裂强度(tear)B    148    153
比重    1.226    1.203
实施例4
用63份的煅制二氧化硅和100份的聚合物胶重复实例1的Drais混合步骤。将来自Drais混合步骤的的产物立即加至班伯里混炼机中，在此，其与2.5份的甲氧基终端的流体处理剂、2.5份的硅烷醇流体处理剂/加工助剂和0.8份的乙烯基甲氧基硅烷交联剂进行配料。各物料的样品在班伯里混炼机中在各种rpm下进行配料。配料后的样品用1.5份的2,4-二氯苯甲酰基过氧化物于260°F下硫化12分钟。将形成的片状样品在200 ℃下后烘烤4小时。表3提供了对75Duorometer样品所获得的物理性质。
                       表3性质/实施例RPM数    1400     2000     2800     3200肖氏A硬度           76       77       75       75伸长率              324      347      308      323100％模量           410      407      385      366拉伸强度            1327     1398     1210     1220撕裂强度B           134      126      126      130比重                1.207    1.209    1.198    1.199
实施例5
用63份的煅制二氧化硅和100份的聚合物胶重复实例1的Drais混合步骤。将来自Drais混合步骤的的产物连续加至双螺杆、同向旋转互啮合挤出机中进行配料，然后连续加至单螺杆往复挤出机中进行均匀质和汽提。最终的产物包括1.35份的乙烯基二醇交联剂、2.0份的硅烷醇流体处理剂/加工助剂和3份的甲基乙烯基源作为交联剂/增塑剂。产物的挥发性物质含量低于1％。产物用1.5份的2,4-二氯苯甲酰基过氧化物于260°F下硫化17分钟。将形成的片状产物在200℃F下后烘烤4小时。表4提供了对75 Duorometer样品所获得的物理性质。实施例6
用61份的煅制二氧化硅和100份的聚合物胶重复实例1的Drais混合步骤。将来自Drais混合步骤的的产物连续加至双螺杆、同向旋转啮合挤出机中进行配料，然后连续加至反转、非互相啮合式双螺杆挤出机中进行均匀质和汽提。最终的产物包括1.0份的硅烷醇流体处理剂/加工助剂和0.5份的甲基乙烯基源作为交联剂/增塑剂。产物的挥发性物质含量低于1％。产物用1.5份的2,4-二氯苯甲酰基过氧化物于260°F下硫化17分钟。将形成的片状产物在200℃下后烘烤4小时。表4提供了对40 Duorometer样品所获得的物理性质。
            表2
性质/实施例  5       6
肖氏A硬度    70.1    37.8
伸长率       327     519
100％模量    420     108
拉伸强度     1467    1078
撕裂强度B    123     69
比重         1.21    1.106
结果表明，预混物可连续地在高速混合段中制备以形成自由流动的颗粒状浓缩物，其可连续排放至配料装置以制备可热硫化的硅氧烷组合物。
以上描述了本发明的优选实施方案，但本发明能够进行其它的改进和变化，因而，本发明不受实施例的具体描述的限制。本发明包含了在权利要求范围内所有的变化和改变。

Claims (26)

1、一种填充的可热硫化的硅氧烷组合物的配料方法，包括：
将填料与硅氧烷聚合物连续加至高速混合段以形成自由流动的颗粒状浓缩物；和
将所述的自由流动的颗粒状浓缩物连续从所述混合段中排放至配料装置中。
2、根据权利要求1的方法，包括连续在所述的配料装置中对所述的浓缩物进行配料以形成填充的可热硫化的硅氧烷组合物。
3、根据权利要求1的方法，其中，所述的混合段包含剪切和搅拌机械。
4、根据权利要求1的方法，其中，所述的混合段包含连续环状料层混合机。
5、根据权利要求1的方法，其中，所述的配料装置为螺旋驱动的挤出机机械。
6、根据权利要求1的方法，其中，所述的混合段包含两个顺序连接的连续环状混合机，其包含：
在所述的连续环状料层混合机中使所述填料与所述的硅氧烷聚合物混合，停留时间为约5秒至约10分钟，以形成一种预混物；和
将所述的预混物排放至所述的配料装置中。
7、根据权利要求1的方法，其中，所述的混合段包含至少两个顺序连接的连续环状混合机，其包含：
在所述的连续环状料层混合机中使所述填料与所述的硅氧烷聚合物混合，停留时间为约10秒至约5分钟，以形成一种预混物；和
将所述的预混物排放至所述的配料装置中。
8、根据权利要求1的方法，其中，所述的混合段包含两个顺序连接的连续环状混合机，其包含：
在所述的连续环状料层混合机中使所述填料与所述的硅氧烷聚合物混合，停留时间为约20秒至约3分钟，以形成一种预混物；和
将所述的预混物排放至所述的配料装置中
9、根据权利要求9的方法，其中，所述的连续环状料层混合机靠近并与所述的配料装置连接。
10、根据权利要求9的方法，包括：
使所述的填料与所述的硅氧烷聚合物在所述连续环状料层混合机中以部件末端速度为约3m/s至约100m/s进行混合形成一种预混物；和
将所述预混物排放至所述配料装置中。
11、根据权利要求9的方法，包括：
使所述的填料与所述的硅氧烷聚合物在所述连续环状料层混合机中混合，停留时间为约3秒至约5分钟，形成一种预混物；和
将所述预混物排放至所述配料装置中。
12、根据权利要求9的方法，其中，所述的连续环状料层混合机具有以下顺序的至少三部分：包含向前推进的混合部件的第一部分、包含向前推进的切割部件或中立切割部件的第二部分和包含向后推进的混合部件的第三部分。
13、根据权利要求19的方法，其中，所述的连续环状料层混合机包含约5至约80％的第一部分部件，约10至约85％的第二部分部件和约0至约75％的第三部分部件。
14、根据权利要求19的方法，其中，所述的连续环状料层混合机包含约10至约65％的第一部分部件，约10至约65％的第二部分部件和约10至约75％的第三部分部件。
15、根据权利要求19的方法，其中，所述的连续环状料层混合机包含约15至约55％的第一部分部件，约10至约45％的第二部分部件和约20至约65％的第三部分部件。
16、根据权利要求19的方法，其中，所述的连续环状料层混合机还包含最后一部分，其含有向前推进的切割或向前推进的混合部件。
17、一种填充的可热硫化的硅氧烷组合物的配料方法，包括：
将填料与硅氧烷聚合物在连续环状料层混合机中以部件末端速度为约3m/s至约100m/s混合形成一种预混物；和
将所述预混物排放至下面的加工装置中。
18、根据权利要求24的方法，其中，所述的末端速度为约15m/s至约80m/s。
19、一种形成用于制备填充的可热硫化的硅氧烷组合物的预混物的方法，包括：
将填料与硅氧烷聚合物在连续环状料层混合机中混合；和
从所述混合机中排放填充的硅氧烷聚合物预混物。
20、一种连续环状料层混合机，其包含以下顺序的至少三部分：包含混合部件的第一部分、包含切割部件的第二部分和包含混合部件的第三部分。
21、一种配料装置，其包含：
第一段连续环状料层混合机；和
至少一个随后的一段，其包含一个与所述第一段连接的挤出机，以从所述第一段连续排放加工后的物料至所述第二段。
22、根据权利要求37的配料装置，其中，第二段包含同向旋转非互相啮合式的双螺杆挤出机。
23、根据权利要求37的配料装置，其中，所述的段是分离并相邻的两段。
24、根据权利要求37的配料装置，其中，所述的第一段包含多个顺序设置操作的混合机。
25、根据权利要求37的配料装置，其中，所述的第一段包含多个混合机，其中，至少两个混合机设置为串联操作。
26、根据权利要求37的配料装置，其中，所述的至少一个随后的段包含同向旋转啮合双螺杆挤出机、反转双螺杆挤出机、单螺杆挤出机或单螺杆往复式挤出机。
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US6913380B2 (en) 2005-07-05
CN1162471C (zh) 2004-08-18
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EP1110690A3 (en) 2002-03-20
US20040257905A1 (en) 2004-12-23
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