CN1355738A - 用浆液原料制备组合物的方法和设备 - Google Patents

用浆液原料制备组合物的方法和设备 Download PDF

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CN1355738A
CN1355738A CN00808881A CN00808881A CN1355738A CN 1355738 A CN1355738 A CN 1355738A CN 00808881 A CN00808881 A CN 00808881A CN 00808881 A CN00808881 A CN 00808881A CN 1355738 A CN1355738 A CN 1355738A
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reactor
composition
equipment
matter
blender
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P·T·谢勒三世
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Dow Chemical Co
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Dow Chemical Co
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Abstract

一种用连续反应器(20)结合浆液容器(10)将浆液原料流(15)送入到该反应器中以制备组合物的方法和设备,该组合物包括一种或多种树脂材料和/或其它成分。更具体说,该方法和设备通过将一种或多种单体和/或低聚物的活性浆液送入到连续反应挤出机(20),以制造一种或多种树脂材料来制备组合物。该树脂材料可以任选地连续传送到用于连续地将树脂材料与其它成分混合的混合器中,从而形成掺混组合物。

Description

用浆液原料制备组合物的方法和设备
本发明涉及使用连续挤出机制备组合物的方法和设备。更具体说，本发明涉及通过将浆液从浆液容器送入一个连续反应器制备组合物的方法和设备。
迄今为止，比如象聚合物的化学组合物都是用连续反应挤出机制备的。比如，美国专利4,612,355公开了挤出机在制造塑料方面的应用。更具体地说，美国专利4,612,355公开了反应挤出机在制备环氧树脂方面的应用。
一般说来，加入到这种挤出机内的原料，在进入挤出机前是呈固态或熔融态的。这样就难于在把固体加入挤出机之前或当中将该固体充分而紧密地混合在一起。某些化学物质不能以固态加入，必须以不同的方式制备。
此外，连续过程对加料精确度的要求很高，特别是当连续方法是要求尽可能小反混的塞流过程和分步聚合时。分步聚合涉及到两种不同的双官能原料，分别表示为A-A和B-B，这里A与B反应，此反应对A-A和B-B的比例是非常敏感的，关系到最终的分子量和最终的物理性能。
一般说来，分步聚合方法优选使用液体原料，因为使用液体原料可以使加料的精确度达到0.1％以内。然而，在某些制造工艺中，一种或多种原料必须是固体的，因为在降解和安全方面的考虑，不希望使用液体原料。因此，当不能使用液体原料时就需要一种固体加料系统，比如失重(loss in weight)加料器。失重加料器在一分钟间隔内的精确度可以达到0.25％，但在5秒的间隔一般大于1％。在不能精确地处置固体的工艺中，最好避免使用固体加料系统。
因此希望提供一种方法和设备，用来将浆液原料加入到反应器，如挤出机中，以制备组合物。更优选的是，希望提供一种方法和设备，通过在一个连续搅拌和反混的容器中，将原料与液体原料一起保持几分钟，而使固体加料器的短期精确度平均化。
本发明涉及从一种或多种树脂材料和其它成分制备组合物的方法和设备，其使用连续反应器，结合使用浆液连续加料装置，将浆液原料的物流加入到反应器中。
在本发明的一个具体实施方案中，本发明的方法和设备通过将一种或多种单体和/或低聚物的浆液加入到一个连续反应器中，以制造一种或多种树脂材料，从而制备出组合物。该树脂材料可以在混合器中任选地与其它添加剂结合，或者以薄片的形式回收供进一步使用。
该方法将浆液的加料操作和反应性挤出操作结合在一起。当在液体材料中使用固体添加剂而又不必须熔融该固体时，本发明避免了与原料加料速度变化有关的问题。本发明的优点在于提供了固体加料器的精确加料流。
图1显示了本发明设备的一个实施方案的示意图，具体说明与连续反应挤出机同时使用的浆液加料容器。
本发明涉及到在一个连续方法中实现固体原料稳定加料的方法和设备，在该方法中使用了连续形成和混合的固体原料的浆液，或者固体原料和液体原料的混合浆液。一般说来，使用失重加料器将固体加入到浆液混合容器中，而使用一个液体的精确计量系统加入在浆液中使用的各种液体原料。
通过工艺中送料泵的速度来控制浆液过程的液面。应该用不会将气体带入系统中的装置来测量液面，比如膜片式液面转换计或超声波液面转换计。需要稳定的液面控制来给过程提供稳态的加料速度，并保证充分的混合。容器中的液面被控制在搅拌器上方以建立能够夹带固体的涡流。失重加料器的排料应该直接将固体原料送入到该涡流中。
本发明方法和设备的一个实施方案涉及到制备组合物和/或在组合物中所含的某些树脂材料，这里与反应挤出机同时使用了浆液容器。
在本文中“浆液”是指悬浮在液体物质中的一种或多种固体物质。
参见图1，这里显示了与反应器20相连的浆液容器10。热交换器(未显示)可以加热从存储容器(未显示)到管道(11)的液体单体物流，用调速添加泵(未显示)或者控制阀(未显示)控制加入到浆液容器10中的速度。控制液体单体物流11的温度，得到可以泵送的浆液物流。在某些情况下，液体单体物流11被加热到使浆液容器10中存在的固态单体熔融所需的温度。
从固体加料系统13到管道12中的固体单体物流被按比例加入到浆液容器10中，在浆液容器10中的高速混合器14把固体单体和液体单体混合在一起，形成在管道15中的活性浆液物流。使用计量加料泵(未显示)，将该浆液物流15连续计量地加入到反应器20中。如果须要完成反应，浆液15要和从催化剂添加泵(未显示)来的催化剂混合在一起。可以在浆液加料管1 5中将浆液与催化剂混合在一起，或者在位于浆液管15中的高速在线混合器中混合在一起，并送入到连续反应器20中。
将加入到连续反应器20中的单体和其它添加剂如催化剂加热到足够的温度，使得在反应器中发生反应，最后反应产物的物流通过管道21离开反应器20。
虽然没有显示，本发明的各个其它的实施方案可以包括，比如用树脂材料泵通过连接着配有连续混合器的连续反应器20的管道，强制输送连续反应器20的产品，如树脂材料。在该系统上也可以连接液体添加剂存储容器和计量流体控制泵，以在树脂材料被输送到混合器以前加入任何液体添加剂或其它成分。在本发明中用于将反应器和混合器结合的优选方法和设备公开在Keillor等人在同一日期提交的共同未决美国专利申请(发明名称为《用串联的连续反应器和混合器制备组合物的方法和设备》(Process and Apparatus For Preparing A CompositionUsing A Continuous Reactor And Mixer In Series)，代理号为44646)中。
此外，在加入到连续混合器以前，从连续反应器出来的树脂材料的条件必须变更。比如，可使用过滤系统，以从该树脂材料中除去任何颗粒状物质；或者使用热交换器系统以将树脂材料的温度降低到适当混合所要求的温度。可以从连续添加系统向混合器中添加其它的固体成分，并且和树脂材料的加料物流合并在一起。在连续混合器的固体排料口，可将产物转移到刨片机中，从而使组合物产物固化并成型为薄片。
在图1中所叙述的另一个实施方案中，可以将多个连续的浆液加料物流送入连续反应器，或者将一个浆液加料物流送入多个连续反应器中。
在本发明的一个实施方案中，可以通过本发明的方法，在一个连续反应器中制备可以用作本发明制备的组合物组分的树脂材料。用于该目的的连续反应器可以是一个管或管状反应器，或者挤出机。优选使用挤出机。可以使用一个以上的反应器制备不同的树脂材料。可以使用任何数量的反应器，并且这些反应器中的任何一个或者全部任选地直接连接到混合器上，在该混合器中也可以制备组合物。管或管状接头适于用作实现这种连接的装置。
通过在一个连续聚合反应器中使一种或多种单体和/或低聚物进行聚合，以形成树脂材料，更具体地说是形成聚合物，来制备在本发明中可以使用的树脂材料。一般说来，可以在聚合反应混合物中加入催化剂，用于得到特定类型的树脂材料，或者达到所需的转化率。当需要时，可以以溶液、浆液或者干燥物质混合物的形式中的一种或多种，把单体、低聚物和催化剂分别单独或两个或多个一组地送入聚合反应器。然而，这些组分中至少有一种或多种是以浆液的形式送入反应挤出机的。
按照本发明制备的组合物的树脂材料实际上可以是任何聚合物或共聚物。作为组合物中的组分，该树脂材料无须具有任何特定的分子量。该树脂材料可以具有的重复单元数，可以从两个重复单元到几百或几千个重复单元。可以在本发明方法中使用的特定的树脂材料包括比如环氧树脂、聚酯、聚氨酯、丙烯酸酯和在美国专利5,094,806中提出的其它聚合物。在上述所列的本发明中可以使用的树脂材料中，最优选的是环氧树脂和聚酯。在本发明中可以使用的环氧树脂和用来制备环氧树脂的材料公开在美国专利4,612,156中。在本发明中可以使用的聚酯和用于制备聚酯的材料公开在《聚合物科学和工程百科全书》(Encyclopedia of Polymer Science and Engineering)，第12卷，p.1-313中。
在生产可作为本发明组合物的组分的树脂材料中，各种条件或参数都对聚合反应的进程有影响。这些条件或参数的典型例子如下：向反应器中加入单体和/或低聚物的速度、反应进行的温度、反应经历的时间以及反应进行时反应物混合和搅拌的程度。单体和/或低聚物的加入速度可以受到比如在加压管上阀门调节的影响。反应进行的温度受到比如单体和/或低聚物，或者对反应器本身直接加热或冷却的影响。反应经历的时间长短受到比如反应器发尺寸如管、管道或挤出机的长度的影响，或者受到反应物进入或离开反应器的速度如由于挤出机螺杆的具体速度或设计的影响，或者进入管或管道内的加压惰性气体的影响。在反应时反应物混合或搅拌的程度可能受到比如桨叶或其它混合组件的尺寸、形状和速度的影响，在管或管道中存在的静态混合组件的影响，或者挤出机螺杆转速的影响。
如果用来作为本发明组合物的树脂材料的性能是已知的并保持在所需的水平，用本发明的方法和设备制备的组合物的质量能够得到改进。对于该目的可以分析的树脂材料性能的例子是粘度、熔体指数、熔体流动速度、分子量、分子量分布、当量、熔点、玻璃化转变温度、密度、比重和纯度。比如，当使用环氧树脂作为树脂材料时，希望其粘度为1-100,000厘泊。可以用来测定上述树脂材料性能的分析技术包括超声波能、拉曼光谱、红外光谱、近红外光谱和介电能。测量本发明使用的树脂材料性能的优选方法和设备公开在Shawn Maynard在相同日期提交的共同未决美国专利申请(发明名称为《用超声设施制备物质组合物的方法和设备》(Process And Apparatus For Preparing AComposition of Matter Utilizing An Ultrasonic Device)，代理号为446462)中。
一般说来，用本发明的浆液法制备的组合物是通过连续地将活性浆液溶液由浆液容器加入到反应挤出机而制备的。可以在浆液容器中、在反应器的加料管中或在反应器中加入任何量的其它成分，以形成组合物。比如，可以是一种或多种不是在反应器中制备的聚合物，活性或惰性的化合物，或者诸如颜料、填料或稳定剂的添加剂。当最终组合物是各种物质的掺混物时，可以把从反应器中出来的组合物任选地从反应挤出机经过反应器和混合器之间的连接装置传送到混合器中，以形成组合物。如果使用多于一个的反应器，在每个反应器和混合器之间都要建立连接装置。
使用的混合器的优选类型是挤出机，特别是双螺杆挤出机，但也可以使用其它类型的混合器，比如共捏合机。
在本发明的另一个实施方案中，可以通过将树脂材料与其它组分进行混料以制备最终组合物。最终组合物的其余组分包括多种其它的成分，其还可包括树脂材料，比如环氧树脂或聚酯，或者在上面列出的其它树脂材料。组合物的其余组分还可以包括诸如通用添加剂的成分，例如环氧树脂固化剂(比如二氰基二酰胺)、填料、颜料和稳定剂。在美国专利5,416,148中公开了作为本发明方法和设备制备的组合物成分的其它添加剂。这些添加剂可以以液体的形式加入到组合物中。在混合器中混合该组合物以后，以适用处理的形式回收该组合物，比如薄片或颗粒形式。
实施例1
通过液体环氧树脂和双酚A的反应制备固体环氧树脂。对于该应用，将熔融的双酚A加入到反应挤出机中被认为是不可接受的，因为在停车和开车时会产生颜色。因此，以如下面表1所示的希望的流速连续地将液体环氧树脂和双酚A加入到浆液容器中。然后用MoynoTM型的递进空腔泵(progressing cavity pump)将该浆液从浆液容器送到Krupp Wemer&Pfleiderer ZSK-40型反应挤出机中，用超声探头测量液面。随时间测量的在反应器中得到的产物的环氧当量列在表1中。EEW粘稠度是可以接受的，这表明该浆液加料系统是有效的。下面的表格给出了该实施例的结果。
表1
  试样   时间 环氧树脂(LER)加料速度(lb/hr) 双酚A加料速度(lb/hr) 环氧树脂当量(EEW)
    1#   1545     101.716   38.284   688.5
    2#   1600     101.716   38.284   675.1
    3#   1615     101.716   38.284   678.8
    4#   1630     101.716   38.284   685.2
    5#   1645     101.716   38.284   680.8
    6#   1700     101.716   38.284   691.2
    7#   1715     101.716   38.284   683.2
    8#   1730     101.716   38.284   690.3

Claims (29)

1.一种制备物质组合物的方法，该方法包括如下的步骤：
(a)连续地制备该物质组合物的一个或多个组分的浆液；
(b)将该物质组合物的一个或多个组分的浆液连续地加入到至少一个连续反应器中；
(c)在该反应器中由所述浆液连续地形成物质组合物；
(d)从所述反应器中回收所述物质组合物。
2.如权利要求1的方法，其中物质组合物是树脂材料。
3.如权利要求2的方法，其中的树脂材料是聚合物。
4.如权利要求3的方法，其中该浆液含有一种或多种单体和/或低聚物。
5.如权利要求3的方法，其中该聚合物是环氧树脂。
6.如权利要求1的方法，其中的反应器是挤出机。
7.如权利要求3的方法，该方法包括如下步骤：
(e)经过反应器和混合器之间的连接装置，把聚合物从反应器传送到混合器中；
(f)通过在混合器中将聚合物和物质组合物的一种或多种其它组分进行混合来制备该物质组合物。
8.如权利要求7的方法，其中的混合器是挤出机。
9.如权利要求7的方法，其中的物质组合物是一种涂料。
10.如权利要求9的方法，其中由(i)含平均每个分子一个以上临近环氧基团的物质，和/或(ii)含平均每个分子一个以上能够与物质(i)反应的基团的物质，来制备该浆液。
11.如权利要求10的方法，其中的物质(ii)是多羟基化合物。
12.如权利要求11的方法，其中的多羟基化合物是双酚A。
13.如权利要求10的方法，其中在步骤(f)中，与聚合物混合的一种或多种其它组分选自与环氧树脂反应的物质、不与环氧树脂反应的物质、颜料、稳定剂和填料中的至少一种。
14.如权利要求13的方法，其中与环氧树脂反应的物质是聚酯。
15.如权利要求13的方法，其中在第一反应器中制备环氧树脂，在第二反应器中制备与环氧树脂反应的物质。
16.一种制备物质组合物的设备，该设备包括：
(a)将该物质组合物一个或多个组分的浆液连续加入到至少一个连续反应器中以形成物质组合物的装置，以及
(b)从所述反应器中回收所述物质组合物的装置。
17.一种制备聚合物的设备，该设备包括：
(a)用于连续制备一种或多种单体和/或低聚物浆液的浆液容器；
(b)与所述浆液容器相连的至少一个连续反应器，所述反应器通过使一种或多种单体和/或低聚物在反应器中反应，适于连续制备一种或多种聚合物；
(c)一种将浆液连续地加入到至少一个连续反应器中以形成聚合物的装置，以及
(d)从所述反应器中回收所述聚合物的装置。
18.如权利要求17的设备，其中的反应器是一个挤出机。
19.如权利要求17的设备，该设备包括：
(e)与所述反应器连接的混合器，所述混合器适于通过在混合器中将在每个反应器中制备的聚合物、组合物的一种或多种其它组分混合来制备物质组合物，以及
(f)经过在每个反应器和混合器之间的连接装置将聚合物从每个反应器传送到混合器的装置。
20.如权利要求19的设备，该设备包括以控制速率将聚合物从每个反应器传送到混合器的装置。
21.如权利要求17的设备，其中制备的聚合物是环氧树脂。
22.如权利要求19的设备，其中与聚合物混合的至少一种或多种其它组分选自与环氧树脂反应的物质、不与环氧树脂反应的物质、颜料、稳定剂和填料中的至少一种。
23.如权利要求19的设备，其中的混合器是一个挤出机。
24.如权利要求19的设备，该设备包括制备环氧树脂的第一反应器和制备与环氧树脂反应的物质的第二反应器。
25.如权利要求24的设备，其中与环氧树脂反应的物质是聚酯。
26.如权利要求17的设备，其中的物质组合物是一种涂料。
27.如权利要求26的设备，其中的浆液是(i)含平均每个分子一个以上临近环氧基团的物质，和/或(ii)含平均每个分子一个以上能够与物质(i)反应的基团的物质的混合物。
28.如权利要求27的设备，其中的物质(ii)是多羟基化合物。
29.如权利要求28的设备，其中的多羟基化合物是双酚A。
CN00808881A 1999-06-15 2000-06-15 用浆液原料制备组合物的方法和设备 Pending CN1355738A (zh)

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ATE238098T1 (de) 2003-05-15
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