CN1802390A - 烯烃催化聚合的方法,反应器体系和它在该方法中的用途 - Google Patents

烯烃催化聚合的方法,反应器体系和它在该方法中的用途 Download PDF

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CN1802390A
CN1802390A CNA2004800157623A CN200480015762A CN1802390A CN 1802390 A CN1802390 A CN 1802390A CN A2004800157623 A CNA2004800157623 A CN A2004800157623A CN 200480015762 A CN200480015762 A CN 200480015762A CN 1802390 A CN1802390 A CN 1802390A
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冈特·魏克特
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Abstract

本发明涉及烯烃催化聚合的方法，其中烯烃在流化床中和在移动床中与颗粒状催化剂接触，从而独立地控制在流化床中的停留时间和在移动床中的停留时间；还涉及反应器体系，其包括：设置有反应物进口、产物出口和在流化床反应器中维持流化床的设备的流化床反应器和设置有直接连接到流化床反应器的进口和连接到流化床反应器的出口的移动床反应器，从而独立地控制在流化床反应器中的停留时间和在移动床反应器中的停留；以及涉及该体系用于烯烃催化聚合的用途。

Description

烯烃催化聚合的方法，反应器体系 和它在该方法中的用途
本发明涉及烯烃催化聚合的方法、特定的反应器体系以及该反应器体系用于烯烃催化聚合的用途。
烯烃的催化聚合使用齐格勒-纳塔型催化剂。包括单中心催化剂(称为齐格勒-纳塔催化剂)的用于烯烃聚合的新一代催化剂由于具有较高的活性和/或选择性而发展起来。在催化聚合期间，在催化颗粒周围的烯烃组成基本上恒定。离开反应器的反应器气体被压缩并再循环。根据需要加入补充的单体和任选的氢气。通过插入的旋风分离器分离夹带的颗粒并再循环到聚合反应器。
使用新近一代的齐格勒-纳塔催化剂制备的聚烯烃具有相对窄的分子量分布。分子量分布的宽度影响所制备的聚烯烃的流变行为和最终的机械性能。
为了获得更宽的或双峰型分子量分布，使用不同的反应器条件，如不同的单体、共聚单体和/或氢气浓度。另一个选项是使用特定的和/或结合的催化剂。
通常，系列反应器在催化聚合期间用于施加不同的反应条件以获得宽的或双峰的分子量分布。
使用流化床反应器用于烯烃气相催化聚合是本领域熟知的(EP-A-0301872)。
由于受到与流化床的产生和维持相关的对流的热传递和气流限制，聚烯烃产率较低。
通过冷凝模式的催化聚合可以增加聚烯烃产率，其中添加单体或共聚单体以使注入的液体在流化床反应器中蒸发(US-A-5,405,922)。液体反应物或惰性化合物的添加会影响流化床的维持。WO 02/41986公开了连接管的使用，经由该管更多液体组分可以供给反应器而不会干扰流化床稳定性。与已知的相同尺寸的反应器相比，这一冷凝模式催化聚合获得更高的产率。
为了获得宽的分子量分布或双峰型分子量分布，US-A-5,326,835公开了使用包括例如二个串联使用的流化床反应器的多阶段方法。
US-A-5,698,624公开了烯烃气相聚合的方法和设备，其中流化床反应器和移动床反应器形成回路结构，其中来自流化床的全部产品通过旋风分离器以便从将要再循环到流化床的气体级分中分离将要输入移动床的产品颗粒。在流化床中存在所谓的快速或湍流的流化条件，其要求特定单元操作来维持快速流化条件。另外，来自流化床反应器的全部产品流通过下向移动床，以致获得的产品在流化床反应器中和在移动床反应器中经过了基本相同的循环数。因而在该两个反应器中的停留时间不能独立地控制。
本发明的目的是提供尤其适于烯烃气相催化聚合的方法和反应器体系，它允许多种聚烯烃的生产，例如具有所需的多分散性和/或双峰性的单峰和双峰产品。
使用烯烃催化聚合的方法达到这一目的，其中烯烃在流化床中和在移动床中与颗粒状催化剂接触，从而独立地控制在流化床中的停留时间和在移动床中的停留时间。相对于总的工艺停留时间，在流化床中和在移动床中的停留时间可以独立地控制和调节。在工艺总停留时间中，在一定数量的循环期间聚合物颗粒被再循环。在流化床中和在移动床中的循环的数目可以根据本发明方法的需要进行选择。因此，可以在流化床和移动床反应器中积聚顺序形成的具有所需数目和厚度的聚合物层的聚合物颗粒。
根据优选实施方案，独立地控制在移动床中的停留时间，例如通过控制聚合物颗粒进入移动床的量而更优选通过控制聚合物颗粒离开移动床的流出量。流出速率的控制可以有调节在移动床出口中开口的形式。
在移动床中，催化聚合条件不同于在流化床中的那些条件。首先，因为在移动床中催化颗粒具有更高的密度。此外，为了施加不同的聚合条件，使用分离流体以便创造不同催化聚合条件。例如，以更低的链增长终止剂(例如氢气)浓度进行聚合。对移动床施用分离用流体导致在流化床和移动床之间反应条件的分离，从而导致在流化床和移动床中存在的聚合条件的分离。优选分离流体加到移动床的顶端并在移动床上形成缓冲，通过该分离用流体缓冲聚合物材料微粒沉降在正在形成的移动床上。分离流体可以是气体或液体。分离流体可以是对催化聚合惰性的，例如氮气和C1-C12-烷烃。
分离流体可以是反应活性的，例如单体、共聚单体例如C1-C12-链烯烃或它们的混合物。根据需要可以使用惰性的和催化聚合反应活性的分离流体的混合物。
优选使用是液体的分离流体，其在移动床中在催化聚合期间存在的条件下蒸发。因此，在蒸发期间，形成分离流体的气体缓冲，同时当使用反应活性分离流体时，放热聚合反应的冷却随同时更高的反应物浓度而发生。
分离流体并且反应物都加入到流化床和移动床可以使得在流化床中和/或在移动床中发生冷凝模式的聚合，这是对产率和选择性有利的。
本发明另一方面涉及反应器体系，其包括：设置有反应物进口、产品出口和在流化床反应器中维持流化的设备的流化床反应器，和设置有直接连接到流化床反应器的进口和连接到流化床反应器的出口的移动床反应器，从而独立地控制在流化床反应器中的停留时间和在移动床反应器中的停留时间。在这一反应器体系中，移动床与流化床相连使得所需的部分或全部流化床反应物通过移动床。通过控制在移动床反应器出口的流出速率来控制在移动床反应器中的停留时间。当移动床反应器充满颗粒状聚合物材料，则可以没有来自流化床反应器的进一步的颗粒材料加入移动床反应器并将在流化床反应器中再循环。在转换进入移动床反应器中之前，流化床反应器的流化和填充程度决定了颗粒状聚合物材料在流化床反应器中的停留时间。在移动床反应器中，停留时间取决于流出速率和颗粒状聚合物材料在进入移动床反应器后在移动床反应器内完成一个周期。
当在流化床反应器中和在移动床反应器中存在不同的聚合反应条件，那么由于在颗粒上形成不同的聚合物材料，形成的聚合物颗粒会包括多层不同的聚合物材料。
为了在流化床反应器中和尤其在移动床反应器中独立地控制停留时间，移动床反应器的进口布置在流化床反应器中使得来自流化床反应器的部分材料可以输入移动床反应器中，而其它剩余的部分进一步流化并在流化床反应器中混合。通常，离开移动床反应器的材料转移入流化床反应器中并最终从流化床反应器中排除。然而，产品也可以从移动床反应器中取出。
流化床反应器和移动床反应器的多种取向可以加以考虑，与此同时仍可以独立地控制在流化床反应器中和在移动床反应器中的停留时间。在一个实施方案中，移动床反应器布置在流化床反应器内。在另一个实施方案中，移动床反应器布置在流化床反应器周围并具有基本上环形的构型。在另一个实施方案中，移动床反应器临近流化床反应器布置或甚至布置在流化床反应器外面，同时它的进口和任选地它的出口布置在流化床反应器中。优选(如上所述)，移动床反应器至少在它的进口提供了用于供给分离流体的设备。这一分离流体优选是气体或液体，选自惰性气体或液体，例如氮气和C1-C12-烷烃，或C1-C12-链烯烃。
移动床反应器可以设置有扩散段，使得自它的进口起反应器体积增大，从而允许从在流化床中再循环的颗粒状材料中更好地分离进入移动床的颗粒状材料。在另一个实施方案中，移动床反应器可以设置有收敛段，从而自它的进口起在移动床反应器周围提供更稳定的流化床。
为了控制在移动床反应器中的停留时间，它的出口优选设置有用于控制颗粒从移动床流出速率的设备。那些流出速率控制设备可以有阀的形式或构造原理适于控制流出速率的任何形式。
最后，本发明涉及前面提到的反应器体系在烯烃催化聚合中的用途。
根据本发明方法和反应器体系提到的和其它的发明特征和优点通过多个实施方案进一步解释，这些实施方案以示例性目的给出并不打算限制本发明于此，同时参考附图。在附图中：
图1和2是用于烯烃催化聚合的根据本发明反应器体系的示意图；
图3、4和5是其它反应器体系；和
图6-9分别是用在实施例1、2、3和4中举例的方法获得的分子量分布。
图1示出了根据本发明烯烃催化聚合的反应器体系。用于根据本发明方法的烯烃包括C2-C12-烯烃，优选C2-C8-烯烃，例如乙烯、丙烯、1-丁烯、1-戊烯、1-己烯，4-甲基-1-戊烯和辛烯。这些烯烃可以用于生产均聚物。可以通过使用，例如乙烯和/或丙烯结合其它C2-C8-α-烯烃生产共聚物。更高级烯烃可以用于共聚合，例如二烯，如1，4-丁二烯、1，6-己二烯、双环戊二烯、乙叉基降冰片烯和乙烯基降冰片烯。
对于这一催化聚合使用齐格勒-纳塔催化剂，它是本领域可获得的和根据需要选择的常规催化剂。
反应器体系1包括流化床反应器2，在流化床反应器2中心设置移动床反应器3。
单体经由管线4进入流化床反应器2和任选地惰性气体、共聚单体和/或氢气经由管线5进入流化床反应器2。
反应气体经由较低空间6和气体分布盘7进入流化床反应器2。经由管线10和其它催化剂组分经由管线11供给的催化剂体系从装置9经由管线8添加。侧向围绕移动床反应器3生成并保持催化剂颗粒的流化床，在该颗粒上由于聚合反应形成聚合物。形成的聚合物的组成取决于单体、共聚单体、惰性组分和氢气的存在浓度。保持的流化床通过箭头12示出。在流化床反应器的顶部，颗粒在分离段13中与气体分离。气体经由再循环管道14离开流化床反应器，任选地在热交换器15中冷却、在压缩机16中压缩和任选地在热交换器17中进一步冷却之后再次经由流化床的进口18添加到流化床反应器2。
箭头19示出的在流化床反应器2中的部分颗粒状材料进入移动床反应器3并形成沉降聚合物颗粒床，它们大致以活塞流向下缓慢地向出口21移动，该出口部分地被经由控制线23控制的阀22封闭。在移动床3中，在聚合物颗粒向下移动的床上形成了分离流体缓冲，该分离流体经由管线24和喷管25添加。在这种情况下，这一分离流体是液体，它在移动床顶部存在的条件下蒸发。移动床顶端部分，在喷管25之上，优选通过上游蒸发的分离流体流化。
在流化床反应器2和移动床反应器3两者中充分的总停留时间之后，聚合物经由设置有阀26的出口25取出。在分离器27中，聚合物材料经由出口28分离和取出，而气态材料经由管线29和管线14再循环。
图2示出反应器体系30的另一个实施方案，其包括流化床反应器2和中心设置在流化床反应器2内的移动床反应器31。移动床反应器31具有第一上部扩散段32和第二收敛段33。
由于扩散段32和收敛段33在流化床反应器中形成了互补结构，从而形成了把流化床划分为下段35和上段36的限制34，这样有益于稳定所形成的流化床。
在图3示出的反应器37中，移动床反应器38仅具有杯子形状，从而更多来自流化床反应器2的材料被输入移动床反应器38中。
在如图4所示的反应器体系39中，移动床反应器在外壁40和圆柱形内壁41之间形成，这样移动床反应器42具有环形或空心圆筒形式而流化床反应器43中心设置。移动床反应器42的出口44是以窄环形缝形式的限制，通过该限制颗粒状材料以限定的流出速率按照箭头45流回流化床反应器43中。
最后，如图5所示的反应器体系46包括设置在流化床反应器48外边并经由进口49和出口50与其连接的单独的圆柱形移动床反应器47。出口50设置有控制阀51用于控制从移动床反应器进入移动流化床反应器的颗粒材料的流出量。
如果它们在相似条件下操作，在图1-5中示出的所有反应器类型提供基本上相同的聚合物质量。在几乎等温条件下，除了典型的参数如温度、压力、气和固相组成，“相似条件”通过以下主要变量定义：
a)固和气相在整个体系中的平均数停留时间
b)比率(平均数流化床反应器停留时间)∶(平均数移动床停留时间)
c)通过流化床和移动床的粉末周期的平均数/总平均停留时间
d)注入液体的量
e)比率(在流化床反应器中固体量)：(在移动床反应器中固体量)
流化行为受到流化床反应器和移动床反应器设计的影响，但在很宽的几何变量范围内是可控制的。
当反应器在“相似条件”下操作时，以下实施例的结果基本上不取决于具体的设计。不会观测到器壁结膜(sheeting)。在所有施加的条件下，温度梯度总是小的。
实施例1：
在75℃和28巴的压力下操作特征为总生产率为20千克每小时的中试反应器。对流化床反应器和移动床反应器两者来说，通过控制移动床反应器中的粉末通量，乘积P＝(平均停留时间)x(聚合速率)保持大致恒定(大约25个周期/整个体系的平均停留时间)。反应器入口的气体组成保持恒定(88mol％的丙烯和12mol％的氢气)。
第一，体系没有经由管线24供给分离流体就已经运行。这导致如图2所示的相对窄的分子量分布(j为链长和Yj为链长分布密度函数)。因为在整个反应器区域内相对高的氢气浓度(12mol％)，所以平均分子量是低的。
图6
实施例2
通过经由管线24供给更多催化剂到反应器和供给液体丙烯作为分离流体，在如实施例1描述的同等状态下起动双峰模式的操作。分子量分布显著地加宽(参见图7)，在达到稳态条件后生产率达到32千克/小时。
Figure A20048001576200112
图7
重均链长为大约4070对应于170.000克/摩尔的重均分子量。达到大约3.6的多分散度(MWD)和双峰性。同时在实施例1和2中，在流化床反应器和移动床反应器中生产的聚合物的比率几乎相同。
实施例3
在图3的构型中使用显示强烈氢气响应的催化剂。反应条件与描述在实施例2中的相同。显然，与移动床反应器相比流化床反应器中的生产率更高。因此，观察到更清楚的双峰性，并且低分子量峰比高分子量部分更高。
Figure A20048001576200121
图8
因此，多分散度更高并达到大约5.6(重均分子量大约为205.000g/Mol)。
实施例4
在90℃和22巴下聚合乙烯。测量到仅大约11个聚合物周期/平均固体停留时间。生产率(在稳态中)为16千克聚合物/小时。液体丙烷用作分离流体。因为在移动床反应器部分中长的停留时间(以减少的单体浓度和非常低的氢气浓度)，所以高分子量部分减少(参见图9)，但是观察到产品的(弱)双峰性。重均链长略微超过4000，而多分散度为大约7.8。
图9

Claims (19)

1.烯烃催化聚合的方法，其中烯烃在流化床中和在移动床中与颗粒状催化剂接触，从而独立地控制在流化床中的停留时间和在移动床中的停留时间。
2.根据权利要求1的方法，其中独立地控制在移动床中的停留时间。
3.根据权利要求1或2的方法，其中通过控制颗粒从移动床的流出速率来控制在移动床中的停留时间。
4.根据权利要求1-3的方法，其中移动床通过分离流体与流化床分离。
5.根据权利要求4的方法，其中将分离流体供给移动床。
6.根据权利要求4或5的方法，其中分离流体是气体或液体，选自惰性气体或液体，例如氮气，C1-C12-烷烃或烯烃，例如C1-C12-烯烃，或它们的混合物。
7.根据权利要求6的方法，其中分离流体是在存在的聚合条件下蒸发的液体。
8.根据权利要求5-7的方法，其中液体烯烃作为分离流体添加以使移动床中的聚合是冷凝模式聚合。
9.根据权利要求1-8的方法，其中液体烯烃添加到流化床以使流化床中的聚合是以冷凝模式聚合。
10.根据权利要求4-9的方法，其中分离流体是聚合单体或共聚单体，或它们的混合物。
11.反应器体系，其包括：设置有反应物进口、产物出口和在流化床反应器中维持流化床的设备的流化床反应器，和设置有直接连接到流化床反应器的进口和连接到流化床反应器的出口的移动床反应器，从而独立地控制在流化床反应器中的停留时间和在移动床反应器中的停留。
12.根据权利要求11的反应器体系，其中移动床反应器的进口设置在流化床反应器中。
13.根据权利要求11或12的反应器体系，其中移动床反应器的出口连接到流化床反应器。
14.根据权利要求11-13的反应器体系，其中移动床设置在流化床反应器中、围绕着流化床反应器或邻近于流化床反应器。
15.根据权利要求11-14的反应器体系，其中移动床反应器设置有用于供给分离流体的设备。
16.根据权利要求11-15的反应器体系，其中分离流体是气体或液体，选自惰性气体或液体，例如氮气和C1-C12-烷烃，或烯烃，如C1-C12-烯烃。
17.根据权利要求11-16的反应器体系，其中移动床反应器的进口设置有扩散段。
18.根据权利要求15-17的反应器体系，其中移动床反应器的出口设置有用于控制颗粒从移动床反应器流出速率的设备。
19.根据权利要求17-19的反应器用于烯烃催化聚合的用途。
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