CN1301786C - 聚合反应器 - Google Patents
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Abstract
联接到环管反应器(1)下部的聚合反应器沉降支管。导管(2)焊接到环管反应器上,并通向上部阀门(3)和下部隔断阀(4)。下部隔断阀(4)的下游是另外的通向下部区域(6)和产品输出(PTO)阀(7)的导管(5)。导管(5)具有比导管(2)显著大的横截面积。使用中,隔断阀(3)和(4)始终开启,使得来自反应器环管的淤浆进入沉降支管。PTO阀(7)有规律地打开,使得沉降的聚乙烯“绒毛”沿导管(8)快速排出。导管(5)的较大的面积显著增加了聚乙烯“绒毛”的沉降速度和聚合物浓度。
Description
本发明涉及一种用于制造聚合物的装置,更具体地,本发明涉及聚合反应器的沉降支管的设计。
典型地在加压的环管反应器中,使用所谓淤浆系统(slurry system),其中聚合物随着液态反应物围绕环管反应器循环而连续形成,按照Phillips工艺制造聚合物例如聚乙烯。聚合物作为固体悬浮在液体中形成。
当用该方法制备聚乙烯时,高纯乙烯和某些其它材料供应到反应器中。用低沸点烃例如异丁烷溶解反应器中的乙烯单体,并悬浮催化剂和聚合物颗粒。异丁烷在实际聚合反应中没有任何反应,所以其最后被回收、纯化和重复利用。另外,加入烃来控制制备的聚乙烯的分子量,而加入1-己烯共聚单体以便控制产品密度。典型地使用铬、Ziegler Natta或茂金属催化剂催化反应。
乙烯气体、稀释剂和粒状催化剂连续地供入环管反应器,其中用泵将它们快速循环。典型地保持反应器核心的温度在100℃的数量级,压力在4MPa的数量级。在通常操作过程中,反应器含有大约40重量%的聚乙烯。随着过程继续,聚合物颗粒开始形成,更大的作为“绒毛”(fluff)沉淀,并进入沉降区,从沉降区浓缩的淤浆周期性的排出。
制备系统是连续的,使得产品以其形成的同样的速度除去。聚合物产品与异丁烷稀释剂混合,并且明显地希望降低随聚合物离开反应器的异丁烷量。在被送回反应器前,该异丁烷必须纯化并再压缩,这显著增加了工艺的成本。
为了在排出前增加聚合物的浓度,使用沉降支管(settling leg)(或堆放支管)。沉降支管是通过焊接在环管反应器上的出口导管,与环管反应器的部分连接的导管。选择沉降支管的几何形状使得其中的液体比较静止,以便增加绒毛沉降。沉降支管的向外流动由阀门的布置控制,使得浓缩的淤浆周期地从反应器中排出。
尽管建议和使用了其它的布置,对沉降支管最普遍的系统是采取从环管反应器核心的最下面的点向下延伸的垂直管路的形式。沉降支管典型地通过一个或两个隔断阀和附加的在沉降支管的低端配备的所谓产物输出阀(product take-off valve)(PTO)连接到反应器上。布置沉降支管与环管反应器的关系,使得淤浆经过其中的出口的流动提供其中聚合物颗粒从稀释剂中有一点沉降出来的静止区(resting zone)。这可能增加聚合物浓度至60重量%。
隔断阀只有在反应器的无规运转的情况下关闭,例如堵塞,以能够为维护或清洗的目的安全卸下沉降支管。(当它们打开时,其不妨碍支管)因此,在操作过程中,隔断阀持续打开,以便淤浆从反应器能够进入到沉降支管。因为与稀释剂相比聚合物绒毛更高的密度,沉降支管中的绒毛浓度将增加。已知沉降的产品量(即在支管中产品的浓度)取决于颗粒性质、稀释剂密度、支管的横截面积和静止时间。
在已知为燃烧(firing)的工艺中,沉降支管的内容物周期地使用PTO阀排出。在典型的反应器中,存在许多沉降支管,并且每个在不同的时间每分钟燃烧大约1次。为了燃烧支管,PTO阀开放几秒钟。反应器内的压力快速使得支管中的内容物通过PTO阀来到闪蒸室,其中闪蒸混合物,以基本全部除去稀释剂和任何痕量的单体。
此种布置是已知的,并解释于例如US-A-5183866,其首先涉及稀释剂的蒸发的改进。另外的实例是US-A-4461889,其建议在沉降支管的下游使用过滤器容器,以便在聚合物送入闪蒸罐前,促进聚合物固体从稀释剂中的排出。
将要理解在沉降支管中,聚合物在沉降支管中沉降(使得然后可能被排出)的速度,对反应器的整个生产速度有显著影响。其也决定稀释剂流到反应器的速度。每单位时间聚合物沉降的质量称作沉降速度,在现代的环管反应器中沉降速度是对增加生产能力主要的限制之一。可以通过增加稀释剂容量来解决该限制,单质这需要对典型的反应器的极端昂贵的改造。
已经提及,沉降速度取决于聚合物绒毛性质。这些又反过来由催化剂性质决定,不能正常地改变而不影响最终聚合物产品的性质。实际上,从一种催化剂变为另一种(例如为制备具有不同性质的聚合物)可以改变绒毛的性质至生产能力降低25%的程度。例如,如果使用旋转注模法(rotomoulding)的茂金属催化剂制造聚合物,与使用铬催化剂制造的吹模的聚合物相比,可以看到如此降低。因此,在此情况下,增加沉降速度的普遍需要可能特别迫切。
另外,如果聚合物固体含量太低,引起闪蒸槽的操作问题。这是因为闪蒸槽被设计使用喂入其中的材料的热量。固体聚合物具有比稀释剂更高的热容,所以更低的聚合物含量可能导致到达闪蒸槽的热量太少,以致于不能完全蒸发稀释剂。
为了提供改进的聚合物沉降并由此降低淤浆中稀释剂的含量,US-A-4613484说明了使用不同的沉降支管的布置。这些包含使用倾斜的部分与从沉降支管中出来的稀释剂再循环管路和向沉降支管供应的小稀释剂流的结合。但是,建造倾斜的沉降支管造成实际的困难,而提供稀释剂再循环和稀释剂喂料管路涉及的附加的管路和阀门显著增加了复杂性程度和成本。
EP-A-0891990确定了使用沉降支管造成的瓶颈问题,并解释:增加沉降支管的直径引起明显的问题,因为增加环管和支管之间的隔断阀的直径是不实际的。作为后果,该文献解释:本领域的通常实践是增加每个环管上沉降支管的数量。但是,这也引起实际的困难,因为要求的支管数量开始超出了可利用的空间。回应这些问题,该文献建议通过增加反应器中淤浆的聚合物浓度,并利用连续产品输出,完全消除沉降步骤。
WO01/05842也公开了设计用于连续产品输出的环管反应器。
将会意识到在许多情况下,该方法是不适合的,而且改进反应器条件来使得要使用的连续输出成为可能经常是不可能或不希望的。例如不能提高淤浆的聚合物浓度至超出淤浆流动特性赋予的特定限制。
根据本发明,提供了用于聚合反应器的沉降支管,其包含在流体传输中用于与聚合反应器连接的第一管状部分,和通过至少一个隔断阀与第一管状部分连接的第二管状部分,其中所述第二管状部分具有比第一管状部分大的内横截面积。
因此,利用本发明,沉降支管包含增加的横截面积的部分,该部分在使用中在阀的下游。(通常,管状部分是环形的横截面,所以这将与直径的增加相一致。)因此,利用本发明,隔断阀的尺寸不限制沉降支管的最大直径。如EP-A-0891990(参考上述)中解释的,已经认为隔断阀的直径限制沉降支管的直径。
符合通常的实践,优选存在两个阀门,而且这些典型地具有在全部打开时,与第一管状部分的内径基本相同的内径。
已经发现,与具有和第一部分相同的恒定直径的沉降支管相比,该布置对改进聚合物沉降的速度有显著影响。因此,本发明基于以下出乎意料的发现:与本领域被接受的知识相反,可以改进沉降速度而不增加与反应器连接的沉降支管部分的直径,而且不增加隔断阀的尺寸。这是因为已经发现沉降速度由支管的下部的直径确定-已经发现上部的直径不起决定作用。因此可以比以前更容易和更经济地改进沉降速度。
而且,与相同体积的沉降支管相比,其中第一和第二部分是相等直径的,本发明也提供增加的体积对长度的比例,其有助于在支管燃烧过程中,防止排出高稀释剂浓度的淤浆。
第一管状部分优选包含小于支管长度的一半,并仅用作将阀与环管反应器连接。
本发明并不限于第一和第二部分的具体尺寸-这些可以随给定情况的需要而选择。但是,为了本发明具有任何显著的优点,第二部分应该比第一部分的直径大至少10%。为进一步提高性能,第二部分优选大25%或高达50%或更多。人们相信当该值为100%时-即第二部分的直径是第一部分的两倍时,达到了实践的上限。
对于最佳的全面性能,第一部分的直径对第二部分的直径比例优选为1∶1.1~1∶2,更优选为1∶1.2~1∶1.6,最优选为1∶1.25~1∶1.5。
虽然实际管子的直径可以变化,第一部分优选8~12英寸。第二部分直径优选10~14英寸,虽然其可以高达30英寸。(这里使用的管子的尺寸是按本领域规定的典型的标称尺寸,如传统以英寸度量。)。例如,直径可以是直径标称8和10英寸,或直径标称10和12英寸。
在本发明特别优选的形式中,沉降支管包含连接反应器环管部分的第一管状部分(例如标称8″),其下游是一双隔断阀,更下游直径增加以形成依次连接PTO阀的第二管状部分(例如标称10″)。
本发明还扩展到包含前述的沉降支管的聚合反应器。与可能不具有本发明的沉降支管的反应器相比,此反应器可以以更高的生产速度操作,因为更高的沉降速度使得产品从反应器中移除的更迅速。
本发明也扩展到可以使用描述了的沉降支管来制备聚合物的方法。因此,从另一方面看,本发明提供包含使用前述的反应器制备聚合物的方法。更具体地,其提供了制备聚合物的方法,该方法包含向环管反应器提供反应物、稀释剂和催化剂,并周期性的从中由沉降支管排出聚合物的步骤,其中所述沉降支管包含与环管反应器连接的第一部分、所述第一部分下游的并被隔断阀从中隔离的第二部分,所述第二部分具有比所述第一部分大的直径,聚合物从沉降支管的流动被所述第二部分下游的周期性开放的阀门控制。
另外,本发明扩展到使用该反应器或该方法制备的聚合物。
现在将仅以实例的形式并参考附图说明本发明的实施方式。
图1是现有技术沉降支管的示意图;和
图2是本发明的沉淀支管的相应图。
如可以从图1看出的,已知的沉降支管与环管反应器1的下部连接。8″标称直径的(实际上219mm外径和189mm内径)导管2焊接到环管反应器上,并通向上部隔断阀3和下部隔断阀4。
下部隔断阀4的下游是另一个标称直径8″的导管5。其依次通向下部区域6和PTO阀7。该PTO阀7控制流入通向闪蒸罐(未示出)的导管8。
隔断阀只有维护或紧急情况下才关闭。下部隔断阀4与上部隔断阀3完全相同并作为安全装置配备。因此,使用中,隔断阀始终开放使得来自反应器环管的淤浆进入沉降支管。
淤浆主要是单体(乙烯)、稀释剂(异丁烷)、共聚单体(1-己烯)、氢和催化剂的液体混合物。反应器内部的压力大约4Mpa。其围绕环管反应器以大约10-12m/s的速度循环。典型的停留时间是45分钟。
当其制造出来,聚乙烯形成悬浮于淤浆中的固体“绒毛”。在沉降支管内,淤浆比较静止,所以绒毛沉降出来并沉到支管的底部,由此其浓度从40重量%增加到60重量%。
图解的沉降支管是与环管反应器的底部连接的许多中的一个。PTO阀7每分钟打开几秒钟,由此这些中的每个周期性的“燃烧”。阀7下游的压力仅为0.15Mpa(与4MPa的上游相比),所以其内含物沿导管8快速排出。
导管8通向其中分离出聚合物绒毛或粉末的闪蒸槽。然后纯化剩下的异丁烷,加压然后返回反应器。
图2图解了与图1相同的沉降支管,除了导管5的直径增加到10″标称(实际上273mm外径和222mm内径)。8″直径部分长1.9m,而10″直径部分长1.7m,总长为3.6m。
以与图1相同的方式操作图2的沉降支管,但是由于导管5的直径增加,沉降速度和聚合物浓度显著增加。
Claims (9)
1.一种用于聚合反应器的沉降支管,其包含在流体传输中用于与聚合反应器连接的第一管状部分,及通过至少一个隔断阀与所述第一管状部分连接的第二管状部分,其中所述第二管状部分具有比第一管状部分大的内横截面积。
2.根据权利要求1的沉降支管,其中所述第一管状部分包含小于一半的所述沉降支管的长度。
3.根据权利要求1的沉降支管,其中所述管状部分的截面是环形的,而且所述第一部分的直径与所述第二部分的直径的比例为1∶1.1~1∶2。
4.根据权利要求2的沉降支管,其中所述管状部分的截面是环形的,而且所述第一部分的直径与所述第二部分的直径的比例为1∶1.1~1∶2。
5.根据权利要求1~4中任一项的沉降支管,其中所述第二部分的横截面积比所述第一部分大至少50%。
6.根据权利要求1~4中任一项的沉降支管,其中所述第一部分的标称直径为8~12″,所述第二部分的标称直径为10~14″。
7.根据权利要求5的沉降支管,其中所述第一部分的标称直径为8~12″,所述第二部分的标称直径为10~14″。
8.包含前面权利要求任一项的沉降支管的聚合反应器。
9.一种利用权利要求1~7中任一项的沉降支管制备聚合物的方法,包括向环管反应器中提供反应物、稀释剂和催化剂,并通过沉降支管周期性地从反应器中排出聚合物的步骤,其中所述沉降支管包含与环管反应器连接的第一部分,所述第一部分下游的并被隔断阀从中隔离的第二部分,所述第二部分具有比所述第一部分大的直径,通过周期性地开启第二部分下游的阀门,控制来自沉降支管的聚合物的流动。
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Application Number | Priority Date | Filing Date | Title |
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EP01309185A EP1310295B1 (en) | 2001-10-30 | 2001-10-30 | Polymerisation reactor |
EP01309185.5 | 2001-10-30 |
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CN1599639A CN1599639A (zh) | 2005-03-23 |
CN1301786C true CN1301786C (zh) | 2007-02-28 |
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CNB028239822A Expired - Fee Related CN1301786C (zh) | 2001-10-30 | 2002-10-30 | 聚合反应器 |
Country Status (6)
Country | Link |
---|---|
US (1) | US6964754B2 (zh) |
EP (1) | EP1310295B1 (zh) |
CN (1) | CN1301786C (zh) |
AT (1) | ATE367198T1 (zh) |
DE (1) | DE60129444T2 (zh) |
WO (1) | WO2003037499A1 (zh) |
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- 2001-10-30 DE DE60129444T patent/DE60129444T2/de not_active Expired - Fee Related
- 2001-10-30 AT AT01309185T patent/ATE367198T1/de not_active IP Right Cessation
- 2001-10-30 EP EP01309185A patent/EP1310295B1/en not_active Expired - Lifetime
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2002
- 2002-10-30 WO PCT/EP2002/012111 patent/WO2003037499A1/en not_active Application Discontinuation
- 2002-10-30 US US10/494,078 patent/US6964754B2/en not_active Expired - Fee Related
- 2002-10-30 CN CNB028239822A patent/CN1301786C/zh not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
DE60129444D1 (de) | 2007-08-30 |
US6964754B2 (en) | 2005-11-15 |
CN1599639A (zh) | 2005-03-23 |
DE60129444T2 (de) | 2007-10-31 |
ATE367198T1 (de) | 2007-08-15 |
EP1310295A1 (en) | 2003-05-14 |
EP1310295B1 (en) | 2007-07-18 |
US20050038206A1 (en) | 2005-02-17 |
WO2003037499A1 (en) | 2003-05-08 |
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