CN101410176B - 多环流反应器中的冲洗 - Google Patents
多环流反应器中的冲洗 Download PDFInfo
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Abstract
本发明公开了多环流反应器,其中可停止使用或者重新打开将聚合物产物从一个环路输送至下一环路的沉降腿之一而不干扰所述多环流反应器的运行。
Description
本发明涉及一种多环流反应器,其中将聚合物产物从一个环路输送至下一环路的沉降腿之一可停止使用或者重新打开而不干扰所述多环流反应器的运行。
高密度聚乙烯(HDPE)最先是通过在为所得聚合物的溶剂的液体中进行的加成聚合而生产的。该方法迅速被依照齐格勒或菲利浦斯的在淤浆条件下的聚合所替代。更具体而言,淤浆聚合在管式环流反应器中连续地进行。形成聚合反应流出物,其为悬浮在通常为反应稀释剂和未反应单体的液体介质中的颗粒聚合物固体物的淤浆(参见US-A-2,285,721)。合意的是将聚合物与包含惰性稀释剂和未反应单体的液体介质分离而不将液体介质暴露于污染物,使得所述液体介质可在最低限度的纯化或无纯化下再循环至聚合区域。如US-A-3,152,872中所述,将聚合物与液体介质的淤浆收集在淤浆环流反应器的一个或者多个沉降腿中,所述淤浆周期性地从所述沉降腿排放到闪蒸室中,闪蒸室由此以间歇方式操作。
闪蒸混合物以从聚合物中除去液体介质。然后必须再压缩气化的聚合稀释剂以将其浓缩至液态,然后,若必须纯化,则在纯化后将其作为液体稀释剂再循环至聚合区域。
通常需要沉降腿以提高在从反应器抽取出的淤浆中的聚合物浓度;但是由于沉降退将间歇技术强加于连续工艺上,因而沉降腿存在若干问题。
EP-A-0,891,990和US-A-6,204,344公开了两种用于减少反应器的不连续行为从而提高固体物浓度的方法(EP-A-0,891,990)。一种方法在于通过富集淤浆的连续回收代替沉降腿的不连续运行。另一种方法在于使用更强劲的循环泵(US-A-6,204,344)。
新近,EP-A-1410843公开了一种淤浆环流反应器,该反应器包括在环路之一上通过与主路线具有不同输送时间的替换路线来连接同一环路的两点的支路管线,用于提高循环淤浆的均匀性。
所述均聚和共聚也可在由两个管式环流反应器所组成的双环流***中进行,所述两个管式环流反应器各自优选使用沉降腿技术并且通过输送管线串联连接,所述***在本说明书中也称为“双峰(bimodal)反应器”。
双峰反应器由于通过在各个反应器中提供不同的聚合条件而提供了制备高度特制的聚烯烃的可能性而十分令人满意。然而,由于在当前的结构下,双环流反应器需要彼此接近以确保生长聚合物从一个环路到另一个环路的足够输送,因而通常难以找到合适的空间来建造这些双环流反应器。在输送管线中循环的物料的平均速度小于1米/秒:因而该管线必须非常短以避免由于残存单体的聚合导致的沉降和堵塞。
因此,需要提供改进的装置以连接两个可彼此远离的现有反应器,或者,建造两个不需要彼此接近的新反应器(如果可用空间这样要求的话),以便成功地进行烯烃淤浆聚合。
在双峰***中,压力通常通过所述腿的设定值与卸料(dumping)之间的相互作用而进行控制。每当达到设定值时,便将一个腿卸料并且因此,压力下降至低于设定值的值:这对于维持压力控制是必需的。如果压力降不充分,则存在用于恢复控制的方案。这种类型的控制对于将作为间歇过程的腿卸料与作为连续过程的在环流反应器中的聚合连接起来是必要的。
在现有技术中,操作双环流反应器的常规方法是用静态设定值和用静态压力差工作。在这样的条件下,难以在两个环流反应器之间维持恒定的压力差,因为所述控制应用于间歇排放和连续运行的混合。
本发明的目的是提供用于连接两个或者多个环流反应器的控制装置(means)。
本发明的目的还为停止使用或者重新打开沉降腿而不干扰***的运行。
本发明的另一个目的为减少物料在连接各反应器的管线中的停留时间。
本发明的又一个目的是改进环流反应器中的流体均匀性。
本发明的进一步目的是增加双环流反应器的循环泵的排量(capacity)。
通过本发明(至少部分地)实现了这些目的中的任何一个。
附图说明
图1示意性地表示本发明中所使用的沉降腿单元。
图2示意性地表示本发明中所使用的将循环流体运送至压力控制容器的***。
因此,本发明公开了包括至少两个串联连接的环路的淤浆环流反应器,其中通过输送管线(10)将图1中所示的第一反应器(1)的至少一个沉降腿单元连接到下一反应器,并且其中所述沉降腿单元包括:
-主阀(2),其布置用于允许聚合物产物进入沉降腿;
-沉降腿(3);
-产物取出(PTO)阀(4),其将沉降腿连接到输送管线(10);
-冲洗管线(5),其布置用于将冲洗流体运送到沉降腿内并包含受主进样阀(2)的位置控制的自动阀(6);
-压力容器(7),其包含被柔韧的膜(11)分开的增压气体(8)和冲洗流体(9)的两相体系;
-冲洗流体输入管线(12),其包含压力调节阀(13)。
在包括至少两个串联连接的环流反应器的本发明的淤浆环流反应器中,连接两个环路的管线经受动态压力差。第二反应器的设定值与第一反应器的过程值直接关联。该动态控制***能将两个反应器中的间歇卸料过程与连续的聚合过程相关联,由此一直维持期望的压差。
本发明的沉降腿单元允许腿的停止使用和重新打开而不干扰反应器的运行。当允许聚合物产物进入腿中的主阀(2)(通常为Borsig阀)关闭时,冲洗程序开始并且持续通常约2分钟的时间。自动阀(6)打开并且允许冲洗流体进入沉降腿内。在压力容器中经受增压气体的压力的冲洗流体快速地流入沉降腿内。同时,PTO阀打开并且以通常为1转/秒的速度旋转,将聚合物产物释放到输送管线内。随后运行压力调节阀(13)以允许更多的冲洗流体进入冲洗管线中。如果PTO阀处于打开位置(意味着PTO阀以1转/秒的速度旋转),则额外的冲洗流体直接流向沉降腿。通常,PTO阀保持运行约两分钟。当PTO阀关闭时,沉降腿完全地被冲洗流体充满并且压力容器被再加压。这终止了冲洗程序。当主阀(2)关闭时自动阀(6)保持打开,由此将沉降腿保持在冲洗流体压力下。因此,沉降腿停止使用而不停止反应器的运行。当再次需要重新打开沉降腿时,可简单地通过打开主阀(2)以及与之相关联的自动阀(6)的自动关闭而将沉降腿重新打开。该***通常用于清洗腿。
优选地,压力容器中的增压气体为氮气。冲洗流体可为新鲜溶剂或者单体,优选地,其为循环溶剂、或者循环单体、或者其组合,更优选地,其为循环溶剂。
在图2中所示的根据本发明的最优选的实施方式中,冲洗流体为循环溶剂,优选为循环异丁烷(iC4)。
当下游压力低于给定值时,位于压力容器之前的冲洗管线之上的自动压力阀打开。自动压力阀必须缓慢地打开以避免循环泵(21)的气穴(cavitation)现象,所述循环泵(21)在使用循环溶剂和/或单体时是必要的。
包含在容器(20)中的循环溶剂被送至循环泵(21)。通过控制阀(22)调节溶剂流量以将泵的流速维持在通常为约7.5吨/小时的恒定值。溶剂的一部分通过管线40、41和42送至环流反应器,其它部分通过管线23送至一个或多个压力容器(30)。管线23装有监测和作用于下游压力的变化的压力控制器(24)。在将循环溶剂送至其压力容器的各条管线(32)上存在限制进入所述腿中的最大速度的节流孔板(31),以在PTO泄漏的情况下保护***免于出现气穴现象。
在根据本发明的该优选的实施方式中,双环流反应器包括通过与主路线具有不同输送时间的替换路线而将第二环流反应器的两点连接起来的支路管线,所述支路管线还收集通过输送***排出第一环流反应器的生长聚合物,并且将所述生长聚合物送至第二反应器。输送***理想地包括一个或多个各自通过产物取出(PTO)阀连接到输送管线的沉降腿。该***已描述于例如WO06/003144中。
在整个本说明书中,将形成淤浆环流反应器的环路串联连接,并且各个环路可折叠。
任选地,所述管线可装有夹套。
当使用支路管线时,在连接环流反应器的管线中循环的物料的速度必须足以避免沉降和可能的堵塞:该速度必须至少为3米/秒。
本发明可与所有类型的催化剂体系一起使用。本发明可用于烯烃的均聚或者共聚。优选的单体为乙烯和丙烯,更优选乙烯。优选的共聚单体为乙烯、丙烯和己烯。合适的稀释剂是本领域中众所周知的,并且包括在反应条件下为惰性和液态的烃。它们包括异丁烷、丙烷、正戊烷、异戊烷、新戊烷和正己烷,更优选异丁烷。
本环流反应器已被证明对于用茂金属催化剂体系制备双峰聚乙烯特别地有用。
实施例
用循环异丁烷在30秒内代替被停止使用的腿和其输送管线的总体积为36L的内容物。每个腿的平均冲洗速度为2.3吨/小时。
循环异丁烷的泵的排量如下:
-至第一反应器的为1.8吨/小时;
-至第二反应器的为4.4吨/小时,其分为:用于冲洗沉降腿的为1吨/小时,用于冲洗输送管线的为0.4吨/小时,和至反应器的为3吨/小时,
-重新送至循环泵的为1.3吨/小时。
当下游压力低于48巴表压(barg)时,冲洗管线的压力控制(PIC)阀(24)打开。将其缓慢打开以避免泵的气穴现象。
通过减少去往泵的再循环以及降低去往第一和第二反应器的流量来抵消冲洗速度的突然增加。在48巴表压的压力下PIC调节为4.6吨/小时的iC4,这对于同时冲洗2个腿是需要的。
在冲洗循环过程中***中的高的压力变化通过安装压力容器(每个腿有一个压力容器)和置于压力控制阀(PIC)(24)之上的缓慢发生作用的制动器(actuator)补偿。在冲洗循环之初,当允许聚合物产物进入沉降腿中的Borsig阀关闭时,腿的冲洗管线上的开/关阀自动打开,并且当PTO阀打开且以1转/秒的速度旋转时,沉降腿中的压力下降。当异丁烷冲洗管线上的PIC阀缓慢地打开时,来自压力容器的异丁烷流至腿。当PIC阀打开时,来自泵的流体或者在PTO阀打开时去往沉降腿,或者去往压力容器以限制循环泵处的压力变化。
两分钟后,通过关闭PTO阀结束冲洗。
位于各个腿的冲洗管线之上的节流孔板(31)在7巴表压的压差下将去往任何一个腿的最大冲洗速度限制为2.3吨/小时,以在PTO泄漏的情况下保护***免于发生气穴现象。
当通过PIC阀的流量超过循环泵的流量时,将去往第二反应器的流量中断以增加(free up)冲洗排量。这对于一个腿的冲洗是足够的。当同时冲洗两个腿时,必须减少输送管线的冲洗,这也是为了进一步增加冲洗排量。
三个腿可以有可能被同时关闭。在该情况下,隔离反应器比确保沉降腿的适当冲洗显得更好。
Claims (9)
1.一种包括至少两个串联连接的环流反应器的淤浆环流反应器,其中通过输送管线(10)将第一环流反应器(1)的至少一个沉降腿单元连接到第二环流反应器,并且其中所述沉降腿单元包括:
-主阀(2),其布置用于允许聚合物产物进入所述沉降腿;
-沉降腿(3);
-产物取出(PTO)阀(4),其将所述沉降腿连接到所述输送管线(10);
-冲洗管线(5),其布置用于将冲洗流体运送到所述沉降腿内并包括受主阀(2)的位置控制的自动阀(6);
-压力容器(7),其包含被柔韧的膜(11)所分开的增压气体(8)和冲洗流体(9)的两相体系;
-冲洗流体输入管线(12),其包含压力调节阀(13)。
2.权利要求1的淤浆环流反应器,其中当主阀(2)关闭时,自动阀(6)自动打开。
3.权利要求1或2的淤浆环流反应器,其中所述冲洗流体为循环溶剂、或者循环单体、或者其组合。
4.权利要求3的淤浆环流反应器,其中所述冲洗流体为循环异丁烷。
5.权利要求1或2的淤浆环流反应器,其中所述增压气体为氮气。
6.权利要求1或2的淤浆环流反应器,其中两个环流反应器通过支管线路连接,所述支管线路通过与主路线具有不同输送时间的替换路线而连接第二环流反应器的两点,所述支路管线还收集通过输送***排出第一环流反应器的生长聚合物并将所述生长聚合物送至第二环流反应器。
7.权利要求1到6中任一项的淤浆环流反应器在乙烯或α-烯烃的均聚或共聚中的用途。
8.权利要求7的用途,其用于乙烯的均聚或共聚。
9.权利要求1到6中任一项的淤浆环流反应器用于清洗一个或多个沉降腿而不干扰所述淤浆环流反应器的运行的用途。
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EP06112008.5 | 2006-03-30 | ||
EP20060112008 EP1839742A1 (en) | 2006-03-30 | 2006-03-30 | Flushing in a multiple loop reactor |
PCT/EP2007/052908 WO2007113167A1 (en) | 2006-03-30 | 2007-03-27 | Flushing in a multiple loop reactor |
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CN101410176B true CN101410176B (zh) | 2012-05-02 |
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US (1) | US7985378B2 (zh) |
EP (2) | EP1839742A1 (zh) |
JP (1) | JP5179466B2 (zh) |
KR (1) | KR101176388B1 (zh) |
CN (1) | CN101410176B (zh) |
AT (1) | ATE457829T1 (zh) |
DE (1) | DE602007004836D1 (zh) |
DK (1) | DK2004323T3 (zh) |
EA (1) | EA014616B1 (zh) |
ES (1) | ES2340627T3 (zh) |
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WO (1) | WO2007113167A1 (zh) |
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EP2055725A1 (en) * | 2007-11-05 | 2009-05-06 | Total Petrochemicals Research Feluy | Reduced blockage when transferring polymer product from one reactor to another |
CN105008413B (zh) * | 2013-01-22 | 2017-02-22 | 道达尔研究技术弗吕公司 | 具有连续排放的烯烃聚合工艺 |
BR112015016302B1 (pt) * | 2013-01-22 | 2020-05-26 | Total Research & Technology Feluy | Processo de polimerização de olefinas com descarga contínua |
KR102462535B1 (ko) | 2019-10-17 | 2022-11-01 | 주식회사 엘지화학 | 올리고머 제조 장치 |
CN114643136B (zh) * | 2022-04-11 | 2024-03-26 | 中国神华煤制油化工有限公司 | 甲醇制烯烃工艺急冷塔气液旋流分离器的冲洗***及方法 |
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JP2009531498A (ja) | 2009-09-03 |
DE602007004836D1 (de) | 2010-04-01 |
JP5179466B2 (ja) | 2013-04-10 |
ES2340627T3 (es) | 2010-06-07 |
ATE457829T1 (de) | 2010-03-15 |
EP2004323B1 (en) | 2010-02-17 |
KR101176388B1 (ko) | 2012-08-27 |
EA200802094A1 (ru) | 2009-04-28 |
KR20080114755A (ko) | 2008-12-31 |
EA014616B1 (ru) | 2010-12-30 |
US20090246092A1 (en) | 2009-10-01 |
EP1839742A1 (en) | 2007-10-03 |
CN101410176A (zh) | 2009-04-15 |
US7985378B2 (en) | 2011-07-26 |
WO2007113167A1 (en) | 2007-10-11 |
EP2004323A1 (en) | 2008-12-24 |
PT2004323E (pt) | 2010-05-06 |
DK2004323T3 (da) | 2010-05-17 |
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