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CN1039427A - 气相聚合方法和设备 - Google Patents

气相聚合方法和设备 Download PDF

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CN1039427A
CN1039427A CN89104801A CN89104801A CN1039427A CN 1039427 A CN1039427 A CN 1039427A CN 89104801 A CN89104801 A CN 89104801A CN 89104801 A CN89104801 A CN 89104801A CN 1039427 A CN1039427 A CN 1039427A
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琼-克劳德·希诺
安德烈·杜梅因
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Abstract

链烯在恒温下的流化床反应器中气相聚合的方法和设备。包含要被聚合链烯的气态反应混合物通过反应器并靠循环线路循环进入反应器，循环线路包括第一传热装置、压缩机和第二传热装置。包括把易挥发液态烃导入第一传热装置的进口或在上流在第一传热装置附近导入循环线路。第一传热装置把气态反应混合物冷却到低于T1的温度T2，使易挥发液态烃挥发而不使气态反应混合物的组分凝结。第二传热装置把气态反应混合物冷却到低于T2的温度T3，保持流化床所需温度T1。

Description

本发明是关于烯烃在流化床反应器中气相聚合的方法以及实现该方法的设备。
一种或多种烯烃在流化床反应器中进行气相聚合属于公知内容，在流化床反应器中聚合物颗粒在其形成过程中借助于在上升物流中循环的并含有待聚合的一种或多种烯烃的气态反应混合物而保持为流化态。聚合反应一般在齐格勒一纳塔型催化剂或基于铬氧化物的催化剂存在下进行。催化剂可以连续地或间断地给入流化床反应器中，而生成的聚合物也可以连续地或间断地从反应器中排出。在流化床反应器中循环的气态混合物只和催化剂接触有限的时间，一般少于30秒左右。因此只有一部分给入反应器的烯烃能够反应，所以实际上须把气态混合物再循环进入反应器。此外，烯烃的聚合是放热反应，为使流化床保持恒温必须把产生的热排出。
法国专利第1        566        967号公开了一种烯烃在流化床反应器中气相聚合的方法，反应器安装有传热设备，为了冷却流化床而将传热设备设置在流化床内。反应器安装有增稳室，目的是为了减少从反应器顶端离开的气态反应混合物所夹带的小颗粒量。气态混合物可通过循环线路再次给入反应器底部。循环线路包括，在气态混合物的流动方向上依次为，旋风分离器、过滤器、冷却和气/液分离装置，其具体目的是为了液化包含在气态反应混合物中的可凝结的化合物并把它们从该混合物中分离出来、用于循环和重复循环气态反应混合物的压缩机、以及在气态反应混合物根据需要被再次给入反应器之前能够加热或冷却气态反应混合物的热交换器。此外，聚合活化剂，例如有机铝化合物，可以在压缩机与能够加热或冷却的热交换器之间的某一点直接给入循环线路。现已发现，既使使用灰尘分离器也不能非常有效地阻止最细的粒子。这些粒子一般在聚合时活性非常高，因为它们由催化剂和生长着的聚合物粒子的碎屑组成。因此，细粒子能迅速地在热交换器的表面沉积，具体地说，在热交换器的进口和第一部分沉积。它们能继续与烯烃反应，被加热到其熔点并部分地或全部地堵塞交换器。冷却和气/液分离装置安装在压缩机的上游，其主要目的是凝结气态反应混合物中的某些组分。现已发现，冷却和气/液分离装置不能把全部分离出气态混合物中的凝结产物。这就使吸入包含有小滴状液体的气态混合物的压缩机受到过渡磨损。此外，众所周知，气/液分离        装置会大大地增加循环线路中的压力损失从而增加了压缩机的能量消耗。
现在发现了一种烯烃气相聚合的方法，它使用图1所示意地表示的设备，具体地说，该设备包括流化床反应器和用于循环从反应器顶端出来的气态反应混合物的线路。具体地说，循环管线包括压缩机、两台传热装置和易辉发液态烃的供给管路，其安装方式可避免上述缺点。尤其是，从反应器带出的聚合物或催化剂的小粒子不再干扰压缩机和传热装置的操作。业已发现，有待循环的气态反应混合物也可含有易凝结烃而不损坏或干扰设备尤其是压缩机，压缩机的使用寿命大大地延长了。还发现对传热装置的后续清洗作业时间间隔大大地延长了。
本发明是关于含有2-10个碳原子的一种或多种烯烃在流化床反应器中在齐格勒-纳塔型催化剂体系或基于铬氧化物的催化剂存在下进行气相聚合的方法，烯烃可以连续地或间断地给入反应器，聚合物在流化床中在低于其熔点的温度T1下生成，并连续地或间断地从反应器排出，床中的固体粒子借助于包含一种或多种待聚合的烯烃的气态反应混合物而保持流化态，气态反应混合物以上升物流通过反应器，从反应器的顶端离开并通过循环线路返回反应器的底部，循环线路包括，在气态反应混合物的流动方向上依次为，第一传热装置、压缩机和第二传热装置，特征在于：
一种易辉发液态烃或者给入第一传热装置的进口或者在上流并在第一传热装置附近给入循环线路，使得进入第一传热装置的混合物含有呈液态的易挥发烃，
气态反应混合物被第一传热装置冷却到温度T2，T2低于T1并使得该混合物中没有气态组分凝结以及使得易挥发液态烃在第一传热装置挥发，以及
已加入易挥发液态烃的气态反应混合物被第二传热装置冷却到温度T3，T3低于T2并使得流化床的温度保持在要求的温度T1。易挥发液态烃可包含至少一种惰性烃，该烃可选自含有2-7个碳原子的烷烃，尤其是正丁烷、异丁烷、正戊烷、异戊烷和正己烷。易挥发液态烃还可以包含至少一种烯烃，该烯烃可选自含有3-10个碳原子的烯烃或二烯烃，尤其是丙烯、丁-1-烯、己-1-烯、4-甲基戊-1-烯和辛-1-烯。它也可选自二烯烃，尤其是己-1，4-二烯和5-亚乙基-2-降冰片烯。易挥发液态烃也可以由两个或多种这些材料的混合物组成。令人惊奇地发现，液态烯烃在循环线路的一个热点，或者在第一传热装置的上流或者在其实际进口，给入气态反应混合物不会使被夹带粒子的温度突然增加，由于含有催化剂的粒子的活化，温度会上升到其软化点或熔化点，当将高级α-烯烃加入乙烯中时，这种催化剂的活化作用尤为增强。这种活化已公开， 例如在PoLymer        Science        USSR，第22卷，1980，第448-454页。
气态反应混合物首先被第一传热装置冷却到温度T2，T2低于流化床中的聚合温度T1。
只要气态反应混合物的组分不凝结，温度T2可以低为10℃，最好是最低为20℃，但低于T1。而且，温度T2的选择应使得易挥发液态烃在第一传热装置全部挥发。因此，已加入易挥发液态烃的气态反应混合物完全呈气态离开第一传热装置，从而使得压缩机能满意地操作。换言之，选择的温度T2高于在第一传热装置出口流通的气体混合物的露点Tdp，第一传热装置包括气态反应混合物和呈气态的挥发液态烃。更具体地说，选择温度T2应使：
T2＞Tdp+2℃
较好地是，
T2＞Tdp+5℃
此外，气态反应混合物中夹带的小粒子本身被冷却到温度T2，这能阻止它们在压缩机中软化或熔化，由于对气体混合物的压缩，压缩机中的温度一般会上升几度。而且，压缩机中给入的是冷却了的气体混合物，这能大大降低其能耗。
然后，含有呈气态的易挥发液态烃的气态反应混合物被第二传热装置再次冷却到温度T3，T3低于T2。更具体地说，温度T3可以最低为30℃，最好是最低为40℃，低于在流化床中的聚合温度T1。由于气态反应混合物在温度T3再次直接给入流化床反应器的底部，温度T3和T1的差别很大程度上决定了反应器的聚合物生产能力。更具体地说，温度T3可以低于由气态反应混合物和易挥发 液态烃组成的气体混合物的露点。
聚合反应一般在压力0.5-5MPa和温度T1下进行，温度T1低于聚合物的熔点，较好地是低于聚合物的软化点或熔结点，具体地讲温度T1在0℃-150℃之间，最好是在30℃-120℃间。通过流化床聚合反应器并重复循环的气态反应混合物除了含有一种或多种要聚合的烯烃外，还可含有二烯烃、氢和一种选自，例如氮、甲烷、乙烷、丙烷、丁烷、异丁烷、戊烷、异戊烷和己烷的惰性气体。它在上升物流中通过流化床，流化速度一般为最小流化速度的2-8倍，尤其是0.3-0.8m/S，最好是0.4-0.7m/S。流化床包括在形成过程中的聚合物粒子，其重量平均直径为0.3-2mm。
本发明的方法特别适用于在一种高活性催化剂或催化剂体系存在下在气相中借助于乙烯或丙烯的聚合或借助于两种或多种烯烃如乙烯、丙烯、丁-1-烯、己-1-烯和4-甲基戊-1-烯的混合物的共聚制造聚烯烃。催化剂体系可以是齐格勒-纳塔型并且含有一种基本上由镁、齿素如氯或溴、以及至少一种过渡金属元素如钛、钒或锆的原子组成的固体催化剂和一种基于属于元素周期表Ⅱ或Ⅲ族的金属如铝或锌的有机金属化合物的助催化剂。还可能把基于铬氧化物的高活性催化剂与基于高熔点氧化物，比如二氧化硅、氧化铝或硅酸铝的粒状载体联合使用，粒状载体在最低温度250℃和最高温度为粒状载体开始烧结的温度，最好是在350℃-1000℃温度下经热处理而活化。
高活性的催化剂或催化剂体系可以照此直接使用或者以预聚物的形式使用。这种预聚物的转化一般靠使催化剂或催化剂体系与一种或多种烯烃相互接触来完成，其用量应使得每克预聚物含0.002-10毫摩尔过渡金属或铬。这些成份也可以在属于元素周期表Ⅱ和Ⅲ族金属族的有机金属化合物的存在下接触，其用量应使得该有机金属化合物中的金属量与过渡金属或铬的原子比为0.1-50，最好是0.5-20。高活性的催化剂或催化剂体系可以直接地或经预聚合步骤之后被加入到流化床反应器中。
本发明还涉及一种或多种含有2-8个碳原子的烯烃气相聚合的设备，该设备包括流化床反应器和配置有压缩机的循环线路，借助于压缩机，离开反应器顶端的包含一种或多种待聚合烯烃的气态反应混合物返回该反应器的底部，循环线路装配有安装在流化床反应器顶端与压缩机吸入端之间的第一传热装置和安装在压缩机排出端与反应器底部之间的第二传热装置，特征在于导入易挥发液态烃的管路通向第一传热装置的进口或者通向循环线路上流以及第一传热装置进口附近。
因此该设备包括可安装有增稳室的流化床聚合反应器、以及用于循环气态反应混合物的线路，该线路在外部将反应器的顶端和底部相连，并且在气态反应混合物的流动方向上依次配置导入易挥发液态烃管路的进口、第一传热装置、压缩机和第二传热装置。
按照本发明，令人惊奇地发现，为了使传热装置和压缩机能够令人满意地工作，必须使用两个传热装置，使二者分别位于压缩机的两端，还必须有一导入易挥发液态烃的管路，该管路直接与第一传热装置的进口连接或者是通向位于流化床反应器顶端与第一传热装置之间并且靠近第一传热装置进口，尤其是在离该进口的距离能使易挥发液态烃在该进口部分地呈液态的某一循环线路部位。更具体地说，导入管路在循环线路上的开口离第一传热装置进口的距离应使得加入气态反应混合物的易挥发液态烃的平均停留时间少于1秒种，最好是少于0.5秒种。然后，当易挥发液态烃穿过第一传热装置的实际热交换区，更具体地说是该区的第一部分时，就会沿若其长度方向蒸发。这样它就完全地与气态反应混合物混合，并呈完全气态均相混合物的形式离开第一传热装置。
已注意到，如果导入易挥发液态烃的管路在距第一传热装置进口太远的地方通向循环线路，易挥发液态烃在进入第一传热装置之前就会完全挥发。在该传热装置的换热表面上有小粒子沉积，这样使之迅速地失去其大部分换热能力并且甚至由于小聚合物粒子的熔化而将其堵塞。易挥发液态烃导入循环线路的部位与第一传热装置进口之间的距离明显地取决于导入的易挥发液态烃的性质、以及组成、温度、压力和气态反应混合物在流化床反应器顶端与第一传热装置之间的循环管线内流通的速度。具体地讲，该距离越短，易挥发液态烃挥发越多。估计该距离可以是，例如，最多15至20m，最好是10至15m。
第一传热装置的主要作用是把气态反应混合物冷却到气态反应混合物中没有组分凝结并且易挥发液态烃完全挥发的温度，这同样是至关重要的。第一传热装置不包括能够从气体中分离液体的装置。换言之，已加入易挥发液态烃的气态反应混合物完全呈气态离开第一传热装置并且不干扰压缩机是很重要的。令人十分惊奇地发现，第一传热装置达到了一个没有气体在该传热装置内部凝结、在该传热装置的全部交换表面没有靠凝结形成的液体流过并且不用清洗的洁净状态。
在循环线路中两个传热设备之间安装压缩机的目的是使气态反应混合物在循环线路内流通并使该混合物重复循环进入流化床反应器，该混合物构成了流化气体并在该反应器内部呈气流上升。人们发现，由于到达压缩机吸入端的气态混合物不含有任何呈小滴状的液体以及被第一传热装置中的气态反应混合物带入循环线路并冷却的小粒子在压缩机内不太可能熔化，压缩机的磨损大大地下降了。还发现，由于到达压缩机吸入端的气态反应混合物已经在第一传热装置内预先冷却，压缩机的能耗大大地下降了。此外，循环线路可以包括灰尘分离器，比如旋风分离器或过滤器，流化床反应器可以包含增稳区。然而，这些设备不是必需的。
第二传热装置的主要作用是把气态反应混合物冷却到要求的温度以便使流化床反应器中聚合物的生产在要求的条件下进行。特别是，可以操作该第二传热装置使气态反应混合物的一种或多种组分和/或易挥发液态烃凝结。如果合适的话，可将能够从气态混合物中分离液体的装置以及用于把该液体再循环进入流化床反应器的装置与第二传热装置结合起来。
本发明使用的传热装置可包括已知类型的换热器，它可以是板式换热器，或最好是管式换热器，包括进口区，也称为进口箱、一般呈圆柱形的室，包括均匀地隔开该室内部的板或管、以及出口区，也称为出口箱。具体来说，导入易挥发液态烃的管路可以导向第一传热装置的进口区。使用的换热器设计和/或操作以除去由聚合反应产生的大量的热。
还观察到，本发明的设备可以满意地用来制备许多种聚烯烃。更具体地说，第一与第二传热装置的换热能力比在20/80和70/30之间，最好是在30/70和60/40之间。在这些条件下，能够制造，例如，高密度聚乙烯或者乙烯与至少一种含有3-10个碳原子的α-烯烃的共聚物，密度小于0.930。
流化床反应器一般包括安装有增稳室的竖直圆柱体，增稳室的横截面比圆柱体的大。反应器在其底部可包括流化格栅，该格栅把位于其下部的反应器空间定域为在循环线路内流通的气态反应混合物的供给室。
由于换热装置能保持清洁并且能够长期地高效运行，因此本方法和设备具有很大的优越性。而且，因为要循环的气态反应混合物不含小液滴并且被气态反应混合物夹带的小粒子不能在压缩机的各个部件上熔化和沉积，所以压缩机的磨损降低了。在令人生厌地发生循环线路中压降增大的条件下便可体现这些显著的优点。此外，压缩机的能耗可获得显著下降。
图1示意地表示了烯烃气相聚合的设备。该设备包括流化床反应器（1），该反应器由安装有增稳室（3）的竖直圆柱体（2）组成，在圆柱体（2）的底部配置有流化格栅（4）。该设备还包括用于循环气态混合物的线路（9），线路（9）依次包括：用于将易挥发液态烃从贮存室经（10）管路（5）导入的进口、带有进口（17）的第一管式热交换器（6）、压缩机（7）和第二管式热交换器（8）。循环线路中的各种部件，以及流化床反应器（1）用管路（9）、（11）、（12）和（13）联接在一起。管路（13）把热交换器（8）联接于反应器（1）的底部，流化格栅（4）的下部。管路（14）能够把催化剂或催化剂体系加入反应器（1）。制得的聚烯烃粒子经管路（15）从反应器（1）中排出。与管路（13）连接的管路（16）是气态反应混合物组分的供给管路，能够使得该气态反应混合物的组成和压力保持恒定。
本发明用下列实施例说明。
实施例1。
本方法在由图1所示意的设备中进行，但是循环线路（9）在反应器（1）的顶端与管路（5）和管路（9）的联接点之间安装有旋风分离器。流化床反应器（1），安装有流化格栅（4），基本上由直径4.5m的圆柱体（2）组成，并安装有增稳室（3）。反应器的总高度大约30m。反应器（1）包含保持在90℃的流化床，并包括呈重量平均直径为0.7mm的粒子形式的在形成过程中的高密度的聚乙烯（密度0.96）粉末50T。把由重量平均直径为0.25mm的粒子组成的乙烯预聚物给入反应器（1），上述预聚物用在法国专利第2        405        961号实施例1中所描述的齐格勒-纳塔型催化剂体系制备，该催化剂体系包括基于钛、镁和氯的固体催化剂，以及包含三-正-辛基-铝的助催化剂，其量应使得原子比Al/Ti等于1并且使预聚物含有35克聚乙烯/毫摩尔钛。
含有（体积比）43%乙烯、33%氢、16%氮、3%异戊烷和5%乙烷的气态反应混合物在总压力2.3MPa下以速度0.5m/S上升通过流化床。气态反应混合物在温度90℃下从反应器（1）的顶部离开。在室温（20℃）下用于导入液态异戊烷的管路（5）在第一传热装置（6）的上流并离其进口3m的地方通与循环线路（9）连接。气态反应混合物中的异戊烷在第一管式换热器（6）的进口（17）之前的平均停留时间少于0.2秒。异戊烷进入第一管式换热器（6）时部分呈液态。液态异戊烷在流速100Kg/h下给入。气态反应混合物在通过有水作为冷却流体给入的第一传热装置（6）之后被冷却到47℃。异戊烷离开第一传热装置（6）后完全蒸发。气态反应混合物被第一次冷却之后用压缩机（7） 压缩。然后，气态反应混合物被有水作为冷却流体给入的第二传热装置（8）再次冷却到33℃。现在冷却到33℃的气态反应混合物最终通过管（13）循环进入反应器（1）位于流化格栅下部的底部。
第一和第二传热装置的换热表面之比为50/50。此外，这两个传热装置的操作条件应使得第一和第二传热装置的换热能力之比为70/30。
在这些条件下，大约在一年间，流化床反应器（1）可连续操作生产大约13.5T/h的高密度聚乙烯（密度0.96）而不会使压缩机（7）显著过早磨损也不会使传热装置（6）和（8）发生任何显著堵塞现象。
实施例2.
本方法在实施例1中描述的装置中进行。反应器（1）包含保持在82℃的流化床并包含呈重量平均直径0.7mm的粒子形式的在形成过程中的直链低密度的聚乙烯（密度0.92）粉末50T。给入该反应器（1）的预聚物与实施例1中使用的相同。含有（体积比）37%乙烯、15%丁-1-烯、5%氢、38%氮和5%乙烷的气态反应混合物在压力2MPa以速度0.5m/s上升通过流化床。气态反应混合物在温度82℃下从反应器（1）的顶部离开。导入在室温（20℃）下的液态丁-1-烯的管路在第一传热装置（6）的上流并离其进口3m的地方与线路（9）连接。气态反应混合物中的丁-1-烯在第一管式换热器（6）的进口（17）之前的平均停留时间少于0.2秒。丁-1-烯穿过第一管式换热器（6）时部分呈液态。液态丁-1-烯在流速1100Kg/h下给入。气态反应混合物在第一传热装置中冷却到59℃。气态反应混合物被第一次冷却之后用压缩机（7）压缩。它然后再次被第二传热装置冷却到42℃。这两个传热装置的操作条件应使得第一和第二传热装置的换热能力之比为50/50。现在冷却到42℃的气态反应混合物最终通过管（13）循环进入反应器（1）位于流化格栅下部的底部。
在这些条件下，大约在一年期间，流化床反应器（1）可连续操作生产大约12.5T/h的直链低密度聚乙烯（密度0.92）而不会使压缩机（7）显著过早磨损也不会使传热装置（6）和（8）发生任何显著堵塞现象。

Claims (5)

1、一种含有2-10个碳原子的一种或多种链烯在流化床反应器中在齐格勒一纳塔型催化剂体系或基于铬氧化物的催化剂存在下的气相聚合的方法，链烯可以连续地或间断地给入反应器，聚合物在流化床中在低于其熔点的温度下生成，并连续地或间断地从反应器排出，床中的固体粒子借助于包含一种或多种要被聚合的链烯的气态反应混合物而保持为流化态，气态反应混合物以上升流通过反应器，从反应器的顶端离开并通过循环线路返回反应器的底部，循环线路包括，在气态反应混合物的流动方向上依次为，第一传热装置、压缩机和第二传热装置，特征在于：
-一种易挥发液态烃或者给入第一传热装置的进口或者在上流并在第一传热装置附近给入循环线路，使得进入第一传热装置的混合物含有呈液态的易挥发烃，
-气态反应混合物被第一传热装置冷却到温度T2，T2低于T1并使得该混合物中没有气态组分凝结以及使得易挥发液态烃在第一传热装置挥发，以及
-已加入易挥发液态烃的气态反应混合物被第二传热装置冷却到温度T3，T3低于T2并使得流化床的温度保持在要求的温度T1。
2、权利要求1的方法，特征在于易挥发液态烃包含至少一种惰性烷烃、或链烯、或这些产品的混合物。
3、权利要求2的方法，特征在于惰性烷烃为选自含有2-7个碳原子的烷烃。
4、权利要求2的方法，特征在于链烯为选自含有3-10个碳原子的链烯或二烯属烃。
5、用于一种或多种含有2-10个碳原子的链烯气相聚合的设备，该设备包括流化床反应器（1）和配置有压缩机（7）的循环线路，借助于压缩机（7），离开反应器（1）顶端的包含一种或多种要聚合链烯的气态反应混合物返回该反应器的底部，循环线路配有安装在流化床反应器（1）的顶端与压缩机（7）的吸入端之间的第一传热装置（6）和安装在压缩机（7）的排出端与反应器（1）底部之间的第二传热装置（8），特征在于导入易挥发液态烃的管路（5）开向第一传热装置（6）的进口（17）或者在上流并在第一传热装置（6）附返开向循环线路（9）。
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