CN1036053C - 流化床反应器中烯烃聚合方法 - Google Patents

流化床反应器中烯烃聚合方法 Download PDF

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CN1036053C
CN1036053C CN94192687A CN94192687A CN1036053C CN 1036053 C CN1036053 C CN 1036053C CN 94192687 A CN94192687 A CN 94192687A CN 94192687 A CN94192687 A CN 94192687A CN 1036053 C CN1036053 C CN 1036053C
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J·科斯基宁
H·安德茨焦
J·塔卡凯霍
K·萨兰蒂拉
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Borealis Polymers Oy
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/38—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
    • B01J8/382—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it with a rotatable device only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/40—Mixers using gas or liquid agitation, e.g. with air supply tubes
    • B01F33/402—Mixers using gas or liquid agitation, e.g. with air supply tubes comprising supplementary stirring elements
    • B01F33/4021—Mixers using gas or liquid agitation, e.g. with air supply tubes comprising supplementary stirring elements the gas being introduced through the shaft of the stirring element
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1872—Details of the fluidised bed reactor
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S526/00—Synthetic resins or natural rubbers -- part of the class 520 series
    • Y10S526/901—Monomer polymerized in vapor state in presence of transition metal containing catalyst

Abstract

本发明涉及一种在流化床聚合反应器中烯烃聚合的方法，其中，由含聚合催化剂的聚合粒子形成的流化床中烯烃单体进行聚合。通过将至少一种含可聚合单体和必要时的氢、惰性气体或稀释气体的循环气流引入反应器(10)中使流化床维持在流化态。利用连结在必要的垂直驱动轴(19、20)的至少一种搅拌工具搅拌流化床。按照本发明，至少一部分导入反应器(10)的气流是通过所说轴(20)和所说的搅拌工具(21、22)内部的气流通道进入反应器的。

Description

流化床反应器中烯烃聚合方法
本发明涉及在一适用于烯烃气相聚合并装有搅拌器的流化床反应器中进行烯烃聚合和共聚的方法。
通常烯烃气相聚合是在流化床中进行。这时，聚合反应是在聚合过程形成的粒子组成的床中进行。聚合反应产生的热量是将含要聚合的单体以及还常含氢、惰性稀释剂或惰性气体的循环气经反应器和流化床循环而除去的。将循环气体在置于反应器外的冷却器中冷却，然后送回反应器的下部。经反应器上升的循环气体保持流化床呈流化态，并维持流化床的有效搅拌。反应器越大，在整个流化床体积中保持均匀的流化和搅拌越难。事实上已经发现，特别是在反应区的下角可能存在不足的流化和搅拌，这会使传热不良。传热不良又会引起局部过热，这样，聚合物粒子的温度达到软化点，从而使附聚粘块增长，然后粘到反应器壁上。当这些聚合物的附聚块从反应器壁剥落下来，会影响产品质量。
通过使用可增强搅拌作用的各种类型的机械搅拌器元件，来完善反应器，用以克服上述的流化床反应器的问题。所用的典型的搅拌器装置是一种锚状搅拌器，搅拌器上有一对或多个支持臂连于垂直驱动轴上，支持臂端载有垂直排列的与垂直驱动轴等距离的搅拌器叶片。这种搅拌器的缺点是，由搅拌器施加的离心力驱动的聚合物粒子常朝向反应器的内壁运行。结果聚合物附聚块开始粘于反应器壁。如果搅拌器臂相当短，在反应器中心区会同时产生旋涡区，这样，从反应器下部导入的循环气体优选地追向旋涡区。已经提出解决这个问题的方法是使搅拌器带有许多长度不同的臂。
美国专利4,366,123公开了一种锚状搅拌器，其设计的主搅拌器臂长到使连于臂端的搅拌器叶片运动起来很接近反应器垂直内臂。此外，此种搅拌器还有短的搅拌器臂，这些短臂的搅拌器叶片运动时接近驱动轴。还有，至少主搅拌器叶片具有三角形横截面。这种设计的目的是达到足够的搅拌效率，避免由于搅拌器转动发生的振动。
美国专利4,188,132公开了一种流化床反应器的螺旋搅拌器。只有螺旋搅拌器的下部连于驱动轴的末端，其下端高于第一圈螺旋的长度处还装有分离的分配器螺旋元件。作为冷却介质的新鲜气体通过驱动轴的入口通道进入反应器。分配器螺旋元件的目的是反转进入反应器的气流方向，从而防止在反应器底生成聚合物附聚块。
然而，上述美国专利未能克服在反应器角落和内壁的流化不足和聚合物粒粘附于反应器内壁的问题，这些问题一般发生在大直径反应器中。本发明专门涉及消除这些问题。
本发明的方法既能达到在临界区有效搅拌作用和改进流化，同时防止聚合物粒子粘附于反应器的内表面。因此，本发明涉及一种在流化床聚合反应器中聚合烯烃的方法，其中，烯烃单体在由含聚合催化剂的聚合粒子形成的流化床中聚合。所说的流化床通过在反应器导入至少一利含可聚合单体以及必要时的氢、惰性气体或稀释气体的循环气流保持流化态，并且通过至少一种连结于基本垂直驱动轴的搅拌工具搅拌该流化床。此工具适用于搅拌流化床。本发明方法的特征是，至少一部分导入反应器的气流通过提供给所说驱动轴和所说搅拌工具内部的至少一种流动通道进入反应器。
因此，在本发明的方法中，使用了一种流动通道。经过此通道，气体介质可以高速直接进入反应器中通常流化气流最弱的区域。在这种方式中，利用一种冲洗作用，大幅度降低聚合物粒子附聚和粘附于反应器底部的下部边缘和内壁。
按照本发明的一个优选的具体实施方案，搅拌器驱动轴，连接于所说的混合器驱动轴上的搅拌器臂以及连接于所说的臂上的搅拌器叶片，都是中空的并形成连续的流动通道，通过这些通道，搅拌气体能够经过搅拌器叶片的孔导入反应器。由这些孔排出的气体冲洗反应器壁并改善了流化和床中粒子的搅拌作用，同时使否则容易出现过热的区域得到了冷却。
搅拌器叶片最好(尽管不一定必须)使连于搅拌器臂(此臂与搅拌器驱动轴相连的桨)向上垂直伸长。搅拌器臂最好(尽管不一定必须)水平伸长具有可自由选择的横截面的臂。然而，一般来说，设计臂的横截面要使之阻搅动最低。搅拌器臂的长度应设计得使连结于搅拌器臂末端的搅拌器叶片尽可能接近伸向流化作用本来就最弱的反应器容器的内壁。
按照本发明的一个具体实施方案，搅拌器可以包括至少一种带搅拌叶片的辅助臂，辅助臂的长度可以比主搅拌器臂短。辅助臂和连于其上的搅拌叶片可以是中空的，从而可形成流动通道，以便将搅拌气体导入反应器中。一般来说，一对辅助臂足以达到满意的搅拌效果。
通过搅拌器进入的气体介质可以是通常进入反应器的任何气体。因此，混合或分别使用单体或共聚单体原料、氢、惰性气体或惰性气体稀释剂作为搅拌气体可以达到预期的作用。通过搅拌器的搅拌气流也可包含经过反应器的来自循环气流的副气流。然而，循环气中可能含有经反应器顶逸出的聚合物细粒，穿过搅拌器的搅拌气体最好是由例如惰性介质、单体或其混合物形成的无催化剂和无聚合物的气体。
穿过搅拌器的气体介质的比例可在0.1-30重量％之间变化。然而，足以达到满意冲洗效果的搅拌气体的实际比例可以选择大大低于上面给出的上限，这样，搅拌气体用量一般为导入反应器气流总量的0.1-10重量％，优选为0.3-5重量％。如果是工业规模的流化床反应器，则上述比例相当于每小时数吨搅拌气流。
装有本发明的搅拌器的聚合反应器可以用于任何可聚合单体的气相流化床聚合或共聚。适宜的单体有乙烯、丙烯、丁烯、戊烯、己烯等烯烃和其它单体。
下面参考附图来说明本发明。
图1装有为实施例本发明方法设计的搅拌器的流化床反应器的底部截面侧视图；
图2为本发明的搅拌器叶片的横截面图。
在图1中，数字10表示流化床反应器。反应器有一圆筒形外壳11。带孔的气体分配板12将反应器10分成循环气体的横切部分13，和流化床部分14。反应器10的底部包括两个同心锥形转动面，内锥形壁面15向上逐渐减少，而外锥形壁面16是向下逐渐减少。锥形面15和16由光滑的环形部分17将两者互相连接，而17就成为反应器容器底的最低部分。由内锥面15形成的壁部分在其上部边缘形成水平的支持平面24。
循环气流通过至少一循环气管道(未示出)进入横切部分13，然后经气体分布板12进入流化床部分14。
按照本发明，搅拌器包含一电动马达18，马达转动垂直连接轴19，后者伸到反应器中作为搅拌器驱动轴20，轴上连结搅拌臂21，臂末端连结着搅拌叶片22。带有转动搅拌器驱动轴20的轴承的电动马达18最好置于由反应器底的内锥形壁面15形成的钟形深处之内或之下。轴19最好利用经过水平辅助壁23的旋转密封起作用，这样，辅助壁23、内锥形壁面15和水平支持平面24一起包围了为搅拌气体进入的横切室25。通过在辅助壁23和水平支持平面24的轴承上安装轴19和搅拌器驱动轴20，为这些轴提供了坚固的支撑。同样道理，气体分配板12可支撑在水平支持平面24上。
本发明方法利用的搅拌器最好有一中空连结轴20，气态或液态物质可经其通过。同样，搅拌器臂21也制成中空的，它的中空内通道与混合器驱动轴20的中空内通道互通。而且，搅拌器叶片22也是中空的，其中空内腔与搅拌器臂21的中空通道相连通。因而，从搅拌器驱动轴20到搅拌器叶片22形成连续的通道。
气体介质最好通过室25进入搅拌器。此气体首先通过管道26进入室25，由此在必要时经过滤净器27进入中空搅拌器驱动轴20。泵入搅拌器中的气体可含来自进入反应器10底部的循环气流的副气流。搅拌气体最好是不含催化剂和聚合物的新鲜气体，如单体、共聚单体、氢或惰性介质。
在图2中，在搅拌器叶片22上装有气流孔28，搅拌气体可经过气流孔28进入反应器10。气流孔28可含有如穿孔，可分布在搅拌器叶片22的整个长度上，或仅在其中一部分上。
上述讨论的本发明的方法适于结合利用水平搅拌器臂并具有垂直排列的搅拌器叶片。搅拌器同样可含螺旋形中空搅拌器元件，其中，螺旋的外边缘有供排出搅拌气体的穿孔。

Claims (4)

1.一种在流化床聚合反应器中聚合烯烃的方法，其中，烯烃单体在由含聚合催化剂的聚合粒子形成的流化床中进行聚合，通过在反应器(10)中导入至少一种含可聚合的单体和必要时的氢、惰性气体或稀释气体维持流化床在流化态，利用连结到基本垂直的驱动轴(19、20)并适于搅拌流化床的至少一种搅拌工具(21、22)搅拌该流化床，其特征在于，至少一部分气流通过至少一种所说轴(20)和所说搅拌工具(21，22)内部的气流通道导入反应器(10)，靠近于该反应器内壁，并扩展到接近于反应器壁。
2.权利要求1的方法，其特征在于，所说的一部分气流通过至少一个水平搅拌器臂(21)和连结于其末端的搅拌器叶片(22)进入反应器(10)中，所说的叶片(22)接近于反应器壁(11)。
3.权利要求1-2的方法，其特征在于，所说的一部分气流通过3在所说叶片(22)的排出孔(28)进入反应器(10)。
4.权利要求1所述的方法，其特征在于，所说的搅拌工具包括连结于所说轴(19)的螺旋形的搅拌器元件，在搅拌中所说的元件有所说的气流通道，并且在末端有孔将气体排到反应器(10)中。
CN94192687A 1993-07-05 1994-07-01 流化床反应器中烯烃聚合方法 Expired - Fee Related CN1036053C (zh)

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EP0707513A1 (en) 1996-04-24
CA2166486A1 (en) 1995-01-19
NO960035D0 (no) 1996-01-04
CN1126447A (zh) 1996-07-10
BR9406922A (pt) 1996-07-30

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