CN1166444C - 浆液聚合中的挥发性物质的连续除去 - Google Patents

浆液聚合中的挥发性物质的连续除去 Download PDF

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CN1166444C
CN1166444C CNB998040207A CN99804020A CN1166444C CN 1166444 C CN1166444 C CN 1166444C CN B998040207 A CNB998040207 A CN B998040207A CN 99804020 A CN99804020 A CN 99804020A CN 1166444 C CN1166444 C CN 1166444C
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J·A·肯德里克
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Abstract

公开了一种从含有稀释剂、未反应单体和聚合物固体的聚合流出物中连续分离含有稀释剂和未反应单体的液体介质的方法/设备,包括,使聚合物流出物通过卸料阀和输送管从浆液反应器连续卸料到第一个中等压力的闪蒸釜,它有由沿水平方向的倾斜角等于或大于聚合物固体/浆液的滑动角的基本上直立侧面确定的锥形底,还有具有这样的长度(l)和直径(d)的出口密封室,以致在出口密封室中维持所希望的浓缩聚合物固体/浆液的体积,以便形成压力封,同时从出口密封室通过密封室出口渐缩管,将浓缩的聚合物固体/浆液连续卸料到处于较低压力的第二闪蒸釜中,该密封室出口渐缩管的倾斜侧面由沿水平方向的倾斜角等于或大于从中除去约50至100%惰性稀释剂以后留下的聚合物固体的滑动角的基本上直立侧面确定。

Description

浆液聚合中的挥发性物质的连续除去
发明范围
本发明涉及一种从含有惰性稀释剂和未反应单体的液体介质中连续分离聚合物固体的设备。具体地说,本发明涉及这样一种从液体介质中连续分离聚合物固体、干燥聚合物和回收稀释剂和未反应单体的设备,它减少了为稀释剂蒸汽冷凝成稀释剂液体以便再用于聚合过程所需的压缩。在另一方面,本发明涉及一种从液体介质中连续分离聚合物固体的方法。具体地说,本发明涉及一种从液体介质中连续分离聚合物固体、干燥聚合物和回收稀释剂和未反应的单体以便再用于聚合过程的方法。
发明背景
在许多生产聚合物的聚合方法中,生成这样一种聚合流出物,它为一种颗粒聚合物固体悬浮在液体介质(通常为反应稀释剂和未反应的单体)中的浆液。这样的方法的一个典型的例子在Hogan和Bank的US2285721中公开,其公开内容在这里作为参考并入。虽然在Hogan的专利中公开的聚合方法使用含有氧化铬和载体的催化剂,但是本发明可适用于任何一种生产含有颗粒聚合物固体悬浮在含稀释剂和未反应单体的液体介质中的浆液的流出物的方法。这样的反应方法包括那些在本专业中称为颗粒形式聚合的方法。
在大多数工业规模的操作中,希望以这样一种方式来分离聚合物和含有惰性稀释剂和未反应单体的液体介质,以致液体介质不受到污染,这样液体介质可循环回聚合段,只需要很少的纯化,如果有的话。迄今已使用的一种特别有利的技术是Scoggin等在US 3152872中公开的技术,更具体地说是结合该专利图2说明的实施方案。在这样的方法中,反应稀释剂、溶解的单体和催化剂在环管反应器中循环,在环管反应器中,聚合反应的压力为约100至700磅/平方英寸(绝)。生产的固体聚合物也在反应器中循环。聚合物和液体介质的浆液收集在浆液环管反应器的一个或多具沉降腿中,浆液定期从沉降腿排料到闪蒸室,闪蒸室中混合物突然降到低压例如约20磅/平方英寸(绝)。虽然闪蒸使液体介质基本上完全从聚合物中除去,但是为了使回收的稀释剂冷凝成适合作为液体稀释剂循环到聚合段的液体形式,必需再次压缩已汽化的聚合稀释剂(例如异丁烷)。压缩设备的费用以及这一操作所需的公用工程费用常常占生产聚合物所涉及的费用的重要部分。
一些聚合方法在液体稀释剂循环回反应器以前先蒸馏液化的稀释剂。蒸馏的目的是除去单体和轻质杂质。然后将蒸馏过的液体稀释剂通过一处理器床层,以便除去催化剂的毒物,然后再回到反应器。蒸馏和处理的设备和公用工程费用可为生产聚合物费用的重要部分。
在一工业规模的操作中,希望用最少的费用使稀释剂蒸汽液化。所以,所使用的一个这样的技术在Hanson和Sherk的US 4424341中公开,其中在这样的温度和压力下用中等压力闪蒸步骤除去主要部分的稀释剂,以致这一经闪蒸的稀释剂部分可用热交换代替较为昂贵的压缩步骤来液化。
发明概述
本发明涉及一种从含有惰性稀释剂和未反应单体的液体介质中连续分离聚合物固体的设备。在另一方面,本发明涉及一种从液体介质中连续分离聚合物固体、干燥聚合物和回收稀释剂和未反应单体的设备,它减少了为稀释剂蒸汽冷凝成稀释剂液体以便再用于聚合过程所需的压缩。在另一方面,本发明涉及一种从液体介质中连续分离聚合物固体的方法。在另一方面,本发明涉及一种从液体介质中连续分离聚合物固体、干燥聚合物和回收惰性稀释剂和未反应的单体以便再用于聚合过程的方法。
根据本发明,提供了一种从一种聚合流出物中连续回收聚合物固体的设备,所述聚合物固体是以在含有惰性稀释剂和未反应单体的液体介质中的浆液形式存在。该设备包括在浆液反应器上的卸料阀,浆液反应器的例子包括浆液环管反应器和搅拌釜浆液反应器,卸料阀用于将一部分浆液反应器物料连续卸料到第一输送管;第一闪蒸釜,其底面由水平方向倾斜角等于或大于浆液/聚合物固体的滑动角的基本上直的侧面确定,其中第一闪蒸釜的压力和聚合流出物的温度是这样的,以致约50至约100%的液体介质将汽化以及所述的蒸汽中的稀释剂组分可不经压缩而通过与温度为约65至约135°F的流体热交换而冷凝;与第一闪蒸釜相通的第一闪蒸釜出口密封室,它有这样的长度(1)和直径(d),以致可使浓缩的聚合物固体/浆液的料面积累并在所述的第一闪蒸釜出口密封室中形成压力封;为将浓缩的聚合物固体/浆液活塞流卸料到第二输送管的密封室出口渐缩管,第二输送管将浓缩的聚合物固体/浆液送到第二闪蒸釜,其中所述的第二闪蒸釜的压力和浓缩的聚合物固体/浆液的温度是这样的,以致基本上所有残留的惰性稀释剂和/或未反应的单体将汽化并通过压缩和热交换冷凝作为釜顶产物除去,而聚合物固体从所述的第二闪蒸釜的釜底排出,以便另作加工或贮存。
本发明还提供这样一种方法:通过卸料阀从浆液反应器中连续除去聚合流出物流;在聚合流出物通过所述的第一输送管转移的过程中提高聚合物流出物的热含量,达到聚合物熔点以下的温度,同时将聚合物流出物连续送到第一闪蒸釜,后者有沿水平方向的倾斜角等于或大于浓缩的聚合物固体/浆液的滑动角的基本上直的侧面确定的底;在所述的第一闪蒸釜中约50至约100%的液体介质连续汽化,得到处于这样的温度和压力下的浓缩的聚合物固体/浆液和蒸汽物流,以致所述的蒸汽中的惰性稀释剂物料可不经压缩而通过与温度为约65至约135°F的流体换热而冷凝;将浓缩的聚合物固体/浆液从所述的第一闪蒸釜连续卸料进入有这样的长度(l)和直径(d)的第一闪蒸釜出口密封室,以致连续维持这样一浓缩聚合物固体/浆液的体积,以便在所述的第一闪蒸釜出口密封室中形成压力封;浓缩的聚合物固体/浆液通过沿水平方向的倾斜角等于或大于大约50至100%惰性稀释剂从中除去后留下的聚合物固体的滑动角的基本上直立的侧面限定的密封室出口渐缩管从所述的第一闪蒸釜中连续排出;浓缩的聚合物固体/浆液的连续活塞流通过所述的密封室出口渐缩管从所述的第一闪蒸釜出口密封室送到第二输送管,它将所述的浓缩聚合物固体/浆液的连续活塞流送到第二闪蒸釜;以及在低于所述的第一闪蒸釜的压力下操作的第二闪蒸釜中使基本上所有残留的惰性稀释剂和/或未反应的单体连续汽化;从所述的第二闪蒸釜中汽化的惰性稀释剂和/或未反应的单体通过压缩和热交换冷凝;以及从所述的第二闪蒸釜中连续排出基本上干燥的聚合物浆液,用于进一步加工或贮存。
本发明的一个目的是提供这样一种设备和方法:聚合物固体的连续两段闪蒸干燥,随后通过点卸料阀,从浆液反应器中连续除去含有聚合物固体和含有惰性稀释剂和未反应单体的液体介质的聚合物流出物;在第一闪蒸釜出口密封室中控制这样一连续固体料面,以便在密封室中提供一压力封,它使所述的第一闪蒸釜能在大大高于所述的第二闪蒸釜的压力下操作,而聚合物固体通过密封室出口渐缩管连续排放到第二输送管,进而到第二闪蒸釜,它消除了在第一闪蒸釜中的堵塞并通过热交换而不是压缩使约50至约100%惰性稀释剂蒸汽连续液化。
本发明的另一目的是取消在浆液反应器上的沉降腿,从而消除了由定期排放沉降腿中的物料所引起的浆液反应器中断续的高压脉冲。本发明的另一目的是通过消除在沉降腿中堵塞的可能性来提高安全性。
本发明的另一目的是消除卸料阀下游设备中的堵塞。在聚合反应器的沉降腿中,聚合继续进行,反应热使液体介质进一步加热,有可能使聚合物固体溶解或熔融在一起。当沉降腿中的物料排出卸料阀时,压力降引起一些液体介质突然汽化,它使剩余的液体介质冷却,使溶解的聚合物沉积,它倾向于堵塞下游设备。本发明不需要沉降腿,它还通过避免聚合物固体最初的溶解或熔融消除了下游设备堵塞的可能性。
本发明的另一目的是通过提高乙烯在液体介质中的浓度,例如在反应器出口乙烯在液体介质中的浓度大于或等于4%(重量)来提高反应器的生产率。由于在沉降腿内加速的反应引起的下游设备堵塞的趋势增加,所以沉降腿限制了乙烯的浓度。连续的聚合流出物浆液流使乙烯的浓度仅受反应器中液体介质的乙烯溶解度的限制,从而使聚合的比反应速率和反应器的生产率提高。
从以下的描述和图1、图2中,本发明的其他方面、目的和优点是显而易见的。
所要求的设备和方法比现有技术有以下几个优点:(1)从液化的聚合流出物的卸料点通过卸料阀、第一闪蒸釜、密封室、密封室出口渐缩管到第二闪蒸釜,浆液反应器的物料可连续加工,(2)大大提高乙烯在液体介质中的浓度,从而使反应器的生产率提高,以及(3)通过减少对压缩和/或蒸馏汽-液流出物的需要使能耗下降。可减小循环压缩机和其他设备的尺寸或取消它们。
附图简介
根据本发明,图1和2为说明从稀释剂和未反应的单体中连续分离聚合物固体的设备的示意图。
发明详述
本发明适用于任何一种含有聚合物固体浆液和含有惰性稀释剂和未反应单体的液体介质的混合物,包括由烯烃聚合得到的浆液。通常用于这样的反应的烯烃单体为每一分子有2至8个碳原子的1-烯烃。典型的例子包括乙烯、丙烯、丁烯、戊烯、己烯和辛烯。
用于这样的烯烃聚合的典型稀释剂包括每一分子有3-8个碳原子、优选3-4个碳原子的饱和脂族烃类,例如丙烷、异丁烷、丙烯、正丁烷、正戊烷、异戊烷、正己烷、异辛烷等。其中那些每一分子有3-4个碳原子的稀释剂是优选的,异丁烷是最优选的。
聚合流出物的卸料速率是这样的,以致浆液环管反应器的连续工艺物流从液化的聚合流出物的卸料点通过单点卸料阀,还通过第一闪蒸釜和有关的蒸汽回收和固体回收体系。聚合流出物的卸料速率是这样的,以致在浆液反应器中保持恒定压力以及消除在浆液反应器上的沉降腿出现的,与部分反应器物料卸料有关的断续高压脉冲。
从反应器中排出的聚合流出物浆液为了汽化在输送到第一闪蒸釜的过程中被加热到低于聚合物熔融的温度。这一点可通过适当加热第一输送管来实现。在通过这一第一输送管输送到第一闪蒸釜的过程中,提供给聚合流出物的热量优选应至少等于在第一闪蒸釜中突然汽化这一数量惰性稀释剂所需的热量。然后它还供给要送入第二闪蒸釜的在第一闪蒸釜中形成的浓缩的聚合物固体,达到较高的固体温度,因此有助于通过第二闪蒸釜的操作除去在这样的聚合物固体的孔中残留的稀释剂。在通过第一输送管转移到第一闪蒸釜的过程中,传递给聚合流出物的热量甚至可更大,唯一的条件是,如此传递的热量不会引起其中的聚合物固体被加热到这样的温度,在这样的温度下聚合物固体倾向于熔融或相互团聚。
将浓缩的聚合物固体/浆液从第一闪蒸釜卸料到有这样的长度(l)和直径(d)的第一闪蒸釜出口密封室,以致提供这样一体积,它足以维持这样一浓缩聚合物固体/浆液的体积,以便在出口密封室维持压力封。浓缩的聚合物固体/浆液通过出口密封室渐缩管从出口密封室卸料到第二输送管,它将浓缩的聚合物固体/浆液作为活塞流送到第二闪蒸釜。出口密封室渐缩管由水平方向的倾斜角等于或大于浓缩的聚合物固体/浆液的滑动角的基本上直的侧面确定。
第一闪蒸步骤的压力与稀释剂和未反应单体的性质以及聚合流出物的温度有密切关系。通常,可采用约140至约315磅/平方英寸(绝)范围的压力;更优选约200至约270磅/平方英寸(绝)、最优选约225至约250磅/平方英寸(绝)。
用于冷凝第一闪蒸步骤得到的蒸汽的热交换流体处于约65至135°F的温度范围内。优选的实施方案使用处于约75至约125°F的热交换流体。最优选的实施方案使用处于约85至约115°F的热交换流体。
参考附图1对本发明提供进一步的了解,图1说明本发明一实施方案包括的一体系。
在图1说明的实施方案中,聚合在环管反应器1中进行。聚合混合物用搅拌器2进行循环。稀释剂、共聚单体和单体分别通过各自的处理器床层37、38和39和通过连接到管线6的管线5、4和3从稀释剂贮罐40、共聚单体贮罐41和单体贮罐42送入。催化剂通过管线7加入。通常,催化剂作为在烃类稀释剂中的悬浮液送入。
聚合流出物用连续卸料法通过单点卸料阀8从环管反应器中取出。聚合流出物从卸料阀8送入管线9,管线9安装有管线加热器10,然后送入第一闪蒸釜11,它将汽化的液体介质从聚合物固体/浆液中分离出来。管线9有间接换热设备,例如管线加热器10。
含有稀释剂和未反应单体的汽化的液体介质通过输送管12排出第一闪蒸釜11,汽化的液体介质通过输送管12送入旋风分离器13,它将夹带的聚合物固体从蒸汽中分出。用旋风分离器分离出的聚合物固体通过管线14和用来维持旋风分离器13下方的压力封的双阀组件送入较低压力的闪蒸釜15。
在第一闪蒸釜11底部的浓缩的聚合物固体/浆液通过第一闪蒸釜的直线底面16连续沉降入密封室17,后者在放大的图2中说明。在密封室17中维持一定的聚合物固体/浆液料面43,以便消除第一闪蒸釜11中的堵塞倾向以及形成一个压力封,以致闪蒸釜11可在大大高于闪蒸釜15的压力下操作。聚合物固体/浆液从密封室17连续卸料到较低压力的闪蒸釜15。这样选择密封室的长度(l)、直径(d)和体积以及密封室出口渐缩管18的几何形状,以致提供可变的停留时间和浓缩的聚合物固体/浆液的连续活塞流,以便减少“死”空间和减少堵塞倾向。密封室17的长度必需足以使实际的料面可测量和控制。浓缩的聚合物固体/浆液在密封室17中的典型停留时间为5秒至10分,优选停留时间为10秒至2分,最优选停留时间为15-45秒。浓缩的聚合物固体/浆液的连续活塞流形成压力封,其中在密封室17内,浓缩的聚合物固体/浆液的l/d比通常为1.5-8,优选l/d为2-6,最优选l/d为2.2-3。通常,密封室出口渐缩管18的侧面相对于水平面倾斜60-85度、优选65-80度、最优选68-75度。密封室出口渐缩管18的几何形状由沿水平的倾斜角等于或大于浓缩的聚合物固体/浆液的滑动角的基本上直的侧面确定,它将浓缩的聚合物固体/浆液送至第二输送管19,后者与闪蒸釜15的进料入口相连。在闪蒸釜15中,在浓缩的聚合物流出物中基本上所有残留的惰性稀释剂和未反应的单体在约15至约35psia的压力下汽化并作为釜顶产物通过管线20送入第二旋风分离器21。
聚合流出物中大部分液体介质作为蒸汽送到旋风分离器13。除去夹带的聚合物固体以后的蒸汽通过管线22和热交换器23,其中通过间接与热交换流体换热使处于约140至约315磅/平方英寸(绝)的蒸汽冷凝,以致不需要压缩。
含有稀释剂和未反应单体的冷凝液体介质然后送至贮料罐24。泵25用于将冷凝的液体介质通过管线26输送回聚合段。
在较低压力的闪蒸釜15中,聚合物固体通过管线27送入传统的干燥器28。第二旋风分离器21排出的蒸汽在过滤单元29中经过滤以后通过管线30送入压缩机31,而经压缩的蒸汽通过管线32送入冷凝器33,在那里蒸汽被冷凝,而冷凝液通过管线34送入贮罐35。在贮罐35中的冷凝液体介质通常放空罐顶产物,以便除去轻质杂质。惰性稀释剂可通过处理器床层37除去催化剂毒物后返回该工节过程或在单元36中蒸馏,以便更完全地除去轻质组分,然后通过处理器床层返回该工艺过程。
虽然已广泛地描述了本发明,但是我们认为通过参考以下实施例,本发明将变得更加清楚。应当理解,这些实施例仅是为了说明,不应把它们作为本发明的限制。
实施例
买施例1
在约215°F和565磅/平方英寸(绝)下进行典型的乙烯聚合法。这样的方法的一个实施例得到约83000磅/小时聚合流出物,它含有约45000磅/小时聚乙烯聚合物固体和约38000磅/小时异丁烷和未反应的单体。连续排出的聚合流出物在约240磅/平方英寸(绝)和约180°F下的第一闪蒸釜中闪蒸,以便除去约35000磅/小时稀释剂和未反应单体蒸汽和夹带的颗粒的釜顶产物。在卸料阀和第一闪蒸釜之间的转移过程中,通过适当的加热设备将辅助加热提供的新加热量供给聚合流出物。除去细颗粒以后,不经压缩而通过在约240磅/平方英寸(绝)和约135°F下热交换将异丁烷蒸汽冷凝。从第一闪蒸釜底部排到密封室的聚合物固体/浆形成浓缩聚合物固体/浆液的连续活塞流,它提供了一压力封,在l/d比为5.5的8英寸4英分长密封室中,聚合物固体/浆液塞的l/d比为2.5,在密封室出口渐缩管上有大约68度锥角。浓缩的聚合物固体/浆液的连续活塞流的停留时间为约16秒。浓缩的聚合物固体/浆液从处于约180°F和约240磅/平方英寸(绝)的第一闪蒸釜底部通过密封室、密封室出口渐缩管和第二输送管卸料至第二闪蒸釜上的进料入口。送入第二闪蒸釜的浓缩的聚合物固体/浆液中的残留液体介质在约175°F和约25磅/平方英寸(绝)下闪蒸,除去大约4300磅/小时异丁烷和未反应的单体,它们通过压缩和热交换被冷凝。
实施例2
在约215°F和565磅/平方英寸(绝)下进行典型的乙烯聚合法。这样的方法的一个实施例得到约83000磅/小时聚合流出物,它含有约45000磅/小时聚乙烯聚合物固体和约38000磅/小时异丁烷和未反应的单体。连续排出的聚合流出物在约240磅/平方英寸(绝)和约175°F下在第一闪蒸釜中闪蒸,以便除去约23000磅/小时稀释剂和未反应的单体蒸汽和夹带的颗粒的釜顶产物。除去细颗粒以后,不经压缩而通过在约240磅/平方英寸(绝)和约112°F下热交换将异丁烷蒸汽冷凝。从第一闪蒸釜底部排入密封室的聚合物固体/浆液形成浓缩的聚合物固体/浆液的连续活塞流,它提供一压力封,在l/d为5.5的8英寸4英分长的密封室中,聚合物固体/浆液塞的l/d比为2.5,密封室出口渐缩管上的锥角为约68度。浓缩的聚合物固体/浆液连续活塞流在密封室中的停留时间为约16秒。大约60000磅/小时浓缩的聚合物固体/浆液从处于约175°F和约240磅/平方英寸(绝)的第一闪蒸釜的底部通过密封室、密封室出口渐缩管和第二输送管连续排料到第二闪蒸釜上的进料入口。送入第二闪蒸釜的浓缩的聚合物固体/浆液中残留的液体介质在约125°F和约25磅/平方英寸(绝)下闪蒸,以便除去约16000磅/小时异丁烷和未反应的单体,它们通过压缩和热交换被冷凝。

Claims (24)

1.一种从聚合物浆液中除去和回收聚合液体介质的设备,该聚合物是在反应器中生成的、以颗粒聚合物固体形式悬浮在一种液体介质中,该液体介质含有一种惰性稀释剂和未反应的单体,该设备包括
一个卸料阀,用于将一部分所述的聚合物浆液从所述的反应器连续卸料到第一输送管;
所述的第一输送管将其中的所述的聚合物浆液送入第一闪蒸釜,该釜的底部与长度为(1)和直径(d)的第一闪蒸釜出口密封室相连,后者有一定体积的所述聚合物的连续活塞流,其中所述的浓缩聚合物固体/浆液的连续活塞流的所述体积的长(1)与直径(d)之比(1/d)为约1.5至约8.0;
有密封室出口渐缩管的所述密封室,后者由水平方向倾斜角等于或大于从中除去约50至100%惰性稀释剂以后留下的聚合物固体的滑动角的基本上直立侧面限定,后者将浓缩的聚合物固体/浆液的连续流从所述的第一闪蒸釜出口密封室送至第二输送管,它将所述的浓缩聚合物/浆液的连续流送至第二闪蒸釜;以及
所述的第二闪蒸釜在大大低于所述的第一闪蒸釜的压力下操作,以致基本上所有残留的惰性稀释剂和未反应的单体被汽化,并通过闪蒸釜釜顶出口送至稀释剂和单体的回收体系,而基本上干燥的聚合物固体送至干燥器/贮罐。
2.根据权利要求1的设备,其中第一闪蒸釜的底部由沿水平方向的倾斜角等于或大于从中除去约50至100%惰性稀释剂以后留下的浓缩聚合物固体/浆液的滑动角的基本上直立侧面确定。
3.根据权利要求1的设备,其中所述的第一闪蒸釜出口密封室有一定体积的所述聚合物的连续活塞流,其中所述的浓缩聚合物固体/浆液的连续活塞的所述体积的长(1)与直径(d)之比(1/d)为约2至约6。
4.根据权利要求3的设备,其中所述的第一输送管用能提供足以使其中所述的浆液维持在低于聚合物熔点温度的热量的加热器设备加热。
5.根据权利要求1的设备,其中卸料阀以这样的速率使聚合流出物卸料,以便在浆液反应器中维持恒定的压力。
6.一种生产聚合物的方法,其中包括生产在液体介质中的聚合物浆液,该方法包括,
在一个浆液反应器中使至少一种单体在一种惰性稀释剂中聚合,生成一种在液体介质中的聚合物固体的浆液;
将浆液作为聚合流出物从浆液反应器中连续卸料到第一闪蒸釜;
在第一闪蒸中使所述的聚合流出物闪蒸,其中在所述的第一闪蒸釜中的压力和所述的聚合物流出物的温度是这样的,以致使约50至约100%的液体介质变成蒸汽,所述的蒸汽可不经压缩而通过与约18至约57℃的流体作热交换而冷凝,以产生浓缩的聚合物流出物和蒸发的液体;
连续分离浓缩的聚合物流出物浆液和蒸发了的液体;
其中从浆液反应器中聚合流出物的卸料比率要使浆液反应器中的压力维持恒定。
7.根据权利要求6的方法,其中
通过卸料阀将所述的聚合流出物连续卸料到第一输送管;
将所述的第一输送管中的所述的聚合流出物加热到低于聚合物熔点的温度;并
通过所述的第一输送管将所述的聚合物流出物连续送入第一闪蒸釜。
8.根据权利要求6或7的方法,其中
在所述的第一闪蒸步骤中制得的所述的蒸汽不经压缩而通过与约18至约57℃的流体热交换而连续冷凝;
将浓缩的聚合物固体/浆液从所述的第一闪蒸釜连续卸料到第二闪蒸釜;
将所述的浓缩的聚合物固体/浆液中剩余的液体介质连续暴露到从所述的第一闪蒸釜中的较高压力:约965.3至约2171.8kPa(绝)到所述的第二闪蒸釜中的较低压力:约103.4至约241.3kPa(绝)的进一步压降中,其中所述的第二闪蒸釜的压力和所述的经加热的浓缩聚合物浆液的温度是这样的,以致使基本上所有的残留稀释剂和单体都变成蒸汽,而所述的蒸汽通过压缩和冷却可冷凝;以及
使基本上不含稀释剂或未反应单体的聚合物固体从所述的第二闪蒸釜连续卸料。
9.根据权利要求8的方法,其中通过将浓缩的聚合物固体/浆液通过这样一密封室,从所述的第一闪蒸釜连续卸料到第二闪蒸釜,其中所述的密封室有这样的长度(1)和直径(d),以致在所述的密封室有一定体积的所述聚合物的连续活塞流,其中所述的浓缩聚合物固体/浆液的连续活塞的所述体积的长(1)与直径(d)之比(l/d)为约1.5至约8.0;
将所述的浓缩的聚合物固体/浆液通过这样一密封室出口渐缩管连续送至第二闪蒸釜,密封室出口渐缩管由沿水平方向的倾斜角等于或大于从中除去约50至100%惰性稀释剂以后留下的聚合物固体滑动角的基本上直立侧面确定。
10.根据权利要求6或7的方法,其中第一闪蒸釜的底部由沿水平方向的倾斜角等于或大于从中除去约50至100%惰性稀释剂以后留下的浓缩聚合物固体/浆液的滑动角的基本上直立侧面确定。
11.根据权利要求6或7的方法,其中向聚合流出物中提供的热量至少要等于在所说闪蒸中待蒸发的聚合流出物的蒸发热。
12.根据权利要求7的方法,其中所述的第一输送管用这样一种加热设备加热,它的加热能力具有能提供足以使其中的所述聚合物浆液加热到低于聚合物固体熔点温度的热量。
13.根据权利要求12的方法,其中所述的惰性稀释剂为异丁烷。
14.根据权利要求6或7的方法,其中液体介质在反应器出口处含有浓度大于或等于4%(重量)的增加的乙烯浓度。
15.根据权利要求9的方法,其中浓缩的聚合物固体/浆液在密封室中的停留时间为5秒至10分。
16.根据权利要求9的方法,其中浓缩的聚合物固体/浆液在密封室中的停留时间为10秒至2分。
17.根据权利要求9的方法,其中浓缩的聚合物固体/浆液在密封室中的停留时间为15-45秒。
18.根据权利要求9的方法,其中在第二闪蒸釜中,浓缩的聚合流出物中基本上任何残留的惰性稀释剂和未反应的单体都被汽化和除去。
19.根据权利要求6或7的方法,其中聚合流出物的出料比率要消除在浆液反应器中间歇的高压脉动。
20.根据权利要求6或7的方法,其中聚合在一个回路反应器中进行。
21.根据权利要求8的方法,其中,从第一次闪蒸中蒸发的液体含有夹带的聚合物固体并进行一次分离,以使聚合物固体与蒸发了的液体相分离。
22.根据权利要求21的方法,其中,从第一次闪蒸中得到的分离了的、蒸发了的液体通过间接的热交换而冷凝。
23.根据权利要求22的方法,其中,从第二次闪蒸中蒸发了的液体含有夹带的聚合物固体并进行一次分离,以使聚合物固体与蒸发了的液体相分离。
24.根据权利要求23的方法,其中,从第二次闪蒸中蒸发的液体通过压缩而冷凝。
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CN1293592A (zh) 2001-05-02
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BR9908487A (pt) 2000-12-05
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US6204344B1 (en) 2001-03-20
JP2002506718A (ja) 2002-03-05
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