CN100377772C - 具有用于固体床催化剂的过滤器的反应器 - Google Patents
具有用于固体床催化剂的过滤器的反应器 Download PDFInfo
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- CN100377772C CN100377772C CNB2003801101391A CN200380110139A CN100377772C CN 100377772 C CN100377772 C CN 100377772C CN B2003801101391 A CNB2003801101391 A CN B2003801101391A CN 200380110139 A CN200380110139 A CN 200380110139A CN 100377772 C CN100377772 C CN 100377772C
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Abstract
本发明公开了一种反应器结构,这种反应器结构特别适合相间质量传递和混合多种相,即气相、液相和固相,其中,反应是通过固体催化剂催化的,该反应器包括通风管反应器,其中,固体催化剂颗粒通过过滤部件(26,27)保持在反应器的通风管(21)和环形限定壁之间的环形空间(26)中,过滤部件位于催化剂床的下游,并且可选择地位于它的上游。
Description
技术领域
本发明涉及特别适用于在液相中采用了固体催化剂的多相反应的反应器配置,并且涉及采用所述反应器的烯烃环氧化工艺。
背景技术
当今产生的大部分环氧丙烷是通过所谓的“副产物”过程产生的,其中,容易氧化的底物被氧化,以便产生过氧化氢物和/或过氧化物,它们随后被用于“间接”氧化丙烯。所述氧化底物的还原产物是大量产生的,并且作为副产物出售。典型的副产物是苯乙烯和甲基-t-丁基醚。由于所述工艺需要购买可氧化的底物,并且销售副产物,它们中每一个的价格可能有很大的差异,业已研究了“直接氧化”工艺,其中,市场波动不会控制该工艺的总体经济效益。
由于在支撑的银催化剂上用氧气对乙烯进行环氧化业已被广泛地应用,对丙烯的类似的氧化作用是不可行的。最近的针对丙烯的“直接氧化”的研究活动,集中在过氧化氢的使用方面,过氧化氢是在存在作为催化剂的诸如钛硅质岩(titanium silicalite)的硅酸钛沸石(titaniumsilicate zeolite)的条件下在外部或原位产生的。可以对固体晶体催化剂颗粒进行处理,以便含有贵金属,它能催化由氢和氧产生的过氧化氢产物。如果这种工艺在商业上是可行的话,只会使用低成本的反应剂,并且不会产生副产物。
在美国专利号6,376,686中披露了一种烯烃环氧化工艺,该工艺将固体催化剂应用在一种反应器结构中,该反应器结构类似于在美国专利号5,972,661中所披露的结构。在后一份专利文件中,披露了“导管”反应器,图1示出了该反应器的简化示意图。包括固体催化剂在内的反应剂糊状物进入中央导管,并且被通过它里面的叶轮沿导管的轴向引导。位于叶轮之间的一系列垂直方向的挡板阻止了有可能导致固体催化剂分离的回旋流。在到达导管端部之后,糊状物沿逆流方向在导管和反应器壁之间的环形区流过。连续地排出产物,与夹带的催化剂分离,并且逐渐排出溶剂,副产品等。必须将催化剂送回反应器。业已发现所述反应器结构具有高的质量转移和混合速度。催化剂是活性成分和惰性粘合剂的组合。在剧烈搅拌条件下,催化剂可能逐渐发生分解,产生细粒,这些细粒会导致过滤设备的堵塞。所述细粒还可能通过过滤设备,导致催化剂从反应器-过滤装置中流失。
需要生产一种反应器结构,它能够具有导管反应器的质量转移特征,同时导致较少的催化剂损耗。
发明内容
本发明涉及导管反应器,其中,催化剂位于固定床上,固定床位于内部通风管和反应器壁之间的环形区,通过优选放置在催化剂床上面和下面的过滤介质,将催化剂保持在所述环形区中。由于催化剂不是作为糊状物循环的,降低了催化剂损耗,使得可以使用多种催化剂颗粒,包括催化剂颗粒聚集物。
本发明涉及在一种包括使液体反应介质中的催化剂糊中的烯烃在上述的反应器中环氧化并且从它的产物流中分离氧化烯烃的方法,其特征在于:所述入口输入流包括氢和氧,而所述催化剂包括处理过的包含钯的钛硅质岩。
附图说明
图1表示现有技术中导管反应器在反应中的使用,其中,固体催化剂的糊状物是循环的。
图2示意性地表示本发明的通风管反应器,其中,将催化剂的固定床用于反应器环形区。
图3表示采用催化剂筐的本发明的导管反应器的一种实施方案;
图4a-4e表示催化剂筐的一种实施方案的结构。
具体实施方式
图1表示现有技术中导管反应器1,可将它用于多相反应,并且包括糊状固体催化剂。导管3位于反应器外壳2中,将相关的输入流引入其中,在这里是指液体输送管4和蒸汽(气体)输送管5。在导管内具有由马达M驱动的叶轮6,它导致通过导管3的向上流动,并且充分混合反应剂输送流和催化剂糊状物。在导管3的顶部,反应混合物糊状物通过导管3和反应器壁2之间的环形空间7反向流动。一部分通过导管3的底部向回再循环,而其他部分被从出口8中排出,并且由循环泵9泵送通过过滤器10。排出过滤的产物流11,并且加工,以便排出产品、未反应的原材料、再循环的溶剂等,同时将富含固体催化剂的糊状物12送回所述反应器。通过在反应器、泵和循环管道中通过固体催化剂磨损产生的催化剂细粒积累在过滤器10上,最终堵塞该过滤器。
在本发明中,固体催化剂颗粒保持在中央通风管和反应器壁之间的环形区。参见图2,中央通风管21包含安装在由马达M驱动的轴23上的叶轮22。在导管21和反应器壁24之间是环形区25,它包括固体催化剂。在环形区25的顶部覆盖有滤板26。第二滤板27位于该环形区的底部。滤板可以用烧结的金属、陶瓷、金属网等制成。反应剂通过一个或多个入口28进入反应器,并且在通风管中密切地混合,通风管选择性地包括位于叶轮之间的挡板29。液体成分在到达通风管端部时,通过滤板26向下引导通过催化剂床,并且通过滤板27。所述液体的一部分重新进入通风管,同时一部分被从出口30中排出,用于分离产物和其他成分的适当处理/再利用。
本发明的反应器特别适用于以下场合,其中,各种反应剂流,优选还包括气体反应剂,必须与固体、多相催化剂密切混合并且接触。所述反应器特别适用于“直接的”烯烃环氧化反应,不过它的用途并不局限于此。在以下说明中,烯烃环氧化将被用于说明所述反应器的用途。
例如对于丙烯环氧化来说,环氧化催化剂可以是具有较大尺寸的钯处理过的钛硅质岩晶体,以便可以保持合理的反压力,或者可以是较大的钛硅质岩晶体的聚集物,正如在美国专利5,500,199和6,106,803中所披露的。反应剂输入流可以包括丙烯、氢、氧、液相、即甲醇、惰性气体如挥发性烃或氮气、二氧化碳、氩等。产物流通常包括可以分离和再循环的未反应的气体,通常可再循环的溶剂,以及环氧丙烷和“环氧丙烷等同物”,即开环的和各种缩合产物。环氧丙烷产物是通过烃加工领域的技术人员所熟知的方法分离和提纯的,优选通过一系列分馏进行。任何磨损的催化剂都会积累在第一分馏器底部,除非事先通过诸如离心的其他技术分离。可以对回收的催化剂细粒进行加工,以便重新得到贵金属的价值。
由于催化剂颗粒不会受到叶轮或泵的高的剪切力,磨损是非常低的。通过磨损所产生的任何细粒都允许积累在分馏器底部,以便定期排出,而不是采用小孔过滤器进行堵塞。不过,由于存在少量的细粒,对于本发明的反应器来说,通过过滤或通过离心或其他技术排出仍然是可选方案。
所述反应器设计优选是这样的,即过滤部件可以定期更换。所述过滤部件通常还需要物理上的支持。在图3中示出了允许这种特征的反应器结构,虽然,有多种支撑过滤部件的方法对于化学工程和反应器设计领域的技术人员来说是显而易见的。
在图3中,大体上为圆筒状的反应器50包括“催化剂筐”31,它作为整体组件。催化剂筐优选紧靠反应器内壁32安装。从催化剂筐周围流过而不是通过催化剂筐流过的流体由O-形圈密封件34和35阻止,不过其他结构可能也是适合的。例如,可以在反应器壁上设置接收平台,将该筐安装在它上面。例如,安装可以通过螺栓环(ring ofboIt)实现,并且可以将垫圈放置在接收平台和所述筐之间。尽管整个反应器通常保持在高压下,所述压力在整个内部空间中是大体上相等的,因此,所述O-形圈、垫圈或类似装置只需要能够控制由液体流产生的压力差即可。在很多场合下,可以省去O-形圈和垫圈等。所述筐环绕通风管21和叶轮22。在某些设计中,所述筐的内壁可以构成通风管的管壁。
催化剂筐31可以通过化学工程和金属加工领域认可的任何技术组装,例如,通过组装图4a-4e中所示出的部件。在一种优选实施方案中,在顶部环36上加工出平台38和40,以便接纳内管37和外管39。内管用作反应器的通风管或它的一部分,或具有一定尺寸从而能环绕固定的中央通风管。还制备了具有类似平台42和44的底部环48。一般,将内管和外管焊接在所述平台上,以便产生基本的催化剂筐。在图4c中示出了顶部环的俯视图,它还示出仰视的底部环。
跨越催化剂筐的外套筒39和通风管37之间的环形空间的顶部盖子49可安装在顶部环上。所述盖子包括通道41(参见图4b),并且顶部过滤部件42通常安装在顶部盖子和顶部环36之间。如果液体流是来自通风管的顶部并且通过催化剂筐的环形空间的顶部的话,顶部过滤部件42孔的尺寸可能是相当大的,并且例如可以采用一个或多个不锈钢网层的形式。在其他场合下,只要稳定地保持所述液体流稳定,就可以省去最上面的筛网。不过,这样的实施方案不是优选的。图4b示出了来自上部和下部的顶部盖子和底部盖子。图4c表示环36的俯视图,示出了部分47b,它允许通过位于相应的结构47a上的孔将顶部盖子49安装在顶部环36上。图4d表示顶部和底部过滤器,而图4e表示内管和外管之间的关系。
在催化剂筐的底部是类似的底部盖子45。将底部过滤部件46固定在底部盖子45和底部环之间。底部过滤部件46应当加工成具有这样的孔的尺寸,以便能保留固体催化剂,少量的催化剂细粒除外。例如,合适的公称孔尺寸可以为4-10μm。预计尺寸小于1μm的某些催化剂细粒能够通过所述过滤部件。特别对于约为0.2μm或更小的颗粒来说更是如此,这种颗粒在堵塞催化剂过滤器方面最成问题。不过,所述细粒的数量是很小的。底部过滤部件46可以用细的筛网制成,不过优选是烧结的金属或陶瓷过滤部件。如果期望具有非常小的催化剂颗粒,即尺寸<1μm的颗粒的床的话,所述底部过滤部件要用更细的有孔材料制成。
反应器可以包括一个催化剂筐或多个催化剂筐,在它们之间没有密封装置或有常规的密封装置,例如,O-形圈,垫圈等。阻止液体在所述筐之间流动而不是从一端流向另一端还可以通过用管状衬里衬在所述复合通风管上来阻止,或通过其他方式阻止。例如,所述反应器可以包括固定在适当位置的通风管,并且催化剂筐可以设置中央孔,该孔的内径是这样的,使得该筐可以插入反应器壁和固定通风管之间。
催化剂筐的使用使得可以方便地更换反应器中的该筐,以便提供新的催化剂,修复过滤部件等,而又没有停机时间,这些时间是其他反应器设计所需要的。不过,能够以商业上认为可行的任何方式组装反应器。例如,当过滤部件是烧结的不锈钢时,它们能够以具有中央孔的圆盘形式提供,并且焊接在通风管和焊接在反应器壁上。优选地,所述过滤部件的设计和/或它们安装在反应器或催化剂筐中的模式使得能够取出用过的催化剂并且更换它们。在有目的地将过滤器孔做得很大以便细粒能够从反应器中排出的设计中,还可以在操作期间掺入其他催化剂,例如,在使用时以新鲜催化剂的糊状物形式直接导入反应器的环形空间或导入催化剂筐。
流过通风管的方向优选是通过叶轮确定的,不过气体或液体反应剂的向上流动可用于在无叶轮的结构中建立流动。在使用叶轮时,流动可以是向上的或向下的。反应器还可以是水平定位的。优选地,垂直的反应器具有向上的、通过通风管的叶轮驱动的流动。
反应剂、溶剂、和其他原料流通常是在靠近通风管端部或在其内部引入反应器的。叶轮在通风管中的良好的混合作用,能非常有效地混合所述成分。例如,可以迅速获得诸如氢和氧的气体的最大溶解度。当通风管中的液体离开通风管并且通过催化剂床开始流动时,所述反应剂业已充分混合。
在反应剂流过催化剂床时,进行了催化过程,并且产物、副产物、未反应的原始反应剂等离开催化剂床。由于催化剂可以具有大的尺寸而不用担心磨损,可以使用大量的催化剂,例如,可以超过在常规反应器中颗粒的糊状物能够保留的数量。结果,更大比例的反应剂能够起反应,并且较少的未反应的原材料可以离开催化剂床。
产物的排出通常是从反应器的靠近催化剂床的出口的端部排出的。在具有向上的通风管流的垂直反应器中,所述排出优选位于底部环形过滤部件的下面。当然,其他产物出口也是可能的。所述离开的产物可以是成比例的,从而使离开过滤器床通过通风管返回、并且从这里再次通过过滤器床的一部分液体进行循环。这样,可以最佳地调整转化效率。
产物流可以直接进行纯化/回收/再利用,或者可以用作进入流输入其他反应器,以便进一步使反应最大化。在使用第二个反应器时,它们可以是相同类型或不同类型的。例如,它们可以是具有位于过滤部件之间的固体催化剂的简单的管状反应器。可以将一个或多个其他的原料流送入第二反应器,以便减少存在于第一反应器产物流中的反应剂,或将永久性气体的含量调整到不爆炸的极限。例如,当产物流包括未反应的氢和氧时,可以添加额外的丙烯,以便降低氧的含量。可以添加甲烷、乙烷或丙烷以便调节可燃性极限等。
产物流通常包括未反应的可冷凝的或永久性气体,即氢、氧、丙烯、氮气、甲烷等,反应器溶剂和产物混合物。所述产物混合物包括环氧丙烷和“环氧丙烷等同物”,即其它物质中的丙二醇,二丙二醇,丙二醇甲醚等。可以通过闪蒸(flashing)或其他技术除去所述永久性气体,并且再次加压和再利用。另外,可以将它们注入锅炉中用于它们的燃料价值。优选回收丙烯和可冷凝的气体并且再循环。溶剂,即甲醇,优选也被再循环。从环氧丙烷等同物和其他杂质中分离环氧丙烷可以使用常规蒸馏技术进行。
可以改变过滤部件的孔的尺寸,以便适应特定的催化剂尺寸,并且预期通过磨损产生细粒。合适的公称孔尺寸在0.1μm-40μm范围内,更优选在1μm-20μm范围内,最优选在4μm-15μm范围内。本发明的特征是,与在催化剂糊状物循环的其他系统相比,催化剂的尺寸不是那么重要。例如,在具有增加截面积的所述床上可以使用小的催化剂粒度,以便减少压力下降。在使用这种小的催化剂时,过滤部件的孔尺寸应当在上述范围的低端侧。在使用大尺寸催化剂,即2μm-40μm或更大尺寸时,可以进一步提高孔尺寸。对于尺寸为6-12μm的催化剂来说,例如单一的大型钛硅质岩晶体,3-4μm的公称孔尺寸被认为是合适的。尽管看上去这种过滤器允许相对较大的,即2-3μm的“细粒”通过,但是业已发现,在实践中,这种“粗糙的”过滤器通常不能通过这种颗粒尺寸,也许是因为通过用来形成过滤部件的烧结工艺所产生的孔的螺旋形特性。可以特别地选择某些孔尺寸,以便允许某些细粒通过,特别是具有非常小的颗粒尺寸的细粒通过。所述细粒通常会积聚在产物蒸馏底部并且由于它们的量很小,不会造成分离问题。
“大体上阻止”催化剂离开催化剂床,表示大部分催化剂会留在催化剂床上,正如上面所描述的。优选的是,所述孔尺寸应当为大体上阻止具有超过填充到反应器中的平均体积催化剂颗粒尺寸20%的颗粒尺寸的催化剂颗粒通过。
本文所使用的术语“固体催化剂”表示位于催化剂床中以便液体流可以被引导通过催化剂床的颗粒状的催化剂。所述液体流的阻力与催化剂颗粒的尺寸以及它们的几何形状和反压力相关,随着颗粒尺寸的降低,催化剂床的反压力随着每一个截面积增量而增加。不能够紧密组合在一起或具有大致为球形几何形状的催化剂颗粒允许增加的流体流。对于用L/h表示的给定流体流来说,通过相应地增加或降低残留催化剂的环形空间的截面积,所述流可以增加或降低催化剂颗粒的给定的尺寸和形状。所述流还会受到催化剂床长度的影响。由于在本发明的反应器中催化剂磨损不太严重,可以使用较多数量的催化剂,这是因为催化剂的工作寿命显著提高了。
优选的过滤部件是用烧结的多孔不锈钢制成。这种烧结的过滤器产品可以从Mott公司获得。
在不超出本发明构思的前提下,有多种所披露的反应器的变化形式是可行的。例如,所述反应器可以设计为带有加热和/或冷却部件,即散热片、板式换热器、螺旋管、回路等。还可以增加其他混合部件以及液体再循环回路等。最低限度的要求是一个通风管反应器,在通风管和反应器内壁之间具有环形空间,在该环形空间中放置有固体催化剂,并且通过至少一个、优选为两个过滤部件保持在所述环形区中,至少一个过滤部件相对流体流动方向而言位于催化剂床之外。应当指出的是,用于说明通风管位置的术语“中央的”并不意味着该通风管绝对位于反应器的中央。例如,它可以偏离中央。用于表示过滤部件位置的“位于环形空间”表示位于该环形空间中或位于环形空间顶部,以便能大体上阻止流体进入或离开所述环形空间,例如,液体不通过过滤部件的情况。例如,过滤部件可以位于环形空间上方,如图3所示。
在某些优选实施方案中,可能需要可溶性反应剂、溶剂和反应产物穿过或通过通风管的壁流动。在使用具有多孔侧,即金属筛网材料侧的催化剂筐时,这样的实施方案可能是特别有用的。这种通过通风管壁的流动,可以通过在所述壁上开孔、开槽等,或者通过构成全部或部分多孔材料,即多孔的烧结不锈钢制成的通风管而易于实现。上述实施方案是示例性的而不是限定性的。
尽管业已解释和说明了本发明的实施方案,但是并不意味着这些实施方案解释和说明了本发明的所有形式。而是,在本说明书中所使用的词语是说明性的词语,而不是限定性的,并且,应当理解的是,在不超出本发明构思和范围的前提下,可以进行各种改变。在权利要求书中,除非另有说明,单词“a”和“an”表示一个或一个以上。
Claims (8)
1.一种反应器,其具有位于反应器中的中央的通风管、位于通风管中的至少一个叶轮、位于通风管和反应器壁之间的环形空间、以及位于通风管中的沿一个方向的流体通道,和通过所述环形空间的逆流,其特征在于
a)在所述环形空间内提供至少一个空间,用于接纳固体催化剂,以便形成催化剂床;
b)在所述环形空间中设置一顶部过滤部件,其相对通过所述环形空间的流体流方向而言位于所述催化剂床的下游,所述顶部过滤部件具有孔以允许流体流通过所述顶部过滤部件,所述孔的尺寸足够小,以便大体上能阻止催化剂颗粒离开所述催化剂床;
c)提供底部过滤部件,其上具有孔,以便允许流体流通过位于所述环形空间中的底部过滤部件,该底部过滤部件相对通过所述环形空间的流体流方向而言位于所述催化剂床的上游;
所述反应器具有至少一个入口输入流,和至少一个产品输出流;
所述反应器包括具有内壁的反应器外壳,和位于所述反应器中的至少一个催化剂筐,所述催化剂筐包括:
i)中央管和较大的环面限定管;
ii)顶部环和底部环,所述顶部环和底部环中的每一个固定在所述中央管和所述环面限定管上,所述中央管和环面限定管之间的空间限定一适合容纳固体催化剂填充量的环形空间;
iii)所述顶部过滤部件位于所述顶部环上方以便进入所述环形空间的流体通过所述顶部过滤部件;
iv)所述底部过滤部件位于所述底部环下方以便离开所述环形空间的流体通过所述底部过滤部件,
所述中央管环绕所述通风管或包括所述通风管。
2.如权利要求1所述的反应器,其中,所述通风管包括靠近所述至少一个叶轮的一个或多个挡板,并且所述挡板在所述通风管中垂直定向。
3.如权利要求1所述的反应器,其具有至少一个入口,该入口靠近所述通风管中相对于所述通风管内的流体流方向的上游端终止,或其在所述通风管内终止。
4.如权利要求1所述的反应器,其具有相对通过所述环形空间的流体流方向位于所述环形空间的下游的出口。
5.如权利要求1所述的反应器,其中,所述过滤部件中的至少一个选自下列一组:金属网筛,烧结的多孔金属,多孔陶瓷材料,以及它们的组合。
6.如权利要求1所述的反应器,其中,所述环形空间包括固体催化剂。
7.一种方法,其包括:
(a)使烯烃在权利要求1所述的反应器中环氧化,从而产生包括氧化烯烃的产物流,其中,环氧化是在具有催化剂的情况下在液体反应介质中进行;以及
(b)使氧化烯烃与产物流分离,
其中,所述入口输入流包括氢和氧,所述催化剂包括处理过的包含钯的钛硅质岩。
8.如权利要求7所述的方法,其中,所述液体反应介质包括含氧的溶剂。
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BR0318173A (pt) | 2006-02-21 |
EP1601453B1 (en) | 2009-10-14 |
ATE445456T1 (de) | 2009-10-15 |
AU2003300361A1 (en) | 2004-09-30 |
CN1758954A (zh) | 2006-04-12 |
DE60329716D1 (de) | 2009-11-26 |
EP1601453A1 (en) | 2005-12-07 |
US7279145B2 (en) | 2007-10-09 |
CA2514456A1 (en) | 2004-09-23 |
US20040179983A1 (en) | 2004-09-16 |
KR20050106068A (ko) | 2005-11-08 |
WO2004080584A1 (en) | 2004-09-23 |
US7642365B2 (en) | 2010-01-05 |
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