CN102292416B - 从於浆反应器中取出液体产物和细粒的***和方法 - Google Patents
从於浆反应器中取出液体产物和细粒的***和方法 Download PDFInfo
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Abstract
本发明提供在三相淤浆法中将浆料液体与催化剂分离的方法和装置。本发明实施方案的特征在于在以提供含催化剂浓度为约20重量%或更小的浆料上部区域和催化剂浓度为高于约20重量%的下部区域的条件下进行三相方法。将该上部区域中的一部分浆料脱气并送入液体-固体分离装置中以回收液体产物。
Description
发明领域
本发明一般性地涉及三相液体淤浆法中催化剂、反应产物或二者的分离。更特别地,本发明涉及该***和方法在烃合成方法中的用途,其中在三相於浆反应器中使氢气和一氧化碳的混合物与催化剂颗粒的浆料在液体中接触。
发明背景
三相淤浆法,特别是在泡罩塔中进行的那些广泛报道于科学文献中,因此是本领域技术人员熟知的。该三相淤浆法的实例为通过费-托法制备烃。
通常,费-托烃合成方法通过使合成气(包含H2和CO)的料流与固体催化剂的液体悬浮液接触而进行。合成气通常具有1∶1-3∶1的H2/CO摩尔比。分散液体主要为线性烃反应产物。为促进催化剂与合成气之间的接触,将气体通过产生小气泡的气体分布器供入泡罩塔底部。
通常,於浆方法在足以防止床塌落的条件下,即在防止催化剂颗粒聚集在泡罩塔底部附近的条件下进行。因此,催化剂颗粒的沉降倾向与通过由供入泡罩塔底部的气体产生的上升气泡产生的分散力相反。
由于需要将反应器中的浆料保持在恒定水平,将液体产物连续或定期地从反应器中取出。然而,这样做时,重要的是将分散的催化剂颗粒与要除去的液体分离以保持反应器中恒定的催化剂装料量。通常,分离在位于浆料床内部的过滤区中进行。过滤区通常包含圆柱状过滤介质,液体产物由过滤介质的外部向内部通过它,其中将它收集并从反应器中取出。在一些反应器设计中,将液体产物在外部过滤***中过滤。
与过滤***有关的问题之一是过滤器效率随时间过去而降低,需要补救措施,例如反洗涤过滤介质,最终取出并清洁过滤器元件或置换它。过滤器效率的降低主要是由于液体产物中称为“细粒”的非常小催化剂颗粒的存在,其导致过滤器堵塞。浆料液体中催化剂细粒的存在是由于在存在于反应器容器中的湍流流体动力学条件下随时间过去而出现的催化剂磨耗。
还应提到在外部过滤器***中,由于它不总是保持在工艺条件下,催化剂可变得减活化。
因此,需要提高三相淤浆法中将催化剂颗粒与液体产物分离的效率。还需要控制於浆反应器中的细粒含量以防止过度过滤器反洗涤和积垢。另外,需要不使用过滤器地将液体产物从淤浆法中取出。这些和其它需求通过本发明解决。
发明概述
因此,本发明提供在三相淤浆法中将浆料液体与催化剂分离的方法和装置。本发明实施方案的特征在于在以提供其中浆料中固体浓度为小于约20重量%的在浆料床中的上部区域的条件下进行三相方法。将上部区域中的一部分三相浆料脱气并送入不同于过滤器的液体-固体分离装置中。
在优选实施方案中,淤浆法以塌落床(slumped-bed)模式进行,由此提供其中浆料固体浓度为小于约20重量%固体的在浆料床中的上部区域。
在以下详述中将描述本发明的各个实施方案。
附图简述
图1为说明本发明实施方案的示意图。
图2为说明一种替代分离器在本发明实践中的用途的部分示意图。
图3显示本发明的优选实施方案,其中於浆反应器具有用于取出脱气的浆料以用于本发明分离的外部降液管。
图4为显示本发明另一替代实施方案的部分示意图。
图5为显示当以塌落床模式和分散床模式操作时,浆料催化剂负荷相对于床高度的图。
发明详述
本发明适用于在三相於浆反应器中进行的化学反应。该反应的具体实例为费-托合成法,为方便起见,将特别参考费-托烃合成法描述本发明。
合适地,用于根据本发明进行的费-托合成法的反应器包括用于含悬浮于液相中的催化剂的立式容器,合成气通过它起泡。
如前所述,合成气包含摩尔比为约1∶1-约3∶1的H2和CO。在本方法中,该比优选为2.1∶1。
任何在费-托反应中为活性的催化剂可用于本发明中。优选,催化剂包含有效量的在合适无机载体材料上的Co以及Re、Ru、Fe、Ni、Th、Zr、Hf、U、Mg和La中的一种或多种。
在反应条件下为液体的那些线性烃反应产物包含反应器中的浆料液体。
费-托反应在约320-850°F的温度和80-600psi的压力下进行。
在良好分散的费-托淤浆法中,将合成气以足以克服催化剂颗粒的沉降速度的表观气体速度注入反应器底部或底部附近。
在本发明的实践中,将合成气以足以提供具有上部区域和下部区域的非均相浆料的表观气速注入反应器底部或底部附近。浆料床的上部区域中的催化剂浓度含小于约20重量%的催化剂固体,优选浆料中的固体浓度为小于10重量%,最优选固体浓度为小于5重量%。例如图5显示塌落床操作的两个实例,其中床的上部区域中的固体浓度在约20重量%至约1重量%催化剂固体之间变化。
当然,沿着浆料床中反应器高度的催化剂浓度曲线不仅取决于气体速度,而且取决于催化剂粒度、颗粒密度、总催化剂负荷、反应器的高度和直径,以及浆料液体密度和粘度。
催化剂粒度指有效催化剂粒径。当用于本说明书中时,本体催化剂指平均粒度为大于或等于约10μm,例如约10-150μm的催化剂颗粒。细粒意指粒度为约10μm以下,例如约0.1-10μm的颗粒。
基本上,在本发明方法中,费-托法以塌落床模式操作。在一个实施方案中,这通过使用不具有内部降液管的反应器并将合成操作气体以足够的表观气体速度注入在反应器底部或底部附近使得浆料的上部区域中的催化剂浓度为小于约20重量%固体而实现。在另一实施方案中,塌落床操作使用反应器中具有用于使浆料循环的内部降液管的反应器实现。定径这些降液管并使其位于反应器中使得在操作条件下,在浆料床上部区域中浆料的催化剂固体浓度为小于约20重量%。
在本发明方法中,将含小于约20重量%固体的浆料上部区域中的液体脱气并送入液体-固体分离装置中以分离本体固体。从液体中分离的本体催化剂颗粒返回反应器底部或底部附近。可使分离的液体经受第二段分离步骤以除去细粒,如果需要的话,可将液体产物送入另外的加工。
现在将参考附图描述本发明。
图1显示含有浆料液体11的反应器容器10,所述浆料液体具有上部区域12和下部区域14。容器10包括气体顶部空间15和气体分布器16。提供导管装置以将合成气注入浆料液体中以在其中反应。提供导管装置18用于从顶部空间15除去气体产物。容器10包括位于区域12中的气体分离区19。如图1所示,气体分离区19为在降液管21上的杯状顶20的形式。提供导管装置22用于除去脱气的浆料以输送至液体-固体分离装置23中。在图1中,显示代表斜板分离器的分离器23,可使用其他固体液体分离器。提供导管装置25用于使本体催化剂颗粒返回浆料液体的底部区域。提供导管26用于除去浆料液体以在第二分离段中分离催化剂细粒和根据需要用于另外的加工。
任选地,容器10可包括不横越浆料床11的整个长度且位于下部区域14中的降液管以使催化剂在反应器底部循环。图1所示降液管27代表一个这种降液管。
尽管容器10不需要内部过滤器以取出产物,但也可使用内部过滤器(未显示)。
在图2所示实施方案中,使用水力旋流器29将固体与液体分离。因此,将脱气的浆料经由导管22输送至水力旋流器29中,其将浆料料流分成溢流料流和含催化剂的底流料流。浆料液体溢流料流经由导管26取出用于在第二分离段中分离催化剂细粒和根据需要用于另外的加工。本体催化剂经由导管25返回浆料液体的底部区域。
在图3所示的另一且优选的实施方案中,将脱气的浆料经由管31从外部降液管的主垂直段(section)30中取出用于在液体-固体分离装置32,例如斜板分离器或水力旋流器中分离。液体经由管33除去以用于细粒分离和任何另外的加工,而本体催化剂经由管34返回於浆反应器中。
当然,如图4所示,任选可将浆料从内部降液管的主垂直段21中取出以用于类似于图3的分离和其它处理。
如本文所述,通过以非均相方法操作淤浆法,简化了液体-固体分离。事实上,本发明使得可取消使用过滤器而将固体从由浆料泡罩塔中取出的液体中分离。这通过降低送入液体-固体分离的浆料中的固体浓度而进行。
实施例
於浆反应器***的计算机模型用于说明作为浆料床高度的函数,浆料床中固体催化剂分布。该模型将反应动力学与浆料气泡流体动力学结合。在进行该计算中,向模型提供进料组合物、反应温度和压力、催化剂类型、密度和粒度分布,和反应器几何形状。测定塌落床操作和分散床操作的催化剂浓度并图示于图5中。可以看出,当反应器高度提高时,以塌落床模式操作能实现比约20重量%小得多的催化剂浓度。相同效果也可通过降低反应器降液管高度实现。在图5中可以看出,一旦浆料水平在降液管高度以上,在该实施例中为66英尺,以分散床操作的浆料催化剂浓度就开始快速降低。
Claims (17)
1.一种在三相淤浆法中将浆料液体与催化剂分离的方法,所述方法包括:
在足以提供其中浆料固体浓度为低于20重量%的在浆料床中的上部区域和其中浆料中固体浓度为高于20重量%催化剂的在所述床中的下部区域的条件下操作淤浆法;
将浆料床上部区域中的一部分浆料脱气;
将脱气的浆料引入分离装置中以提供基本包含浆料液体的液体料流和包含催化剂颗粒的料流;和
使包含催化剂颗粒的料流返回浆料床。
2.根据权利要求1的方法,其中所述三相淤浆法在塌落床条件下操作。
3.根据权利要求1的方法,其中所述三相淤浆法在具有一个或多个浆料循环降液管的反应器中在以形成高度高于降液管高度的浆料床的条件下操作,由此提供其中浆料含20重量%或更少催化剂的在浆料床中的上部区域。
4.根据权利要求2或3的方法,其中将所述浆料在具有位于浆料床上部区域中的顶端和延伸至浆料床下部区域中的主段的降液管中脱气。
5.根据权利要求4的方法,其中将脱气的浆料从降液管的顶端取出以引入分离装置中。
6.根据权利要求4的方法,其中将脱气的浆料从降液管的主段中取出以引入分离装置中。
7.一种用于在三相淤浆法中将浆料液体与催化剂分离的***,所述***包含:
用于含浆料液体和催化剂颗粒的立式反应器,所述反应器具有顶部和底部;
用于将气体注入反应器底部的装置,其中在操作条件下,形成具有催化剂浓度为20重量%或更小的上部区域和催化剂浓度为高于20重量%或更大的下部区域的三相浆料;
位于浆料上部区域中用于将一部分浆料脱气的装置;
用于取出脱气的浆料并将它引入用于将浆料液体料流与催化剂颗粒分离的液体-固体分离装置中的导管装置;
用于将分离的浆料液体从所述分离装置中取出的导管装置;和
用于将分离的催化剂取出并输送至反应器中的导管装置。
8.根据权利要求7的***,其中用于将浆料脱气的装置包括具有顶杯部分和向下延伸的主段的降液管。
9.根据权利要求8的***,其中用于取出脱气的浆料的导管可操作地连接在降液管的顶端上。
10.根据权利要求8的***,其中用于取出脱气的浆料的导管可操作地连接在降液管的主段上。
11.根据权利要求8或10的***,其中所述降液管位于反应器内。
12.根据权利要求8或10的***,其中所述降液管的主段位于反应器外部。
13.根据权利要求11的***,其中分离装置包括斜板分离器。
14.根据权利要求11的***,其中分离装置包括水力旋流器。
15.根据权利要求12的***,其中分离装置包括斜板分离器。
16.根据权利要求12的***,其中分离装置包括水力旋流器。
17.根据权利要求7的***,其包括具有位于三相浆料上部区域以下的顶端的一个或多个浆料循环降液管。
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US20352508P | 2008-12-23 | 2008-12-23 | |
US61/203,525 | 2008-12-23 | ||
US12/592,168 US8119014B2 (en) | 2008-12-23 | 2009-11-20 | Systems and methods to remove liquid product and fines from a slurry reactor |
US12/592,168 | 2009-11-20 | ||
PCT/US2009/006708 WO2010074762A1 (en) | 2008-12-23 | 2009-12-23 | Systems and methods to remove liquid product and fines from a slurry reactor |
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CN102292416B true CN102292416B (zh) | 2014-04-16 |
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EP (1) | EP2379675A1 (zh) |
CN (1) | CN102292416B (zh) |
AU (1) | AU2009330672B2 (zh) |
WO (1) | WO2010074762A1 (zh) |
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US8389585B2 (en) * | 2009-02-13 | 2013-03-05 | Exxonmobil Research And Engineering Company | Slurry reactor fines segregation and removal |
US8894939B2 (en) * | 2010-08-16 | 2014-11-25 | Emerging Fuels Technology, Inc. | Three phase reactor |
CN102773050B (zh) * | 2012-08-14 | 2014-05-28 | 迈瑞尔实验设备(上海)有限公司 | 一种固液分离循环的结构及方法 |
CN103977747B (zh) * | 2013-02-08 | 2018-01-30 | 上海碧科清洁能源技术有限公司 | 浆态床反应器及用该浆态床反应器进行浆态床反应的方法 |
WO2014121722A1 (en) * | 2013-02-08 | 2014-08-14 | Shanghai Bi Ke Clean Energy Technology Co., Ltd. | A slurry-bed reactor and method of use |
CN103170284B (zh) * | 2013-04-03 | 2016-02-17 | 神华集团有限责任公司 | 高温、高压浆态床反应器费托合成***及其工艺 |
CN103263790A (zh) * | 2013-04-27 | 2013-08-28 | 北京市环境卫生设计科学研究所 | 生活垃圾三相分离方法和通风风帽 |
CN104549064A (zh) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | 一种浆态床反应装置及其应用 |
BR112018003216B1 (pt) * | 2015-08-19 | 2022-04-19 | Sasol Technology Proprietary Limited | Método para partida de um reator de coluna com bolhas de lama |
EP3235560A1 (de) | 2016-04-22 | 2017-10-25 | Evonik Röhm GmbH | Verfahren zur durchführung einer heterogen-katalysierten reaktion |
CN107720959B (zh) * | 2017-11-23 | 2020-08-04 | 青岛理工大学 | 一种气液固三相分离器 |
CN111036150B (zh) * | 2019-12-02 | 2023-07-25 | 河南金鹏化工有限公司 | 一种硫双威醇洗连续化生产工艺及装置 |
CN111905659B (zh) * | 2020-08-24 | 2022-04-19 | 中国科学院青岛生物能源与过程研究所 | 一种浆态床清洁液体的采出方法及采出装置 |
EP4371660A1 (en) * | 2022-11-21 | 2024-05-22 | Röhm GmbH | Method for preparing a catalyst for the production of methyl methacrylate using clarification |
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- 2009-12-23 EP EP09796162A patent/EP2379675A1/en not_active Withdrawn
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CN102292416A (zh) | 2011-12-21 |
AU2009330672A1 (en) | 2011-07-21 |
AU2009330672B2 (en) | 2014-11-27 |
US20100160460A1 (en) | 2010-06-24 |
EP2379675A1 (en) | 2011-10-26 |
WO2010074762A1 (en) | 2010-07-01 |
US8119014B2 (en) | 2012-02-21 |
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