CN101959996B - 用于气化作用的颗粒状组合物及其制备和连续转化 - Google Patents
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Abstract
提供了用于捕获和再循环在气化过程期间所产生的碳质细粒的方法。特别是,将再循环的细粒加工成颗粒状组合物,其可用作碳质原料并且被转化成包括甲烷的气流。
Description
发明领域
本发明涉及包括从气化反应回收的碳质细粒的颗粒状组合物。本发明还涉及一种用于制备含有颗粒状组合物的碳质原料的方法。本发明进一步涉及一种用于通过气化作用将颗粒状组合物转化成多种气态产品的连续方法。
发明背景
由于很多因素例如较高的能源价格和对环境的关切,由较低燃烧值的碳质原料,例如生物质、煤和石油焦炭生产增值的气态产品,正日益受到更新的关注。用来生产甲烷及其它增值气体的这类材料的催化气化被公开在例如US3828474、US3998607、US4057512、US4092125、US4094650、US4204843、US4468231、US4500323、US4541841、US4551155、US4558027、US4606105、US4617027、US4609456、US5017282、US5055181、US6187465、US6790430、US6894183、US6955695、US2003/0167961A1、US2006/0265953A1、US2007/000177A1、US2007/083072A1、US2007/0277437A1和GB1599932中。
较低燃烧值碳质原料在上述参考文献所述的条件下反应典型地产生粗制品气体和炭。该粗制品气体典型地包括一定量的夹带的碳质细粒,其被从气流中除去。许多以前知道的方法对于除去碳质细粒是有效的。典型地这些细粒不可直接使用,其在工业规模上可总计达到显著量的潜在有害废物及相关清理成本。因此,碳质细粒废物的处理、储存及清理操作代表了工业的一个显著的非生产性的成本。
因此,需要允许回收、再循环碳质细粒(例如在碳质原料气化后来自气体排出物的夹带的碳质细粒)并将其最终转化成可用原料来产生气体产物的改进方法和组合物。
发明概述
在第一方面中,本发明提供一种颗粒状组合物,其具有适用于流化床区域中的气化的粒度分布,该颗粒状组合物包括(a)具有小于约45微米的平均粒度的碳质细粒材料;(b)具有适用于流化床区域中的气化的 粒度分布的颗粒状碳质原料;以及(c)气化催化剂的紧密混合物,该催化剂在适当温度和压力并且存在蒸汽的条件下表现出气化活性,藉此包括甲烷以及氢气、一氧化碳、二氧化碳、硫化氢、氨气及其它高级烃中的一种或多种的多种气体由该颗粒状组合物形成,其中:(1)所述的碳质细粒材料和所述的颗粒状碳质原料以约为1∶99至99∶1的重量比存在于所述的颗粒状组合物中;(2)所述的碳质细粒材料与所述的颗粒状碳质原料以物理方式缔合;(3)所述的碳质细粒材料和所述的颗粒状碳质原料各自包括一种气化催化剂;(4)并且该气化催化剂包括至少一种碱金属源并且其存在量足以在颗粒状组合物中提供在0.01-约0.08范围内的碱金属原子与碳原子的比率。
在第二方面中,本发明提供一种用于制备具有适用于流化床区域中的气化的粒度分布的颗粒状组合物的方法,该方法包括以下步骤:a)提供具有小于约45微米的平均粒度并且包括气化催化剂的颗粒状碳质细粒材料;(b)提供具有适用于流化床区域中的气化的粒度分布的颗粒状碳质原料;(b)使该颗粒状碳质原料与含有气化催化剂的水性介质接触而形成浆料;(c)使该浆料脱水而形成湿饼;(d)将所述的颗粒状碳质细粒材料与所述的湿饼混合而形成湿颗粒状组合物;以及(e)使用干燥的惰性气体对该湿的颗粒状组合物进行热处理以形成颗粒状组合物,其中所述的气化催化剂包括至少一种碱金属源并且其存在量足以在颗粒状组合物中提供在0.01-约0.08范围内的碱金属原子与碳原子的比率。
在第三方面中,本发明提供一种用于将碳质原料转化成多种气态产品的连续方法,该方法包括以下步骤:(a)根据第一方面或根据第二方面的方法来制备颗粒状组合物;(b)将该颗粒状组合物供给气化反应器,该气化反应器包括内部细粒去除器、外部细粒去除器或两者,用于去除气体夹带的细粒材料;(c)使气化反应器中的颗粒状组合物在适当的温度和压力并且存在蒸汽的条件下进行反应而形成第一气流,该气流包括(i)包括甲烷以及氢气、一氧化碳、二氧化碳、硫化氢、氨气及其它高级烃中的至少一种或多种的多种气体产品;以及(ii)气体夹带的碳质细粒材料;(d)将气体夹带的碳质细粒材料至少部分地捕获在内部细粒去除器、外部细粒去除器或两者中;(e)从细粒去除器、外部细粒去除器、或两者中回收所捕获的碳质细粒材料;以及(f)使所捕获的碳质细粒材料再循环到步骤(a)的颗粒状组合物的制备中。
详细说明
本发明涉及具有适用于流化床区域中的气化的粒度分布的颗粒状组合物,该颗粒状组合物包括颗粒状碳质原料、从气化反应中回收的碳质细粒材料以及气化催化剂,该气化催化剂在适当温度和压力并且存在蒸汽的条件下能够通过气化反应被转化成多种气体。本发明还涉及用于制备用于气化的颗粒状组合物的方法,其中该颗粒状组合物包括颗粒状碳质原料和从气化反应回收的碳质细粒材料以及气化催化剂,并将这些组分混合。本发明进一步涉及用于将碳质原料转化成多种气态产品的连续方法,该方法包括气化反应器,该气化反应器包括内部和外部碳质细粒去除器、从内部和外部碳质细粒去除器中捕获并回收气体夹带的碳质细粒,用于制备可用作气化反应器的碳质原料的颗粒状组合物。
一般来说,碳质材料的气化产生粗制气流,其包括甲烷、二氧化碳、氢气、一氧化碳、硫化氢、氨气、未反应的蒸汽、夹带的细粒及其它污染物例如COS。通过那些本领域技术人员已知的清洁操作,将粗制气流进行处理以产生含有甲烷、氢气和一氧化碳的净化气流。甲烷可以被用作完全燃烧的高值燃料。从该气流中除去夹带的细粒后,用于提纯粗制气流的分离方法特别地产生碳质细粒副产品。通常这些碳质细粒被认为是废物,但是对这些细粒的处理是昂贵的和能量效率低的。在此描述的方法和组合物为节能装置提供回收并再循环的碳质细粒,该碳质细粒是从粗制气流中的气体夹带的碳质细粒中分离出来的,该粗制气流来自气化反应器内碳质原料的气化。
例如,可以利用以下共同拥有的US2007/0000177A1、US2007/0083072A1和US2007/0277437A1;以及美国专利申请系列号12/178,380(2008年7月23日提交的)、12/234,012(2008年9月19日提交的)和12/234,018(2008年9月19日提交的)中所公开的任何催化气化技术的发展来实施本发明。在此通过参考文献将以上全部引入用于所有目的,就象全部提出一样。
此外,可以结合以下美国专利申请的主题来实施本发明,其各自是在2008年12月28日提交的:系列号12/342,554,名称为“具有由焦炭回收碱金属的催化气化方法”;系列号12/342,565,名称为“用于催化气化的石油焦炭组合物”;系列号12/342,578,名称为“用于催化气化的煤组合物”;系列号12/342,596,名称为“制造合成气及合成气衍生产品的 方法”;系列号12/342,608,名称为“用于催化气化的石油焦炭组合物”;系列号12/342,628,名称为“制造合成气衍生产品的方法”;系列号12/342,663,名称为“碳质燃料及其制造方法和用途”;系列号12/342,715,名称为“具有由炭回收碱金属的催化气化方法”;系列号12/342,736,名称为“具有由炭回收碱金属的催化气化方法”;系列号12/343,143,名称为“具有由炭回收碱金属的催化气化方法”;系列号12/343,149,名称为“用于碳质原料的催化气化的产生蒸汽的淤浆气化器”;系列号12/343,159,名称为“用于将碳质原料转化成气体产品的连续方法”。在此通过参考文献将以上全部引入用于所有目的,就象全部提出一样。
进一步地,可以结合以下美国专利申请的主题来实施本发明,其各自与此同时提交:系列号___________,名称为“用于制造吸附剂的方法及用于利用其从液体中除去污染物的方法”(代理人案号FN-0019 US NP1);系列号________________,名称为“利用生物质原料的蒸汽生产方法”(代理人案号FN-0020 US NP1);系列号______________,名称为“减少碳脚印的蒸汽生产方法”(代理人案号FN-0021 US NP1);系列号______________,名称为“用于从气流中分离甲烷的方法和装置”(代理人案号FN-0022 US NP1);系列号________________,名称为“从气化产物中选择性除去和回收酸性气体”(代理人案号FN-0023 US NP1);系列号_______________,名称为“用于催化气化的煤组合物”(代理人案号FN-0024 US NP1);系列号______________,名称为“用于催化气化的煤组合物”(代理人案号FN-0025 US NP1);系列号________________,名称为“用于煤催化气化的作为补充催化剂来源的生物质的共进料”(代理人案号FN-0026 US NP1);系列号_____________,名称为“压实器-进料器”(代理人案号FN-0027 US NP1);系列号_____________,名称为“用于催化气化的生物质碳组合物”(代理人案号FN-0029 US NP1);系列号________________,名称为“催化气化颗粒状组合物”(代理人案号FN-0030US NP1);以及系列号__________________,名称为“用于催化气化的生物质组合物”(代理人案号FN-0031 US NP1).在此通过参考文献将以上全部引入用于所有目的,就象全部提出一样。
如果不另有指明,将在此提及的全部出版物、专利申请、专利及其它参考文献明确地通过参考文献全部引入用于所有目的,就象全部提出一样。
除非另有定义,在此使用的全部技术和科学术语具有与本发明所属领域普通技术人员通常理解的相同的含义。在抵触的情况下,以本发明的说明书(包括定义)为准。
除了有明确的注解之处,商标以上标示出。
虽然在此描述了合适的方法和材料,但是与此处描述的那些类似或相同的方法和材料可在本发明的实践或试验中使用。
除非另外声明,所有百分比、份数、比率等都是以重量计。
当给出的量、浓度或其它值或参数为一个范围、或上下限值的列表时,这应该理解为明确公开了由任何上下范围极限的任何成对值所形成的全部范围,不管各范围是否被分别公开。当在此列举数值范围时,除非另外声明,该范围旨在包括其端点以及该范围内的所有整数和分数。当定义一个范围时,本发明的范围不打算限于所述特定值。
当在描述一个值或一个范围的端点中使用术语“约”时,本发明应该被理解为包括所提及的特定值或端点。
如在此所使用的那样,术语“包括”、“包含”、“含有”、“含”、“具有”、“有”或其任何其它变型,旨在覆盖非排它性的包含。例如,包括一系列元素的过程、方法、制品或装置不一定仅限于那些元素,而是可包括未明确地列出的该过程、方法、制品或装置或固有的其它元素。此外,除非明确的相反声明,“或”是指可兼的逻辑或而不是指互斥或。例如,条件A或B满足以下任一项:A是真的(或存在)并且B是假的(或不存在),A是假的(或不存在)并且B是真的(或存在),以及A和B两者都是真的(或存在)。
在此使用“一种”或“一个”来描述各种元素和组件只是为了方便起见和给出本发明的一般意义。该说明应该被阅读为包括一种或至少一种并且该单数还包括复数,除非显然它是别的意思。
这里的材料、方法及实施例仅仅是举例说明性的,并且除了明确声明的以外,并不打算作为限制。
碳质细粒的回收
本发明涉及在气化期间回收的碳质细粒材料,其以气体夹带的碳质细粒形式存在于气化反应器和离开气化反应器的粗制气流中。在一方面中,本发明提供包括碳质细粒材料、不是碳质细粒并且适用于在流化床区域中气化的颗粒状碳质原料以及气化催化剂的颗粒状组合物。该颗粒 状组合物具有适用于气化的粒度分布。该气化催化剂可以是如此处所述的任何已知的气化催化剂。在一种实施方式中,该催化剂包括至少一种碱金属源,其量为可提供在约0.01-约0.08范围内的碱金属原子与碳原子的比率。
为了本发明目的,术语“碳质细粒”、“夹带的碳质细粒”或“气体夹带的碳质细粒”材料是指在气化过程期间由碳质原料产生的碳质颗粒,其为未反应的或残余的碳质颗粒(即没有完全参与气化反应的颗粒)。夹带的碳质细粒材料衍生自气化过程,例如以上所述,并且存在于气化反应器内和粗制品气流中。有利地,碳质细粒材料包括气化催化剂,其由先前的碳质原料的催化剂加料步骤提供,碳质细粒材料是从该碳质原料产生的。碳质细粒材料可大小不同,通常平均粒度为约45微米或更小,并且通常主要在约5微米-约50微米,或约10微米-约45微米的范围内。
在气化过程期间所产生的气体夹带的碳质细粒材料(例如在气化反应器和粗产品气体混合物内)可通过本领域通常实践的任何方法捕获。例如,在工业流化床反应器中通常采用分离器,例如一对或多对旋风分离器,每对都具有排入第二旋风分离器的第一旋风分离器。粗产品气体进入第一旋风分离器,在此捕获了大部分夹带的细粒。第一旋风分离器出口排入第二旋风分离器,其携带了在第一旋风分离器中逃避捕获的大部分微细尺寸的颗粒。可选择地,利用颗粒捕获设备可捕获该气体夹带的碳质细粒材料,该颗粒捕获设备例如是湿气体洗涤器(例如文丘里洗涤器);第三旋风分离器;沉淀器;包括例如静电沉淀器;本领域已知的筛眼材料,例如黄铜、铜、铝、钢、铁丝网和镀锌丝,筛孔尺寸为7-500(Screen Technology Group,Inc.,Washougal,WA);或过滤器,包括例如陶瓷、金属或袋式过滤器(参见US7309383和US2934494)。在捕获之后,可通过重力和低速气流的组合将碳质细粒材料输送到收集容器,并且将其储存直到用于制造本发明的颗粒状组合物。
在一种实施方式中,将碳质细粒材料从存在于由气化反应器排出的粗制气流中的气体夹带的细粒中分离出来。在该实施方式中,例如旋风分离器可位于气体反应器的内部或外部、或位于内部和外部两者,任选地后面跟着一个或多个文丘里洗涤器、第三旋风分离器和/或烛形滤器。
包含再循环的细粒及其它碳质材料的颗粒状组合物
在一个方面中,将再循环的碳质细粒材料用于形成本发明的颗粒状组合物。该颗粒状组合物具有适用于流化床区域中的气化的粒度分布,并且包括至少两种类型的碳质材料的混合物。第一种碳质材料是从此处所述的气化反应中回收的碳质细粒材料。第二种碳质材料是可衍生自此处所述的任何碳质组合物的颗粒状碳质原料材料,包括生物质。该颗粒状组合物包括气化催化剂,其量能有效地允许组合物在适当温度和压力下气化。在一种实施方式中,碳质细粒材料和颗粒状碳质原料在颗粒状组合物中以约为5∶95-95∶5的重量比存在。
包括至少一些量的碳质细粒材料的颗粒状组合物可用作碳质气化原料。在气化过程期间,当该颗粒状组合物与不包含碳质细粒材料的原料相比时,其具有更好的流体性能。在一种实施方式中,碳质细粒材料与颗粒状(非细粒)碳质原料的重量比为从约1∶99或从约5∶95或从约1∶10,到约99∶1或到约95∶5或到约10∶1或到约5∶1或到约1∶1或到约1∶2或到约1∶5。
在此所采用的术语“碳质组合物”、“碳质原料”、“颗粒状碳质原料”或“碳质材料”包括碳源,典型地包括煤、石油焦炭、沥青烯和/或液体石油残留物,但可广泛地包括适用于气化的任何碳源,包括生物质。许多颗粒状碳质原料将一般地包括至少一些灰分,典型地包括至少约3wt%的灰分(基于碳质组合物的重量),虽然某些含有非常少的灰分,如下所示。
在此所采用的术语“石油焦炭”包括(i)石油加工中所得的高沸点烃类馏分的固体热分解产物(重质残留物-“残留的石油焦炭”)以及(ii)加工焦油砂的固体热分解产物(沥青砂或含油砂-“焦油砂石油焦炭”)。该碳化产物包括例如新鲜的、煅烧的、针状的和流化床石油焦炭。
例如,通过用于升级高比重残余原油的焦化过程,可由原油得到残留的石油焦炭,该石油焦炭含有灰分作为微量组分,基于该焦炭的重量,其典型地为约1.0wt%或更少,并且更典型地为约0.5wt%或更少。典型地,在该低灰分焦炭中的灰分主要包括金属例如镍和钒。
焦油砂石油焦炭可得自油砂,例如通过用于升级油砂的焦化过程得到。焦油砂石油焦炭含有灰分作为微量组分,基于该焦油砂石油焦炭的重量,其典型地在约2wt%-12wt%的范围内,并且更典型地在约4wt%-12wt%的范围内。典型地,该高灰分焦炭中的灰分主要包括几种材 料例如硅和/或铝的混合物。
基于石油焦炭的总重量,该石油焦炭可包括至少约70wt%的碳、至少约80wt%的碳或至少约90wt%的碳。典型地,基于石油焦炭的重量,该石油焦炭包括小于约20wt%的无机化合物。
在此所使用的术语“沥青烯”是在室温下的芳族碳质固体,并且可得自例如原油和原油焦油砂的加工。
在此所使用的术语“液体石油残留物”包括(i)在石油加工中得到的高沸点烃类馏分的液体热分解产物(重质残留物-“残留液体石油残留物”)以及(ii)加工焦油砂的液体热分解产物(沥青砂或含油砂-“焦油砂液体石油残留物”)两者。该液体石油残留物大体上是非固体的;例如其呈现为粘稠液体或泥浆的形式。
残留液体石油残留物还可得自原油,例如通过用于升级高比重原油蒸馏残留物的方法。该液体石油残留物含有灰分作为微量组分,基于残留物的重量,其典型地为约1.0wt%或更少,并且更典型地为约0.5wt%或更少。典型地,在该低灰分残留物中的灰分主要包括金属例如镍和钒。
焦油砂液体石油残留物可得自油砂,例如通过用于升级油砂的方法。焦油砂液体石油残留物含有灰分作为微量组分,基于残留物的总重量,其通常在约2wt%-12wt%的范围内,并且更通常在约4wt%-12wt%的范围内。通常,在该高灰分残留物中的灰分主要包括几种材料例如硅和/或铝的混合物。
在此所使用的术语“煤”是指泥炭、褐煤、次烟煤、烟煤、无烟煤或其混合物。在某些实施方式中,基于煤总重量,以重量计,该煤的碳含量小于约85%、或小于约80%、或小于约75%、或小于约70%、或小于约65%、或小于约60%、或小于约55%、或小于约50%。在其它实施方式中,基于煤总重量,以重量计,该煤的碳含量范围在至多约85%、或至多约80%、或至多约75%。可使用的煤的例子包括(但不限于)伊利诺伊#6、匹兹堡#8、勃朗(ND)、犹他盲峡谷和波德河盆地(PowderRiver Basin)(PRB)煤。通过在干燥的基础上煤的总重量,无烟煤、烟煤、次烟煤和褐煤可分别包括约10wt%、约5-7wt%、约4-8wt%以及约9-11wt%的灰分。然而,任何特定煤源的灰分含量将取决于该煤的等级和来源,正如那些本领域技术人员所熟悉的那样[例如,参见CoalData:A Reference,Energy Information Administration,Office of Coal, Nuclear,Electric and Alternate Fuels,U.S.Department of Energy,DOE/EIA-0064(93),February 1995]。
在此所使用的术语“灰分”包括存在于碳源内的无机化合物。该灰分典型地包括硅、铝、钙、铁、钒、硫等的化合物。该化合物包括无机氧化物,例如二氧化硅、氧化铝、氧化铁等,但也可包括多种矿物,该矿物含有硅、铝、钙、铁和钒中的一种或多种。术语“灰分”可用于指在气化之前存在于碳源中的这样的化合物,也可用于指在气化后存在于炭中的这样的化合物。
催化气化方法
本发明的再循环和回收方法特别可用于用于将碳质原料例如石油焦炭、液体石油残留物和/或煤转化成可燃气体例如甲烷的联合气化方法中。用于该方法的气化反应器典型地是在中等高的压力和温度下运行的,需要将碳质材料(即原料)引入气化反应器的反应区,同时保持所需温度、压力及原料的流速。那些本领域技术人员对于将原料提供给高压和/或高温环境的进料系统是熟悉的,其包括星形加料器、螺杆加料器、旋转柱塞和闭锁料斗。应该理解的是该进料系统可包括两个或更多个压力平衡的元件,例如闭锁料斗,可将其交替使用。
将催化的原料从原料制备操作提供给催化气化炉,如下所述。在某些例子中,可以在气化反应器的操作压力以上的压力条件下制备颗粒状组合物,因此,该颗粒状组合物可在没有进一步增压下被直接传入气化反应器。
可利用几种催化气化炉中的任一种。合适的气化反应器包括逆流固定床、并流固定床、流化床、夹带流和移动床反应器。用于使液体进料(例如液体石油残留物)气化的催化气化器被公开于先前引入的US6955695中。
典型地让气化反应器在至少约450℃或至少约600℃或以上,到约900℃或到约750℃或到约700℃的中等温度;以及在至少约50psig或至少约200psig或至少约400psig,到约1000psig或到约700psig或到约600psig的压力下运行。
用于颗粒状组合物的增压和反应的气化反应器中所利用的气体典型地包括蒸汽以及任选地包括氧气或空气,并且根据那些本领域技术人员已知的方法将其供给反应器。例如那些本领域技术人员已知的任何蒸 汽锅炉可将蒸汽供给该反应器。可将动力供给该锅炉,例如通过采用任何碳质材料例如粉煤、生物质等,并且包括(但不限于)从颗粒状组合物制备操作中抛弃的碳质材料(例如细粒,同上)。也可从连接到燃气轮机的第二气化反应器供给蒸汽,来自反应器的排气在该燃气轮机中被热交换成水源并产生蒸汽。另一方面,可将蒸汽提供给气化反应器如在先引入的美国专利申请,系列号______________,名称为“利用生物质原料的蒸汽形成方法”(代理人案号FN-0020 US NP1),以及系列号.________________,名称为“减少碳脚印的蒸汽形成方法”(代理人案号FN-0021US NP1)中所描述的那样。
来自其它加工操作的再循环的蒸汽也可用于将蒸汽供给反应器。例如,在催化原料的制备中,当采用流化床淤浆干燥机来干燥浆状颗粒状组合物时,如下所述,则所产生的蒸汽可被进料到催化气化反应器。
用于催化煤气化反应的少量所需热量输入可通过本领域技术人员已知的任何方法通过过度加热进料到气化反应器的蒸汽与再循环气的气体混合物而被提供。在一种方法中,可将压缩的(CO和H2)的再循环气与蒸汽混合并且可通过与气化反应器流出物热交换,紧接着在循环气体炉中过度加热来进一步过度加热所得的蒸汽/循环气混合物。
可以在该方法中包含甲烷重整装置,以补充进料到反应器的循环CO和H2,以确保将充足的循环气供给反应器,使得反应的净热尽可能地接近于中性(仅稍微发热或吸热),换句话说,该反应是在热中性条件下进行的。在该情形中,由甲烷产物可将甲烷供给重整装置,如下所述。
颗粒状组合物在所述条件下的反应典型地提供了粗制产品气体和炭。典型地从气化反应器中除去在本发明的方法期间在气化反应器中所制得的炭以便取样、清洗和/或催化剂回收。除去炭的方法是那些本领域技术人员所熟知的。例如可采用EP-A-0102828所教导的一种这样的方法。该炭可以通过闭锁料斗系统从气化反应器中周期性地取出,虽然其它方法对于本领域技术人员来说是已知的。
用循环气和水可将炭猝灭并将其导向催化剂再循环操作,用于提取和再利用该碱金属催化剂。特别有用的回收和再循环方法被描述在US4459138中、也被描述在前面引入的US4057512和US2007/0277437A1中以及前面引入的美国专利申请系列号12/342,554, 12/342,715、12/342,736和12/343,143中。对于进一步方法的细节,可参考那些文件。
离开气化反应器的粗制产品气体流出物可穿过气化反应器的一部分,其用作分离区,在此处使太重以至于不能被夹带在离开气体反应器的气体中的颗粒(即非气体夹带的细粒材料)返回流化床。该分离区可包括一个或多个内部旋风分离器或用于从气体中除去气体夹带的碳质细粒材料及其它颗粒的类似装置。穿过分离区并离开气化反应器的粗制气流出气流一般含有CH4、CO2、H2和CO、H2S、NH3、未反应的蒸汽、气体夹带的细粒及其它污染物例如COS。
然后,可以让已经从中除去了细粒的气流穿过热交换器来冷却该气体,并且可以使用回收的热来预先加热循环气并且产生高压蒸汽。如上所述,可以通过任何适当的装置例如外部旋风分离器,任选地后面跟着文丘里洗涤器来除去残余的气体夹带的碳质细粒。除了将部分回收的碳质细粒再循环到原料的制备中之外,还可将其加工以回收碱金属催化剂。
可以将已经从中除去了细粒的气流进料到COS水解反应器(发酵过程),用于除去COS并将其在热交换器中进一步冷却以在进入水洗器回收氨之前回收残余的热,产生至少包括H2S、CO2、CO、H2和CH4的洗涤后的气体。用于COS水解的方法对于本领域技术人员来说是已知的,例如参见US4100256。
来自洗涤后的气体的残余的热可用于产生低压蒸汽。可将洗涤水和发酵过程冷凝物加工以解吸并且回收H2S、CO和NH3;这样的加工对于本领域技术人员来说是众所周知的。典型地可以以水溶液形式(例如20wt%)回收NH3。
可以使用后续的酸性气体去除过程通过涉及对气体进行溶剂处理的物理吸收方法来从纯气流中除去H2S和CO2以提供净化的气流。该方法包括使洗涤后的气体与溶剂接触,该溶剂例如是单乙醇胺、二乙醇胺、甲基二乙醇胺、二异丙胺、二甘醇胺、氨基酸的钠盐溶液、甲醇、热碳酸钾等等。一种方法可包括采用 (UOP LLC,Des Plaines,IL USA)或 (Lurgi AG,Frankfurt am Main,Germany)溶剂,该溶剂具有两个系列;每个系列由一种H2S吸收剂和一种CO2吸收剂组成。含有H2S、CO2及其它污染物的用过的溶剂可通过本领域技术人员 已知的任何方法再生,这些方法包括使用过的溶剂与蒸汽或其它解吸气接触以除去污染物,或使失去效能的溶剂通过解吸塔。所回收的酸性气体可被送去进行硫磺回收处理,例如从酸性气体去除及酸性水解吸中回收的任何H2S可通过本领域技术人员已知的任何方法(包括克劳斯工艺(Claus process))转化成单质硫。可以以熔融的液体形式回收硫。可引导解吸过的水再循环用于第一和/或第二碳质原料的制备。一种用于从纯气流中除去酸性气体的方法被描述在前面引入的系列号为___________的美国专利申请中,名称为“从气化产物中选择性除去和回收酸性气体”(代理人案号FN-0023 US NP1)。
通过那些本领域技术人员已知的任何适当的气体分离方法可将净化的气流进一步加工以分离和回收CH4。该方法包括(但不限于)低温蒸馏和采用分子筛或陶瓷膜。一种用于从净化气流中分离和回收甲烷的方法被描述在前面引入的美国专利申请系列号____________中,名称为“用于从气流中分离甲烷的方法和装置”(代理人案号FN-0022 US NP1)。
典型地,由气体分离过程可以产生两种气流:甲烷产物流和合成气流(H2和CO)。可将该合成气流压缩并再循环到气化反应器中。如果必要的话,可将部分甲烷产物引导到重整装置,如先前所述,和/或将部分甲烷产物用作工厂燃料。
负载催化剂的碳质原料
通常的颗粒状组合物装载一定量的碱金属化合物。典型地,组合物中的碱金属化合物的量足以提供范围从约0.01或从约0.02或从约0.03或从约0.04,到约0.06或到约0.07或到约0.08的碱金属原子与碳原子的比率。此外,基于质量,典型地将碱金属装载到碳源上以达到碱金属含量为比碳质材料(例如煤和/或石油焦炭)中混合灰分含量多约3倍至约10倍。
适合用作气化催化剂的碱金属化合物包括选自由以下组成的组的化合物:碱金属碳酸盐、重碳酸盐、甲酸盐、草酸盐、氨基化物、氢氧化物、乙酸盐、卤化物、硝酸盐、硫化物及多硫化物。例如,该催化剂可包括Na2CO3、K2CO3、Rb2CO3、Li2CO3、Cs2CO3、NaOH、KOH、RbOH或CsOH、并且特别是碳酸钾和/或氢氧化钾中的一种或多种。
可以使用那些本领域技术人员已知的任何方法来使一种或多种气化催化剂与颗粒状组合物缔合。该方法包括(但不限于)与固体催化剂源混合并且使该催化剂浸渍到碳质材料上。那些本领域技术人员已知的几种浸渍方法可以被用于引入气化催化剂。这些方法包括(但不限于)始润浸渍法、蒸发浸渍法、真空浸渍法、浸入浸渍法以及这些方法的组合。通过用催化剂溶液(例如水溶液)使其成泥浆状态,可将气化催化剂浸入碳质材料(例如颗粒状碳质原料)中。
在某些例子中,可以提供第二催化剂(例如共催化剂)或其它添加剂;在这样的例子中,可在单独的加工步骤中对该颗粒进行处理以提供该催化剂和共催化剂/添加剂。例如,可以提供主要的气化催化剂(例如钾和/或钠源),接着是分离处理以提供共催化剂源。
例如,然后可以将具有适合在气化反应器中使用的粒度的颗粒状碳质原料部分进一步加工,以通过本领域技术人员已知的方法,例如,前面引入的US4069304、US4092125、US4468231、US4551155和US5435940中所公开的;以及前面引入的系列号为12/234,012、12/234,018、12/342,565、12/342,578、12/342,608和12/343,159的美国专利申请中所公开的方法,来浸渍一种或多种催化剂和/或共催化剂。
一种适用于将煤与气化催化剂混合以提供催化的碳质原料的特定方法,其中已经通过离子交换使催化剂与煤颗粒相缔合,该方法被描述在前面引入的系列号为12/178,380的美国专利申请中。使通过离子交换机制的催化剂装载最大化(基于专门针对煤发展的吸附等温线),并且控制保持湿润的附加催化剂(包括孔内的那些催化剂),使得以受控的方式获得总催化剂目标值。这种装载提供了呈湿饼形式的催化的煤颗粒。所装载的催化剂和脱水的湿煤饼典型地含有例如约50%水分。通过控制催化剂组分在溶液中的浓度以及接触时间、温度和方法,正如可以由那些相关领域中的普通技术人员根据起始煤的特性易于确定的那样,可以控制所装载的催化剂总量。
可以把催化原料储存以便将来使用或者将其转移到加料操作中以便引入气化反应器中。可以按照本领域技术人员已知的任何方法,例如螺杆输送器或气动传送器,把催化原料输送到储存或加料操作中。
用于制备颗粒状组合物的方法
在另一方面中,本发明提供了一种用于制备如上所述的颗粒状组合物的方法。该方法包括提供颗粒状的碳质原料(即,不同于碳质细粒)并使该材料与水性介质接触以形成浆料。在一种实施方式中,该水性介质可包括一定量的气化催化剂,并且其处于足以有效地将该催化剂装载到颗粒状碳质材料之上的条件下。使该浆料经历脱水步骤,其是利用本领域已知的任何方法来进行的,该方法例如是过滤(如鼓式过滤机)、 离心过滤、或高频振动床。该脱水步骤形成颗粒状碳质材料的湿饼。利用本领域已知的任何混合装置(例如商业混合器、挤出机或捏合机)将颗粒状碳质细粒材料和湿饼进行组合并且混合,其形成湿的颗粒状组合物。可通过任何已知的方法(例如热处理、使用惰性气体的热处理、过热蒸汽处理)将所得的湿颗粒状组合物干燥以形成本发明的颗粒状组合物,其为可用的碳质原料。虽然所得的颗粒状组合物的水分含量可以变化,但是在一种实施方式中,基于颗粒状组合物的重量,以重量计,干燥步骤提供水分含量为约10%或更少(即约9%或更少,约8%或更少,约7%或更少,约6%或更少,约5%或更少,约4%或更少,约3%或更少,约2%或更少,约1%或更少)的颗粒状组合物。在另一实施方式中,干燥步骤提供水分含量小于约4%重量的颗粒状组合物。
由于有利地给再循环的气体夹带的碳质细粒材料预装载了气化催化剂(即,来自在原料上进行的催化剂装载步骤,由其产生了细粒),只需要将气化催化剂装载到第二碳质原料(即颗粒状碳质原料)上。该气化催化剂可以包括本领域已知的并且如在此所述的任何气化催化剂,而且其存在量足以在颗粒状组合物中提供在0.01-约0.08范围内的碱金属原子与碳原子的比率。
用于将再循环细粒转化成气态产品的连续方法
本发明提供用于将碳质原料连续转化成多种气态产品的方法,其中该方法包括制备根据本发明或根据本发明的制备方法的颗粒状组合物。将该颗粒状组合物供给气化反应器,其中在气化过程期间产生气体夹带的碳质细粒,但其不经历气化。因此,这些气体夹带的碳质细粒还包括气化催化剂并可以被混入任何其它如下碳质原料中,也给该碳质原料装载气化催化剂而形成用于气化的原料,其包括再循环的碳质细粒。
供给气化反应器的颗粒状组合物的粒度范围为约10微米-约2500微米。
在这一方面,将碳质细粒材料用于通过一系列步骤使碳质原料转化成多种气体产品的连续方法中,这些步骤将在气化过程期间产生的夹带的碳质细粒回收和再循环。通过将初始碳质原料和气化催化剂供给配备有内部和/或外部细粒去除器的气化反应器,并使包括再循环的气体夹带的碳质细粒的碳质原料反应,产生了第一气流。如上所述,该气流包括气化反应的气体产物以及气体夹带的碳质细粒材料。利用内部和/或外部 细粒去除器将夹带的细粒材料从气体产物中分离出来,产生了包括主要量的气体产物的可回收气流。从内部和/或外部细粒去除器中回收所捕获的气体夹带的碳质细粒材料,其是未反应的并且装载了催化剂。一旦回收,可制得该碳质细粒材料以用于与另一种碳质原料混合,该另一种碳质原料包括除碳质细粒之外的碳质材料(例如颗粒状碳质原料材料)。典型地,所回收的碳质细粒在气化反应期间已经被干燥,并且包括气化催化剂。在某些实施方式中,可使所回收的碳质细粒经历另外的干燥步骤以除去来自回收过程的残留水分。除细粒之外的碳质材料在其与回收的碳质细粒混合之前或之后,可给其装载气化催化剂。在一种实施方式中,如此处所描述的,给除细粒之外的碳质材料装载气化催化剂,将其以湿滤饼形式回收并与回收的碳质细粒材料混合,例如通过捏合或类似的混合方法混合,并将其用于生产本发明的颗粒状组合物。“连续的”碳质原料包括一定量的回收的气体夹带的碳质细粒材料以保持稳态操作的气化效率。虽然该碳质原料可包括如此处所述的任何碳质材料,但在某些实施方式中,以本发明的颗粒状组合物的形式提供碳质原料和气化催化剂。如此处所述的,在该方法中所采用的气化催化剂的量可以改变,并且在某些实施方式中,该颗粒状组合物包括约15wt%的气化催化剂。
Claims (9)
1.一种颗粒状组合物,其具有适用于流化床区域中的气化的粒度分布,其特征在于该颗粒状组合物包括以下物质的紧密混合物:(a)具有小于45微米的平均粒度的碳质细粒材料;(b)具有适用于流化床区域中的气化的粒度分布的颗粒状碳质原料材料;以及(c)气化催化剂,该催化剂在适当温度和压力且存在蒸汽的条件下表现出气化活性,藉此由该颗粒状组合物形成多种气体,该多种气体包括甲烷,以及氢气、一氧化碳、二氧化碳、硫化氢、氨气及其它高级烃中的一种或多种,
其中:
(1)所述的碳质细粒材料和所述的颗粒状碳质原料材料以为1∶99至99∶1的重量比存在于所述的颗粒状组合物中;
(2)所述的碳质细粒材料与所述的颗粒状碳质原料材料以物理方式缔合;
(3)所述的碳质细粒材料和所述的颗粒状碳质原料材料各自包括所述气化催化剂;
(4)所述的气化催化剂包括至少一种碱金属源并且其存在量足以在颗粒状组合物中提供在0.01-0.08范围内的碱金属原子与碳原子的比率;以及
(5)所述组合物具有10微米-2500微米的粒度范围。
2.根据权利要求1中所述的颗粒状组合物,其特征在于所述碱金属包括钾、钠或两者。
3.根据权利要求1中所述的颗粒状组合物,其特征在于所述碱金属是钾。
4.根据权利要求1-3中任一项所述的颗粒状组合物,其特征在于所述碳质细粒材料包括主要在为5微米至50微米范围内的颗粒。
5.一种用于制备具有适用于流化床区域中的气化的粒度分布的颗粒状组合物的方法,其特征在于该方法包括以下步骤:
a)提供平均粒度小于45微米并且包括气化催化剂的颗粒状碳质细粒材料;
(b)提供具有适用于流化床区域中的气化的粒度分布的颗粒状碳质原料材料;
(c)使该颗粒状碳质原料材料与含有气化催化剂的水性介质接触而形成浆料;
(d)使该浆料脱水而形成湿饼;
(e)将颗粒状碳质细粒材料与该湿饼混合而形成湿颗粒状组合物;以及
(f)对该湿颗粒状组合物进行热处理以形成颗粒状组合物,
其中所述气化催化剂包括至少一种碱金属源并且其存在量足以在颗粒状组合物中提供在0.01-0.08范围内的碱金属原子与碳原子的比率,且所述组合物具有10微米-2500微米的粒度范围。
6.根据权利要求5中所述的方法,其特征在于所述气化催化剂包括钾、钠或两者。
7.根据权利要求5中所述的方法,其特征在于所述气化催化剂包括钾。
8.一种用于将碳质原料转化成多种气态产品的连续方法,其特征在于该方法包括以下步骤:
(a)制备根据权利要求1-4中任一项所述的颗粒状组合物或根据权利要求5-7中任一项所述的方法制备的颗粒状组合物;
(b)将所述颗粒状组合物供给气化反应器,该气化反应器包括内部细粒去除器、外部细粒去除器或两者,用于去除气体夹带的细粒材料;
(c)使气化反应器中的颗粒状组合物在适当的温度和压力并且存在蒸汽的条件下进行反应而形成第一气流,该气流包括
(i)包括甲烷,以及氢气、一氧化碳、二氧化碳、硫化氢、氨气及其它高级烃中的至少一种或多种的多种气体产物;以及
(ii)气体夹带的碳质细粒材料;
(d)将气体夹带的碳质细粒材料至少部分地捕获在内部细粒去除器、外部细粒去除器或两者中;
(e)从细粒去除器、外部细粒去除器或两者中回收所捕获的碳质细粒材料;以及
(f)使所捕获的碳质细粒材料再循环到步骤(a)的颗粒状组合物的制备中。
9.根据权利要求8中所述的方法,其特征在于在步骤(c)中形成炭,并且将该炭从所述的气化反应器中除去,并且将其送到催化剂回收和再循环工艺中,并且所述气化催化剂包括从所述催化剂回收和再循环工艺中回收的气化催化剂。
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