CN101910371A - 用于制备合成气衍生产物的方法 - Google Patents

用于制备合成气衍生产物的方法 Download PDF

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CN101910371A
CN101910371A CN200880122934.5A CN200880122934A CN101910371A CN 101910371 A CN101910371 A CN 101910371A CN 200880122934 A CN200880122934 A CN 200880122934A CN 101910371 A CN101910371 A CN 101910371A
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CN101910371B (zh
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E·T·罗宾逊
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Shunguan Investment Co., Ltd
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Abstract

描述了用于从由碳质材料的催化气化得到的焦炭中提取和回收碱金属的方法。在其他步骤中，本发明的方法包括水热沥滤步骤，其中用二氧化碳和蒸汽在升高的温度和压力下处理包括不可溶碱金属化合物的不可溶颗粒的浆液以实现将不可溶碱金属化合物转化为可溶碱金属化合物。此外，还描述了用于碳质材料的催化气化的方法，其中从由该催化气化方法得到的焦炭中提取和回收实质部分的碱金属。

Description

用于制备合成气衍生产物的方法
发明领域
本发明涉及用于制备合成气衍生产物的方法。
发明背景
由于多种因素(例如较高的能量代价和环境关注)，由较低燃料值的碳质原料(例如石油焦和煤)制备增值气态产物重新受到关注。例如在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中公开了此类材料制备甲烷和其他增值气体的催化气化。
合成气(即具有主要量的CO和H2的气体混合物)典型地用作其他方法(例如用于制备低级醇和醚以及烃质产物(例如费托柴油燃料和合成的原油(合成原油))的方法)的原料。合成气能由较低燃料值的原料利用例如气化方法形成。例如，在一种此类方法中，通过用氧气和蒸汽的混合物的部分氧化非催化地气化碳质原料；在该方法中燃烧约三分之一的原料以提供热量和压力，使该方法的能量效率相对较低。在另一种此类方法中，在催化气化之后是一个或多个低温分离步骤，以将该催化气化产物气体分离成甲烷和CO/H2部分。这些方法能够存在其相对能量密集的缺点。因此，需要能够更有效地由低燃料值碳质原料形成合成气衍生产物的方法。
发明概述
在一个方面，本发明提供了用于由碳质原料制备合成气衍生产物的方法，该方法包括以下步骤：(a)提供碳质原料；(b)在合成气形成区域中将该碳质原料至少部分转化为包含氢气和一氧化碳的合成气流；(c)将该合成气流输送到合成气反应区域；(d)将该合成气流在该合成气反应区域中进行反应以形成该合成气衍生产物和热能；(e)回收该合成气衍生产物；和(f)回收由该合成气流的反应生成的该热能。
在第二方面，本发明提供了用于由碳质原料制备合成气衍生产物的方法，该方法包括以下步骤：(a)提供碳质原料；(b)在合成气形成区域中将该碳质原料至少部分转化为包含氢气和一氧化碳的合成气流；(c)将该合成气流输送到合成气反应区域；(d)将该合成气流在该合成气反应区域中进行反应以形成该合成气衍生产物和可燃烧的尾气混合物；(e)回收该合成气衍生产物；和(f)燃烧该可燃烧的尾气混合物以提供热能。
附图简述
图1提供了依照本发明的一种实施方案用于制备合成气衍生产物的方法的示意图。
详细描述
本发明总的来讲涉及用于制备合成气衍生产物的方法。在图1中的流程图中显示了依照本发明的一个方面的方法的实施例。通常，在依照本发明的一种用于制备合成气的方法中，将碳质原料在合成气形成区域中至少部分转化为包括氢气和一氧化碳的合成气流。如下面更详细的描述，事实上能够使用任意方法将该碳质原料转化为合成气流，包括例如基于催化和非催化气化的方法。将该合成气流输送到合成气反应区域，在此处其进行反应以生成合成气衍生产物，将其回收用于进一步反应、加工或包装。该合成气流的反应还能生成热能，将其回收；或形成可燃烧的尾气混合物，将其燃烧以提供热能。如此产生的该热能能够用于多种应用中。例如，其能够用于(例如通过产生或加热蒸汽)碳质原料的转化中。该热能还能够用于发电，例如通过加热或产生蒸汽并驱动其通过涡轮。在本发明的另一实施方案中，该可燃烧的尾气用作用于重整炉中的补充燃料；这种整合特别有用，因为该可燃烧的尾气的量与该重整炉的燃烧任务成正比。因此，在本发明的该方面中，能够将合成气转化为可用的合成气衍生产物，同时能够释放、回收并利用在CO三键中储藏的能量，由此提高该方法的整体能量效率。
能够使用任意的例如在以下中公开的对催化气化技术的开发实施本发明：共同拥有的US2007/0000177A1、US2007/0083072A1和US2007/0277437A1；和美国专利申请序列号12/178,380(2008年7月23日提交)、12/234,012(2008年9月19日提交)和12/234,018(2008年9月19日提交)。而且，能够与以下美国专利申请(其各自都是与本申请同一日提交的)的主题相结合实施本发明的方法：名称为“PETROLEUM COKE COMPOSITIONS FOR CATALYTIC GASIFICATION”的序列号____(代理机构档案号FN-0008 USNP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的序列号____(代理机构档案号FN-0007 US NP1)；名称为“PETROLEUM COKE COMPOSITIONS FOR CATALYTIC GASIFICATION”的序列号____(代理机构档案号FN-0011 US NP1)；名称为“CARBONACEOUS FUELS AND PROCESSES FOR MAKING AND USING THEM”的序列号____(代理机构档案号FN-0013 USNP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的序列号____(代理机构档案号FN-0014 US NP1)；名称为“COAL COMPOSITIONS FOR CATALYTIC GASIFICATION”的序列号____(代理机构档案号FN-0009 US NP1)；名称为“PROCESSES FOR MAKING SYNTHESIS GAS AND SYNGAS-DERIVED PRODUCTS”的序列号____(代理机构档案号FN-0010 US NP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METALFROM CHAR”的序列号____(代理机构档案号FN-0015 USNP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的序列号____(代理机构档案号FN-0016 US NP1)；名称为“CONTINUOUS PROCESSES FOR CONVERTING CARBONACEOUS FEEDSTOCKINTO GASEOUS PRODUCTS”的序列号____(代理机构档案号FN-0018 US NP1)；和名称为“STEAM GENERATING SLURRY GASIFIER FOR THE CATALYTIC GASIFICAT1ON OF ACARBONACEOUS FEEDSTOCK”的序列号____(代理机构档案号FN-0017 US NP1)。所有上述都通过引用引入此处用于所有目的，如同完全陈述的一样。
如果没有相反指示，此处提及的所有公开文件、专利申请、专利和其他参考文件都通过引用整体明确引入此处用于所有用途，如同完全陈述的一样。
除非相反定义，此处所用的所有技术和科学术语都具有与本发明所属领域的普通技术人员通常理解的相同的含义。在抵触情况下，包括定义的本说明书将占主导。
除非明确指出，商标以大写字母显示。
尽管在本发明的实践或测试中能够使用与此处公开的那些相似或等效的方法和材料，但此处描述了适合的方法和材料。
除非相反声明，所有百分比、份数、比例等都是以重量计的。
当量、浓度或其他数值或参数作为范围或一系列上限和下限值给出时，其应当理解为特别公开了由任何对任意上限和下限范围界限形成的所有范围，无论该范围是否被单独公开。在此处列举了数值范围的情况下，除非相反声明，该范围意于包括其端点以及该范围内的所有整数和分数。本发明的范围并不意于限定于在限定范围时列举的特别值。
当在描述数值或范围端点中使用术语“约”时，本发明应当理解为包括所涉及的该特别数值或端点。
此处所用的术语“包括”、“包含”、“含有”、“具有”、“拥有”或其其他变型都意于包括开放式含义。例如，包括一系列要素的工艺、方法、制品或装置不必限定于仅这些要素，而是能够包括未明确列出的或此类工艺、方法、制品或装置固有的其他要素。此外，除非明确相反声明，“或”表示开放式的或而非封闭式的或。例如，条件A或B是由以下中的任一种满足的：A真(或存在)和B假(或不存在)；A假(或不存在)和B真(或存在)；和A和B都真(或存在)。
此处用于描述多个要素或组分的“a”或“an”的使用仅用于方便且给出所公开的一般含义。除非显然有相反含义，该说明书应当阅读为包括一个或至少一个而且单数形式还包括多个。
此处的材料、方法和实例都仅是示例性的，以及除非特别声明，都不意于限制。
碳质原料
此处所用的术语“碳质原料”表示在催化气化反应中用作原料的碳质材料。该碳质原料可以由例如煤、石油焦、液体石油残余物、沥青质或其混合物形成。该碳质原料能够来自单一来源或来自两种或更多种来源。例如，该碳质原料能够由一种或多种焦油砂petcoke材料、一种或多种煤材料、或这两类的混合物形成。在本发明的一种实施方案中，该碳质原料是煤、石油焦或其混合物。
石油焦
此处所用的术语“石油焦”包括(i)在石油处理中得到的高沸点烃馏分的固体热分解产物(重残余物-“残油(resid)petcoke”)和(ii)处理焦油砂的固体热解产物(沥青砂或油砂-“焦油砂petcoke”)。此类碳化产物包括例如生焦、煅烧焦、针状石油焦和流化床石油焦。
残油petcoke能够来自原油，例如通过用于升级高重力原油蒸馏残余物的焦化方法，基于该焦的总重量，该石油焦包含作为少量组分的典型地为约1.0wt％或更少，或更典型地为约0.5wt％或更少的灰分。典型地，此类较低灰分的焦中的灰分主要包括金属，例如镍和钒。
焦油砂petcoke能够来自油砂，例如通过用于升级油砂的焦化方法。基于该焦油砂petcoke的总重量，该焦油砂petcoke包含作为少量组分的典型地在约2wt％～约12wt％的范围，或更典型地在约4wt％～约12wt％的范围的灰分。典型地，此类较高灰分的焦中的灰分主要包含例如硅和/或铝化合物的材料。
基于该石油焦的总重量，该石油焦(残油petcoke或焦油砂petcoke)能够包括至少约70wt％的碳，至少约80wt％的碳，或至少约90wt％的碳。典型地，基于该石油焦的重量，该石油焦包括小于约20wt％的无机化合物。
液体石油残余物
此处所用的术语“液体石油残余物”包括(i)石油加工中得到的高沸点烃馏分的液体热解产物(重残余物-“残油液体石油残余物”)和(ii)加工焦油砂的液体热解产物(沥青砂或油砂-“焦油砂液体石油残余物”)。该液体石油残余物基本上不是固体；例如其能够是粘稠流体或污泥的形式。
残油液体石油残余物能够来自原油，例如通过用于升级高重力原油蒸馏残余物的方法。基于该残余物的重量，此类液体石油残余物包含作为少量组分的典型地为约1.0wt％或更少，或更典型地为约0.5wt％或更少的灰分。典型地，此类较低灰分的残余物中的灰分主要包括金属，例如镍和钒。
焦油砂液体石油残余物能够来自油砂，例如通过用于升级油砂的方法。基于该残余物的总重量，该焦油砂液体石油残余物包含作为少量组分的典型地在约2wt％～约12wt％的范围内，或更典型地在约4wt％～约12wt％的范围内的灰分。典型地，此类较高灰分的残余物中的灰分主要包含例如硅和/或铝化合物的材料。
沥青质
沥青质通常包括在室温下为芳香碳质固体，且能够源自例如原油和原油焦油砂的加工。
煤
此处所用的术语“煤”表示泥煤、褐煤、亚烟煤、烟煤、无烟煤或其混合物。在某些实施方案中，基于煤的总重量以重量计，该煤具有小于约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％的碳含量。在其他实施方案中，基于煤的总重量以重量计，该煤具有高达约85％，或高达约80％，或高达约75％的碳含量。可用的煤的实例包括但不局限于：Illinois #6、Pittsburgh #8，Beulah(ND)、Utah Blind Canyon 和Powder River Basin(PRB)煤。以干重量计，无烟煤、烟煤、亚烟煤和褐煤可以分别包含该煤总重量的约10wt％，约5～约7wt％，约4～约8wt％，和约9～约11wt％的灰分。然而，任意特定煤源的灰分含量将取决于该煤的品级和来源，如本领域技术人员熟知的那样。例如参见“Coal Data：A Reference”，Energy Information Administration，Office of Coal，Nuclear，Electric and Alternate Fuels，U.S.Department of Energy，DOE/EIA-0064(93)，1995年2月。
碳质原料转化为合成气流
在依照本发明的方法中，碳质原料在合成气形成区域中转化为合成气流。该合成气形成区域是在其中将该碳质原料转化为合成气流的区域或一个或多个装置的集合；其能够包括一个或多个反应器、预加工装置、气体提纯装置等。如本领域技术人员将认识到的那样，事实上能够使用任意常规方法和装置进行该转化。以下详细描述了催化气化方法和装置的特别实例；然而应当认识到其仅是本发明的实施方案，本发明的较宽方面并不由其限定。
在上述引用的名称为“PROCESSES FOR MAKING SYNTHESISGAS AND SYNGAS-DERIVED PRODUCTS”的美国专利申请序列号____中描述了适用于本发明中的方法的一种实例。在该发明中，描述了用于制备包括氢气和一氧化碳的合成气流的方法，其中该方法包括：(a)提供碳质原料；(b)将该碳质原料在气化反应器中在蒸汽和气化催化剂存在下在适合的温度和压力下进行反应以形成包含包括甲烷、氢气和一氧化碳在内的多种气体的粗产物气流；(c)从该粗产物气流中除去蒸汽并将其脱硫(sweeten)以形成经脱硫的气流；(d)分离至少第一部分的该经脱硫的气流并向其中添加蒸汽以形成具有第一蒸汽/甲烷比的第一重整器输入气流；和具有第二蒸汽/甲烷比的第二重整器输入气流，其中该第一蒸汽/甲烷比小于该第二蒸汽/甲烷比；(e)重整该第二重整器输入流以形成包含蒸汽、一氧化碳和氢气的循环气流；(f)向该气化反应器中引入该循环气流，和(g)重整该第一重整器输入流以形成该合成气流。
催化气化方法
在本发明的上下文中所称的该气化方法包括将颗粒状碳质原料在气化反应器中在蒸汽和气化催化剂存在下在适合的温度和压力下进行反应以形成包括氢气、一氧化碳、二氧化碳、硫化氢、氨和其他高级烃中的一种或多种以及甲烷的多种气体产物和固体焦炭残余物。例如在以下中公开了此类气化方法的实例：之前引入的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；共同拥有的美国专利申请序列号12/178,380(2008年7月23日提交)、12/234,012(2008年9月19日提交)和12/234,018(2008年9月19日提交)，以及之前引入的名称为“CONTINUOUS PROCESSES FOR CONVERTING CARBONACEOUS FEEDSTOCK INTO GASEOUS PRODUCTS”的序列号____(代理机构档案号FN-0018 US NP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的序列号____(代理机构档案号FN-0014 US NP1)；名称为“PROCESSES FOR MAKING SYNTHESIS GAS AND SYNGAS-DERIVED PRODUCTS”的序列号____(代理机构档案号FN-0010 US NP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的序列号____(代理机构档案号FN-0015 USNP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的序列号____(代理机构档案号FN-0016 US NP1)；名称为“STEAM GENERATING SLURRY GASIFIER FOR THE CATALYTIC GASIFICATION OF ACARBONACEOUS FEEDSTOCK”的序列号____(代理机构档案号FN-0017 US NP1)；和名称为“CARBONACEOUS FUELS AND PROCESSES FOR MAKING AND USING THEM”的序列号____(代理机构档案号FN-0013 US NP1)。
用于此类方法中的该气化反应器典型地是在中等高的压力和温度下操作的，需要将该颗粒状碳质原料引入该气化反应器的反应区域，同时保持所需的温度、压力和该颗粒状碳质原料的流速。本领域的技术人员熟知用于将原料提供到高压力和/或温度环境中的进料系统，包括用于供给固体的星式进料机、螺旋进料机、旋转活塞和闭锁式料斗；和用于供给液体的离心泵和蒸汽雾化喷嘴。应当认识到该进料系统能够包括两个或更多个将会可替代使用的压力平衡元件，例如闭锁式料斗。
在一些情况中，该颗粒状碳质原料能够在高于该气化反应器的操作压力的压力条件下制备。因此，能够将该颗粒状碳质原料直接送入该气化反应器而不经进一步的加压。
典型地，将该碳质原料作为具有从约250微米，或从约25微米，直到约500，或直到约2500微米的平均粒度的颗粒供给该气化反应器。本领域技术人员能够容易地确定该颗粒的适合粒度。例如，当使用流化床气化反应器时，该颗粒状碳质原料能够具有能使该颗粒状石油焦材料在该流化床气化反应器中所用的气体流速下开始流化的平均粒度。下面更详细地描述了用于制备颗粒的方法。
适合的气化反应器包括逆流固定床、并流固定床、流化床、曳出流和移动床反应器。该气化反应器中的压力典型地将约为约10～约100atm(约150～约1500psig)。该气化反应器典型地将在至少约450℃，或至少约600℃或更高，到约900℃，或到约750℃，或到约700℃的中等温度；和至少约50psig，或至少约200psig，或至少约400psig，到约1000psig，或到约700psig，或到约600psig的压力下操作。
用于该颗状碳质原料的加压和反应的气化反应器中所用的气体典型地包括蒸汽和非必要的氧气、空气、CO和/或H2，依照本领域技术人员已知的方法供给到该反应器。典型地，将气化中生成的一氧化碳和氢气回收并循环。然而，在一些实施方案中，该气化环境保持基本不含空气，特别是氧气。在本发明的一种实施方案中，该碳质原料的反应是在具有小于1体积％氧气的气氛中进行的。
本领域技术人员已知的任意蒸汽锅炉都能将蒸汽供给该气化反应器。例如此类锅炉能够通过使用任意碳质材料(例如粉末状的煤、生物质等)提供动力，且包括但不局限于从该颗粒状碳质原料制备操作中除去碳质材料(例如上述的微粒)。还能够由与燃气涡轮相连接的第二气化反应器供应给蒸汽，其中将来自该反应器的排气热交换到水源以产生蒸汽。还可以由从该热的粗汽化器产物气体回收的热量产生蒸汽。
来自其他工艺操作的循环蒸汽也能够用于为该气化反应器供给蒸汽。例如，当用流化床浆液干燥器(如下所述)干燥该浆态颗粒状碳质原料时，能够将通过蒸发产生的蒸汽供给该气化反应器。
能够通过用本领域技术人员已知的任意方法使供给该气化反应器的蒸汽和循环气体的气体混合物过热来提供该催化气化反应少量的所需供热。在一种方法中，能够将CO和H2的压缩循环气体与蒸汽混合，然后通过与气化反应器流出物进行热交换并然后在循环气体炉中过热，进一步使所得到的蒸汽/循环气体混合物过热。
在该方法中可以包括甲烷重整器以补充供应给该反应器的循环的CO和H2以确保该反应在热中性(绝热)条件下运行。在此类情况中，能够将来自该甲烷产物的甲烷供应给该重整器，如下所述。
颗粒状碳质原料在所需条件下的反应典型地提供包括多种气态产物和固体焦炭残余物的粗产物，该多种气态产物包含甲烷以及氢气、一氧化碳和其他高级烃中的至少一种或多种。在本发明的方法过程中在气化反应器中产生的焦炭残余物典型地从该气化反应器中除去用于取样、净化和/或催化剂回收。用于回收焦炭残余物的方法是本领域技术人员公知的。例如可以使用由EP-A-0102828教导的一种此类方法。能够定期从该气化反应器中通过闭锁式料斗系统取出焦炭，但本领域技术人员已知其他方法。
离开该气化反应器的粗产物气流能够通过用作分离区域的该气化反应器的一部分，在此处将重量太大以致于不能被离开该气化反应器的气体夹带的颗粒返回到该流化床。该分离区域能够包括一个或多个内部旋风分离器或用于从气体中除去颗粒的类似装置。通过该分离区域并离开该气化反应器的气体流出物通常包含CH4、CO2、H2、CO、H2S、NH3、未反应的蒸汽、夹带的颗粒和其他痕量污染物(例如COS和HCN)。
典型地能够通过适合的方法(例如外部旋风分离器然后文丘里洗涤器)除去残余的夹带微粒。能够将该回收的颗粒经处理以回收碱金属催化剂。
然后能够将从其中除去了微粒的气流通过热交换器以冷却该气体，且回收的热量能够用于预加热循环气体和产生高压蒸汽。离开该文丘里洗涤器的气流能够供应给COS水解反应器用于除去COS(酸性方法)并进一步在热交换器中冷却以回收残余的热量，然后进入水洗涤器用于氨回收，产生包括至少H2S、CO2、CO、H2和CH4的经洗涤的气体。用于COS水解的方法是本领域技术人员已知的，例如参见US4100256。
然后能够将已经从其中除去了微粒的粗产物气流通过热交换器以冷却该气体，并从其中除去蒸汽。该回收的热量能够用于例如预加热循环气体并产生高压蒸汽。能够通过任意适合的方法(例如外部旋风分离器然后文丘里洗涤器)除去残余的夹带微粒。能够将该回收的颗粒经处理以回收碱金属催化剂。
然后能够通过例如从其中除去酸性气体和硫(即含硫化合物，例如COS和H2S)将该粗产物气流脱硫。例如，能够将离开该文丘里洗涤器的进料给COS水解反应器用于除去COS(酸性方法)并进一步在热交换器中冷却以回收残余的热量，然后进入水洗涤器用于氨回收，产生包括至少H2S、CO2、CO、H2和CH4的经洗涤的气体。用于COS水解的方法是本领域技术人员已知的，例如参见US4100256。
能够使用来自该经洗涤气体的残热来产生低压蒸汽。能够处理洗涤器水和酸性方法浓缩物以汽提和回收H2S、CO2和NH3；此类方法是本领域技术人员公知的。NH3能够典型地作为含水溶液(例如20wt％)回收。
随后能够使用酸性气体去除方法通过包括气体的溶剂处理的物理或化学吸附方法从该经洗涤的气流中除去H2S和CO2，以得到清洁气流。此类方法包括将该经洗涤的气体与溶剂(例如一乙醇胺、二乙醇胺、甲基二乙醇胺、二异丙基胺、二乙二醇胺、氨基酸的钠盐溶液、甲醇、热碳酸钾等)接触。一种方法能够包括使用具有两个序列的
Figure BPA00001168349200111
(UOP LLC，Des Plaines，IL USA)或(Lurgi AG，Frankfurt am Main，Germany)溶剂；每个序列都由H2S吸收器和CO2吸收器构成。能够通过本领域技术人员已知的任意方法再生包含H2S、CO2和其他污染物的废溶剂，包括将该废溶剂与蒸汽或其他解吸气(stripping gas)接触以除去该污染物或通过将该废溶剂通过汽提塔。能够将回收的酸性气体送往硫回收处理。所得到的经脱硫的气流典型地主要包含CH4、H2和CO和典型地少量的CO2和H2O。能够将任何从该酸性气体回收或酸性水汽提中回收的H2S通过本领域技术人员已知的任意方法转化为元素硫，包括Claus方法。元素硫能够作为熔融液体回收。
参照之前引入的公开文件和申请能够获知进一步的工艺细节。
气化催化剂
依照本发明的气化方法使用碳质进料(例如煤和/或石油焦)并进一步使用一定量的气化催化剂，例如作为碱金属和/或包含碱金属的化合物的碱金属组分，以及非必要的助催化剂，如之前引入的参考文件中所公开的。典型地，该碱金属组分在该组合物中的量足以提供在从约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的范围的碱金属原子∶碳原子比。此外，将该碱金属典型地负载在碳源之上以得到以质量计为该碳质材料(例如煤和/或石油焦)的总灰分含量的约3～约10倍高的碱金属含量。
适合的碱金属是锂、钠、钾、铷、铯及其混合物。特别有用的是钾源。适合的碱金属化合物包括碱金属的碳酸盐、碳酸氢盐、甲酸盐、草酸盐、氨化物、氢氧化物、乙酸盐或类似的合物。例如，该催化剂能够包括以下中的一种或多种：Na2CO3、K2CO3、Rb2CO3、Li2CO3、Cs2CO3、NaOH、KOH、RbOH或CsOH，特别地为碳酸钾和/或氢氧化钾。
典型地，碳质原料包括大量无机物质(例如包括钙、氧化铝和/或二氧化硅)，其在气化反应器中形成无机氧化物(“灰分”)。在高于约500～600℃的的温度下，钾和其他碱金属能够与灰分中的氧化铝和二氧化硅反应生成不可溶的碱金属铝硅酸盐。在此类形式中，该碱金属是基本不可溶于水的且作为催化剂是无活性的。为了防止在煤气化反应器中积累该残余物，定期取出焦炭残余物的固体清除物(即由灰分、未反应或部分反应的碳质原料和各种碱金属化合物(水溶性和水不可溶性的)构成的固体)。优选地，从该焦炭残余物中回收该碱金属用于循环；任意未回收的催化剂通常都由催化剂补充流补偿。该原料中有越多的氧化铝和二氧化硅，得到较高的碱金属回收率的成本就越高。
该碳质原料中灰分含量能够经选择以例如为约20wt％或更小，或约15wt％或更小，或约10wt％或更小，其是煤所典型的；或者为约1％或更小，或约0.5％或更小，或约0.1％或更小，其是包括petcoke 的石油残余物所典型的。
在本发明的某些实施方案中，从该焦炭残余物中充分提取该气化催化剂(例如提取率大于80％，大于90％，或甚至大于95％)。已经开发了用于从该固体清除物回收气化催化剂(例如碱金属)以降低原材料成本并使催化气化工艺对环境的影响最小化的方法。能够用循环气体和水对该焦炭残余物淬火并将其引向用于提取和重新利用该碱金属催化剂的催化剂循环操作。特别有用的回收和循环方法描述于以下中：US4459138，以及之前引用的US4057512、US2007/0277437A1、名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的美国专利申请序列号____(代理机构档案号FN-0007 US NP1)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的美国专利申请序列号____(代理机构档案号FN-0014 US NPl)；名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的美国专利申请序列号____(代理机构档案号FN-0015 US NP1)；和名称为“CATALYTIC GASIFICATION PROCESS WITH RECOVERY OF ALKALI METAL FROM CHAR”的美国专利申请序列号____(代理机构档案号FN-0016 US NP1)。对于进一步的工艺细节，能够参考这些文件。
在本发明的某些实施方案中，从该焦炭残余物中提取至少70％，至少80％，或甚至至少90％的水溶性气化催化剂。
用于制备用于气化的碳质原料的方法
在该气化方法中所用的该碳质原料可能需要初始加工。
能够依照本领域中已知的任意方法将该碳质原料压碎和/或磨碎，例如冲击粉碎和湿法或干法磨碎以产生颗粒。根据用于压碎和/或磨碎该石油焦所用的方法，所得到的颗粒可能需要区分大小(size)(例如依照尺寸分离)以提供用于气化反应器的碳质原料的适当粒度范围。该区分大小操作能够用于从适用于该气化方法的该碳质原料颗粒中分离出碳质原料的微粒。
能够使用本领域技术人员已知的任意方法区分该颗粒大小。例如，能够通过将该颗粒过筛或通过一个或多个筛子而进行区分大小。过筛装置能够包括格筛、条杆筛和金属网筛。筛子能够是静态或混合机制，用于摇动或振动该筛子。可替代地，能够使用分级来分离该颗粒状碳质原料。分级设备能够包括矿石分选机、气体旋风分离器、水力旋流器、耙式分级机、旋转转筒筛、或流化或曳出流分级器。还能够在磨碎和/或压碎之前将该碳质原料筛分或分级。
在本发明的一种实施方案中，将该碳质原料压碎或磨碎，然后筛分以从适用于该气化方法的碳质原料颗粒中分离出具有小于约45微米的平均粒度的碳质原料的微粒。如下更详细描述，该碳质原料的微粒能够保持未转化(即在气化或燃烧过程中未反应)，然后与该焦炭残余物结合以提供本发明的碳质燃料。
然后能够将具有适用于该气化反应器中的粒度的该部分碳质原料进一步处理，例如以通过本领域已知的方法浸渍一种或多种催化剂和/或助催化剂，例如如以下中公开的那样：US4069304和US5435940；之前引入的US4092125、US4468231和US4551155；之前引入的美国专利申请序列号12/234,012和12/234,018；和之前引入的名称为“PETROLEUM COKE COMPOSITIONS FOR CATALYTIC GASIFICATION”的美国专利申请序列号____(代理机构档案号FN-0008 US NP1)、名称为“PETROLEUM COKE COMPOSITIONS FOR CATALYTIC GASIFICATION”的序列号____(代理机构档案号FN-0011 US NP1)和名称为“COAL COMPOSITIONS FOR CATALYTIC GASIFICATION”的序列号____(代理机构档案号FN-0009 US NP1)。
将经脱硫的气流转化为合成气流
能够使用本领域技术人员已知的任意方法将该经脱硫的气流转化为合成气流。例如，在本发明的一种实施方案中，从该经脱硫的气流中分离出一氧化碳和氢气以提供该合成气流和甲烷气流。能够使用例如低温分离的方法进行该分离。一种用于进行该分离的方法包括结合使用用于除去残余的H2O和CO2的分子筛吸收剂和用于提供该甲烷气流和该合成气流的低温蒸馏。
在本发明的另一实施方案中，将该经脱硫的气流重整以形成该合成气流。在该重整反应中，甲烷与蒸汽反应以依照下面的方程生成氢气和一氧化碳：
H2O+CH4→3H2+CO
在本发明的某些实施方案中，该重整反应将该经脱硫的气流中基本所有的(例如大于约80％，大于约90％，或甚至大于约95％的)甲烷转化为一氧化碳。该重整反应能够在例如约1300°F～约1800°F范围(例如约1550°F)的温度和在约200psig～约500psig范围(例如约350psig)的压力下进行。该重整反应能够在例如蒸汽重整炉内的管的具有催化剂衬里的内部上进行。该催化剂能够为例如负载在惰性载体上的金属组分。该金属组分能够是例如：选自周期表的VI-B族和铁族的金属，例如铬、钼、钨、镍、铁或钴。该催化剂能够包括少量碳酸钾或类似的化合物作为助催化剂。适合的惰性载体包括二氧化硅、氧化铝、二氧化硅-氧化铝和沸石。该重整反应能够在重整炉内的管(例如形状为盘管)内进行。在本发明的某些实施方案中，能够使用第二部分的该经脱硫的气体用于为该重整炉提供燃料。例如，能够使用在约15～约30％范围(例如约22％)的一部分该经脱硫的气流为该重整炉提供燃料。在本发明的另一实施方案中，通过天然气或通过来自此处公开的任意合成反应器的可燃烧的尾气补充炉燃料。
在本发明的一些实施方案中，该合成气流经过进一步的加工步骤。例如，能够通过热交换冷却该合成气流；回收的热量能够用于加热或产生蒸汽，或者用于加热工艺内的其他气流。该合成气流还能够调节其一氧化碳/氢气比。在本发明的一种实施方案中，通过将二氧化碳与氢气反应以生成一氧化碳和水来提高该一氧化碳/氢气比，从而调节该合成气流的一氧化碳/氢气比。该所谓的二次变换反应(back shift reaction)能够在例如在约300～约550°F范围(例如约412°F)的温度下在包括二氧化碳的气氛中进行。本领域技术人员能够确定用于该二次变换反应的适当的反应条件。
合成气衍生产物
在依照本发明的方法中，将该合成气流输送到合成气反应区域，在其中将其进行反应以生成合成气衍生产物。合成气衍生产物是由合成气的反应生成的产物，其中并入了来自该合成气一氧化碳的碳。该合成气衍生产物能够本身就是最终的可销售的产品；其也能够是在其他产品的合成中的中间产物。该合成气反应区域是在其中该合成气流转化为该合成气衍生产物的区域或一个或多个装置的集合；其能够包括一个或多个反应器、预加工装置、气体提纯装置等。如本领域技术人员将认识到的那样，合成气能够用作广泛各种反应的原料以生成宽范围的各种合成气衍生产物。例如，该合成气衍生产物能够用于制备具有两个或多个碳的化合物，例如一种或多种烃、一种或多种碳氢氧化合物(oxyhydrocarbon)及其混合物。该合成气衍生产物能够是例如甲醇、乙醇、二甲醚、二乙醚、甲基叔丁基醚、乙酸、乙酸酐、线性链烷烃、异链烷烃、线性烯烃、异构烯烃、线性醇、线性羧酸、芳香烃；费托柴油燃料、喷气燃料、其他馏出燃料、石脑油、蜡、润滑油基油或润滑油基原油；或合成原油。该合成气的反应能够产生热能、可燃烧的尾气混合物或两者。
在其中该合成气的反应生成热能的本发明的实施方案中，该热能能够回收并例如用于之前的工艺步骤或其他应用中。例如，该热能能够在将该碳质原料转化为合成气流中使用。该热能能够用于产生或加热蒸汽，其能够用于转化方法或其他应用中。在其中该合成气的反应还形成可燃烧的尾气混合物(例如包括氢气、烃或其混合物)的本发明的实施方案中，能够燃烧该可燃烧的尾气混合物以产生或进一步加热该蒸汽。该蒸汽能够在该碳质原料的转化中使用；例如，其能够用于如上所述在合成气形成区域内的催化气化反应中；如上所述在重整步骤中添加到经脱硫的气流中；和/或用于如上所述干燥碳质原料(例如在催化剂负载之后)。还能够驱动该蒸汽通过涡轮用于发电，其能够用于该装置中或销售。如本领域技术人员将认识到的那样，从该合成气流的反应中回收的热能或由其产生或加热的蒸汽能够用于此处未具体指出的其他应用中。
在本发明的某些实施方案中，该合成气流的反应生成可燃烧的尾气混合物(例如作为副产物)。该可燃烧的尾气混合物能够包括例如氢气、烃、碳氢氧化合物或其混合物。能够燃烧该可燃烧的尾气混合物以提供热能，能够将其回收并用于例如之前的工艺步骤中或用于一些其他应用。例如，在本发明的一种实施方案中，该可燃烧的尾气混合物用于燃烧重整炉。该可燃烧的尾气混合物还能够燃烧以产生或加热蒸汽。该蒸汽能够用于之前的工艺步骤中；例如，能够将其如上所述提供给该气化反应器用于与该碳质原料进行反应；如上所述在一种或两种该重整器输入气流的形成中添加到该经脱硫的气流中；和/或如上所述用于干燥该碳质原料(例如在催化剂负载之后)。还能够驱动该蒸汽通过涡轮用于发电，其能够用于该装置中或销售。如技术人员将认识到的那样，通过燃烧该可燃烧的尾气混合物产生的热能或由其产生或加热的蒸汽能够用于此处未具体指出的其他应用中。

Claims (13)

1.用于由碳质原料制备合成气衍生产物的方法，其特征在于该方法包括以下步骤：
(a)提供碳质原料；
(b)在合成气形成区域中将该碳质原料至少部分转化为包含氢气和一氧化碳的合成气流；
(c)将该合成气流输送到合成气反应区域；
(d)将该合成气流在该合成气反应区域中进行反应以形成该合成气衍生产物和热能；
(e)回收该合成气衍生产物；和
(f)回收由该合成气流的反应生成的该热能。
2.权利要求1的方法，其特征在于该碳质原料的转化包括以下步骤：
(i)将该碳质原料在气化反应器中在蒸汽和气化催化剂的存在下在适合的温度和压力下进行反应以形成包括多种气体的粗产物气流，所述多种气体包括甲烷、氢气和一氧化碳；
(ii)从该粗产物中除去蒸汽并将其脱硫以形成经脱硫的气流；和
(iii)从该经脱硫的气流中分离出一氧化碳和氢气以提供该合成气流和甲烷气流。
3.权利要求1的方法，其特征在于该碳质原料的转化包括以下步骤：
(i)将该碳质原料在气化反应器中在蒸汽和气化催化剂的存在下在适合的温度和压力下进行反应以形成包括多种气体的粗产物气流，所述多种气体包括甲烷、氢气和一氧化碳；
(ii)从该粗产物气流中除去蒸汽并将其脱硫以形成经脱硫的气流；和
(iii)重整该经脱硫的气流以形成该合成气流。
4.权利要求1～3中任何项的方法，其特征在于使用该热能以产生或加热蒸汽。
5.权利要求4的方法，其特征在于该合成气的反应进一步形成可燃烧的尾气混合物；以及其中将该可燃烧的尾气混合物燃烧以进一步加热该蒸汽。
6.权利要求5的方法，其特征在于将该蒸汽驱动通过涡轮以发电。
7.权利要求4的方法，其特征在于将该蒸汽用于该合成气形成区域中的催化气化反应中。
8.用于由碳质原料制备合成气衍生产物的方法，其特征在于该方法包括以下步骤：
(a)提供碳质原料；
(b)在合成气形成区域中将该碳质原料至少部分转化为包含氢气和一氧化碳的合成气流；
(c)将该合成气流输送到合成气反应区域；
(d)将该合成气流在该合成气反应区域中进行反应以形成该合成气衍生产物和可燃烧的尾气混合物；
(e)回收该合成气衍生产物；和
(f)燃烧该可燃烧的尾气混合物以提供热能。
9.权利要求8的方法，其特征在于该碳质原料的转化包括以下步骤：
(i)将该碳质原料在气化反应器中在蒸汽和气化催化剂的存在下在适合的温度和压力下进行反应以形成包括多种气体的粗产物气流，所述多种气体包括甲烷、氢气和一氧化碳；
(ii)从该粗产物中除去蒸汽并将其脱硫以形成经脱硫的气流；和
(iii)从该经脱硫的气流中分离出一氧化碳和氢气以提供该合成气流和甲烷气流。
10.权利要求8的方法，其特征在于该碳质原料的转化包括以下步骤：
(i)将该碳质原料在气化反应器中在蒸汽和气化催化剂的存在下在适合的温度和压力下进行反应以生成包括多种气体的粗产物气流，所述多种气体包括甲烷、氢气和一氧化碳；
(ii)从该粗产物气流中除去蒸汽并将其脱硫以形成经脱硫的气流；和
(iii)重整该经脱硫的气流以形成该合成气流。
11.权利要求8～10中任何项的方法，其特征在于将该可燃烧的尾气混合物燃烧以加热蒸汽。
12.权利要求11的方法，其特征在于将该蒸汽驱动通过涡轮以发电。
13.权利要求11的方法，其特征在于将该蒸汽用于该合成气形成区域中的催化气化反应中。
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