CN102906230B - 液体重烃进料向气态产物的转化 - Google Patents
液体重烃进料向气态产物的转化 Download PDFInfo
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Abstract
本发明涉及由“液体”重烃进料生成轻烯烃、甲烷和其它较高价值气态烃的方法和仪器。
Description
发明领域
本发明涉及由“液体”重烃进料生成轻烯烃、甲烷和其它较高价值气态烃的方法和仪器。
发明背景
液体重烃进料是在环境条件下可流动的,或可在高温条件下可使之流动的粘性液体或半固体材料。这些材料通常是加工烃材料比如原油后的残留物。
例如,精炼原油的第一步通常为蒸馏,以使复杂的烃混合物分离成挥发性不同的馏分。典型的第一步蒸馏需要在大气压力下加热以蒸发尽可能多的烃成分,不超过约650℉的实际温度,因为较高的温度可导致热分解。在大气压力下不蒸馏的馏分常称作“常压石油残留物”。馏分可进一步真空蒸馏,以致最多约650℉的实际温度可蒸发更多的材料。剩余的不能蒸馏的液体称为“真空石油残留物”。常压石油残留物和真空石油残留物两者都被认为是出于本发明目的的液体重烃材料。
液体重烃材料因为它们的高粘度和低挥发性,和增加的杂质(比如硫)浓度,属于相对意义上低价值的材料,例如作为燃料。例如,真空石油残留物中的硫浓度通常是原油中的硫浓度的至少约2.5倍。
就石油残留物来说,残留物馏分通常构成超过初始原油质量的20%,并且就重原油来说,有时构成超过初始原油质量的50%,所以存在高的动机将残留物转化为较高价值产品比如较轻烃液体和气体。
液体重烃材料可经受破坏性热分解以产生裂解的液体和气体,和仍为较低价值的固态石油焦炭。用于热分解的反应器称为焦化器,且它们可以是流化床反应器或固定辊筒。尽管得到的液体产物是较高价值的,但它们仍需通过与氢气反应的许多改进来与其它石油产品共混。
液体重烃材料的其它出路包括同较低粘度的馏出物共混以制造残余燃料油,或用作铺路沥青或屋面沥青,这些也被认为是低价值用途。
液体重烃材料还可通过催化和非催化(热)气化法转化为低等和中等BTU气体(合成气和富集甲烷的合成气)。这类材料在催化剂源、氢气、一氧化碳和蒸汽的存在下,在高温和高压下催化气化(加氢甲烷化)以生产甲烷和其它增值气体,公开于例如US6955695、US2010/0071262A1、US2010/0076235A1、WO2010/033848A2和WO2010/048493A2。
然而仍需要可由液体重烃材料生产更高价值产品比如轻烯烃以及甲烷和其它较高价值的气态烃的方法。
一个这样的方法公开于US3898299,其中将常压石油残留物先氢化,然后真空蒸馏成液相和真空残留物相。随后将得到的较轻液相在蒸汽的存在下热裂解(非催化热解)以生成烯烃。然而这种方法似乎只利用了常压石油残留物的较轻部分,剩余显著量的另外的残留物材料。
一个改进液体重烃材料的催化方法公开于US3816298,但公开的方法集中于中等分子量液体产物而非较低分子量气态产物。具体来讲,公开的方法通过使材料与氢气和含碳氧化物的气体在高于150 psig的压力和约700℉-1100℉的温度下接触,在含有负载的碱金属催化剂的第一反应区,使液体重烃材料转化成硫减少的“通常液体的烃产物”(具有大于70℉的常压沸点)和含氢气体。还生产固体材料(焦炭),其沉积在负载的碱金属催化剂上。随后将一部分负载的碱金属催化剂装入第二反应区,在其中与蒸汽和任选氧气在高于150 psig的压力和高于1200℉的温度下接触以消耗沉积的碳,从而使负载的催化剂再生并生产用于第一反应区的氢气、含碳氧化物的气体和热能。热的再生载体同样回料到第一反应区。因此这种方法的第一反应区主要是焦化器单元,第二反应区主要是气化单元。这种方法期望的液体产物包括比如汽油、加热用油和气体油馏分。尽管在液体产物中似乎存在不饱和化合物,它实际上是公开方法中陈述的减小不饱和组分的益处,因为它们是有害的(比如在汽油产品中)。也没有公开轻烯烃比如乙烯和丙烯的生产。
几个参考文献还公开了从各种残留物进料生产烯烃,包括比如US4975181、US4980053、US6179993、US6303842、WO2007/149917A1和其中引用的其它公开内容。一般来说,在这些公开内容中,使石油残留进料与加热固体的流化床和任选催化剂组分(可为来自加热固体的相同或单独组分)在高温和短接触时间下接触。汽相用轻烯烃和其它轻烃生产,并且焦炭沉积在加热的颗粒上。焦炭包覆的颗粒通常通过烧掉焦炭再生和加热。催化剂通常是酸性组分比如耐火金属氧化物和铝酸盐、沸石和用过的流体催化裂化催化剂、富钒的烟道细粒、用过的铝矾土及混合物。
虽然存在现有方法,但是仍需要将较低价值的液体重烃材料转化成包括轻烯烃和烷烃的较高价值的气态产物混合物的另外的方法。
发明概述
一方面,本发明提供由液体重烃材料生成气态粗产品流的方法,所述方法包含以下步骤:
(a)将液体重烃材料分散在气态载体中以生产分散的重烃进料;
(b)将包含热能和蒸汽,以及任选的一氧化碳和氢气,的过热气体进料流引入含有浸渍碱金属的碳质载体床的反应器中;
(c)任选将富氧流引入反应器中以产生热能,并任选原位产生一氧化碳和氢气;
(d)在浸渍碱金属的碳质载体床的存在下,使分散的重烃进料与蒸汽、一氧化碳和氢气在高压和约1100℉-约1400℉的温度下接触,以生成粗气态混合物,其包含甲烷、乙烯和丙烯的一种或两种、乙烷和丙烷的一种或两种;和
(e)从反应器中取出粗气态混合物流作为气态粗产品流,
其中步骤(d)的反应有合成气需求,且合成气需求至少实质上由可存在于过热气体进料流的一氧化碳和氢气,和可在步骤(c)中生成的一氧化碳和氢气满足。
根据本发明的方法可用于例如由较低价值液体重烃进料生产较高价值的气态产物。
本发明的这些及其它实施方案、特征和优势在阅读以下详细说明后更容易被本领域普通技术人员理解。
附图简述
图1是根据本发明的方法的第一个实施方案的图表,在此含有低级烷烃和低级烯烃的气态粗产品流在竖直流化床反应器中由液体重烃材料生产。
图2是根据本发明的方法的第二个实施方案的图表,在此含有低级烷烃和低级烯烃的气态粗产品流在水平移动床反应器中由液体重烃材料生产。
详细说明
本发明涉及将液体重烃材料最终转化为含有显著量的轻烯烃和轻烷烃的气态产品流的方法。以下提供进一步的细节。
在本描述的上下文中,本文提到的所有出版物、专利申请、专利和其它参考文献若非另外指出,均明确通过引用全文结合到本文中,用于所有目的,如同完全阐明。
除非另外限定,本文使用的所有技术和科学术语均具有本公开内容所属领域普通技术人员通常理解的相同含义。若有冲突,以本说明书(包括定义)为准。
除非明确标注,商标均以大写体显示。
尽管与本文描述类似或等价的方法和材料可用于实施或试验本公开内容,但合适的方法和材料仍在本文中描述。
除非另有说明,所有的百分率、份数、比值等都按重量计算。
除非另有说明,用psi单位表示的压力是表压,用kPa单位表示的压力是绝对压力。
当按范围或上限值和下限值的列举给出数量、浓度或其它数值或参数时,这应理解为具体公开所有由任意对任意上限范围和下限范围形成的范围,与范围是否分别公开无关。在本文叙述数值范围时,除非另有说明,所述范围旨在包括其端点和所有在该范围内的整数和分数。当限定范围时,不旨在将本公开内容的范围限定于所叙述的具体值。
当术语“约”用于描述一个值或一个范围的端点时,本公开应被理解为包括涉及的具体值或端点。
本文使用的术语“包含”、“包含”、“包括”、“包括”、“具有”、“具有”或它们的任何其它变化,均旨在覆盖非排它包含。例如,包含要素列举的工艺、方法、物品或仪器不必只局限于那些要素,而是可包括这些工艺、方法、物品或仪器未明确列举或固有的其它要素。进一步地,除非明确地相反说明,“或”指的是包含性的或而非排它性的或。例如,条件A或B通过以下任一满足:A为真(或存在)且B为假(或不存在)、A为假(或不存在)且B为真(或存在)以及A和B两者均为真(或存在)。
本文使用“一”来描述各要素和组分仅仅是为方便和给出本公开内容的一般意义。该描述应理解为包括一个或至少一个,且单数也包括复数,除非它明显表示其它。
除非本文另外限定,本文使用的术语“实质部分”指的是大于约90%的参考材料,优选大于约95%的参考材料,更优选大于约97%的参考材料。当涉及分子(比如甲烷、二氧化碳、一氧化碳和硫化氢)时,百分比基于摩尔,而其它基于重量。
除非本文另外限定,本文使用的术语“主要部分”指的是大于约50%的参考材料。当涉及分子(比如氢气、甲烷、二氧化碳、一氧化碳和硫化氢)时,百分比基于摩尔,而其它基于重量。
术语“耗尽”与减少同义。例如,从物流中除去材料的实质部分将产生实质上耗尽该材料的材料-耗尽流。
本文使用的术语“碳质”与烃同义。
本文使用的术语“碳质材料”是含有有机烃含量的材料。如本文限定,碳质材料可分为生物质或非生物质材料。
本文使用的术语“生物质”指的是来源于近代(例如,在过去100年之内)的活有机体的碳质材料,包括基于植物的生物质和基于动物的生物质。为了清楚,生物质不包括基于化石的碳质材料,比如煤。例如参见US2009/0217575A1和US2009/0217587A1。
本文使用的术语“基于植物的生物质”指的是来源于绿色植物、作物、藻类和树,比如但不限于高粱、甘蔗渣、甘蔗、竹子、杂种白杨、杂种柳树、合欢树、桉树、苜蓿草、三叶草、油棕、柳枝黍、苏丹草、黍、麻风树属和芒属(例如巨芒(Miscanthus x giganteus))的材料。生物质还包括农业栽培、加工和/或降解的废弃物比如玉米棒和玉米苞叶、玉米秸、稻草、坚果壳、植物油、芥花籽油(canola oil)、菜籽油、生物柴油、树皮、木屑、锯末和庭院废弃物。
本文使用的术语“基于动物的生物质”指的是由动物养殖和/或利用产生的废弃物。例如,生物质包括,但不局限于家畜养殖和加工的废弃物比如动物粪肥、鸟粪、家禽厩肥、动物脂肪和市政固体废物(例如污水)。
本文使用的术语“非生物质”指的是不包含在本文限定的术语“生物质”内的碳质材料。例如,非生物质包括,但不局限于无烟煤、烟煤、次烟煤、褐煤、石油焦炭、沥青烯、液体石油残留物或其混合物。例如参见US2009/0166588A1、US2009/0165379A1、US2009/0165380A1、US2009/0165361A1、US2009/0217590A1和US2009/0217586A1。
本文使用的术语“石油焦炭”和“石油焦”包括以下两者:(i)在石油加工中获得的高沸点烃馏分的固体热解产物(重残余物–“残油石油焦”);和(ii)加工沥青砂的固体热解产物(沥青质砂或油砂–“沥青砂石油焦”)。这类碳化产品包括比如生料、锻烧、针状和流化床石油焦。
残油石油焦也可来自原油,比如通过用于改进重-比重残留原油(比如液体石油残留物)的焦化过程,该石油焦含有微量组分的灰分,所述灰分通常占焦炭重量的约1.0 wt%或更少,且更通常占约0.5 wt%或更少。通常,这类较低灰分焦炭中的灰分包含金属比如镍和钒。
沥青砂石油焦可来源于油砂,比如通过用于改进油砂的焦化过程。沥青砂石油焦含有微量组分的灰分,所述灰分通常占沥青砂石油焦总重量的约2 wt%-约12 wt%的范围,且更通常占约4 wt%-约12 wt%的范围。通常,这类较高灰分焦炭中的灰分包含比如二氧化硅和/或氧化铝的材料。
石油焦炭具有固有的低含水量,通常在约0.2-约2 wt%的范围内(基于石油焦炭的总重量)。
石油焦炭可包含占石油焦炭总重量至少约70 wt%的碳,至少约80 wt%的碳或至少约90 wt%的碳。通常,石油焦炭包含少于约20 wt%的无机化合物(基于石油焦炭的重量)。
本文使用的术语“沥青烯”为室温下的芳香族碳质固体,并可来源于比如原油和原油沥青砂的加工。
本文使用的术语“煤”指的是泥煤、褐煤、次烟煤、烟煤、无烟煤、或其混合物。在某些实施方案中,煤的含碳量按重量计少于约85%、或少于约80%、或少于约75%、或少于约70%、或少于约65%、或少于约60%、或少于约55%、或少于约50%(基于煤的总重量)。在其它实施方案中,煤的含碳量按重量计在最多约85%、或最多约80%、或最多约75%的范围内(基于煤的总重量)。有用的煤的实例包括,但不局限于Illinois #6、Pittsburgh #8、Beulah(ND)、Utah Blind Canyon和Powder River Basin(PRB)煤。无烟煤、烟煤、次烟煤和褐煤可分别含有约10 wt%、约5-约7 wt%、约4-约8重量%和约9-约11 wt%的灰分(基于煤的干基总重量)。然而,如本领域技术人员熟悉的那样,任何特定煤源的灰分含量取决于煤的等级和来源。参见例如“Coal Data: A Reference(煤数据参考)”, Energy Information Administration, Office of Coal, Nuclear, Electric and Alternate Fuels, 美国能源部, DOE/EIA-0064(93), 1995年2月。
如本领域技术人员熟悉的那样,煤的燃烧产生的灰分通常包含飞灰和底灰两种。来自烟煤的飞灰可包含约20-约60 wt%的二氧化硅和约5-约35 wt%的氧化铝(基于飞灰的总重量)。来自次烟煤的飞灰可包含约40-约60 wt%的二氧化硅和约20-约30wt%的氧化铝(基于飞灰的总重量)。来自褐煤的飞灰可包含约15-约45wt%的二氧化硅和约20-约25wt%的氧化铝(基于飞灰的总重量)。参见例如Meyers等人“Fly Ash. A Highway Construction Material(飞灰—高速公路建筑材料),” Federal Highway Administration, 报告号FHWA-IP-76-16, Washington, DC, 1976。
来自烟煤的底灰可包含约40-约60 wt%的二氧化硅和约20-约30wt%的氧化铝(基于底灰的总重量)。来自次烟煤的底灰可包含约40-约50 wt%的二氧化硅和约15-约25wt%的氧化铝(基于底灰的总重量)。来自褐煤的底灰可包含约30-约80 wt%的二氧化硅和约10-约20 wt%的氧化铝(基于底灰的总重量)。参见例如Moulton, Lyle K. “Bottom Ash and Boiler Slag(底灰和锅炉渣),” Proceedings of the Third International Ash Utilization Symposium, U.S.Bureau of Mines, Information Circular No.8640, Washington, DC, 1973。
比如甲烷的材料可根据它的最初来源为上述定义下的生物质或非生物质。
“非气态” 材料实质上为环境条件下的液体、半固体、固体或混合物。例如煤、石油焦、沥青烯和液体石油残留物为非气态材料,而甲烷和天然气为气态材料。
术语“单元”指的是单元操作。当描述存在多于一个的“单元”时,这些单元以并行方式运转。然而一个单独的“单元”可包含多于一个的串联或并联单元,取决于上下文。例如,酸气体去除单元可包含硫化氢去除单元,随后串联的是二氧化碳去除单元。作为另一个实例,污染物去除单元可包含对于第一污染物的第一去除单元,随后串联的是对第二污染物的第二去除单元。作为另一个实例,压缩机可包含将气流压缩到第一压力的第一压缩机,随后串联的是进一步将气流压缩到第二(较高)压力的第二压缩机。
术语“合成气需求”指的是反应器中实质上稳态的合成气平衡的保持。在总体期望的稳态反应中,似乎氢气和一氧化碳在相对平衡下产生和消耗,且氢气和一氧化碳两者通常作为气态产物的一部分取出。因此氢气和一氧化碳必须以至少实质上保持这种反应平衡所需的量添加到(和/或如下所述,任选通过与供应的氧气燃烧/氧化反应而原位单独产生)反应器中。出于本发明的目的,反应必须“添加”(装入反应器和原位产生)的氢气和一氧化碳的量是“合成气需求”。
术语“蒸汽需求”指的是必须添加到反应器的蒸汽的量。蒸汽可通过例如在过热气体进料流、分散的重烃流、任选的富氧流中的蒸汽添加和/或作为单独的蒸汽流添加。要添加的(和来源)蒸汽的量将在以下进一步详细论述。由进料或替代催化剂进料的任何水分含量的蒸发原位产生的蒸汽可帮助满足蒸汽需求;然而,应注意到原位产生或在低于反应器运行温度的温度下装入反应器的任何蒸汽会影响反应的“热量需求”。
术语“热量需求”指的是必须添加到反应器以使步骤(d)的反应保持实质热平衡的热能的量,如以下进一步详细说明。
本文的材料、方法和实施例只是说明性的,除非具体陈述,不旨在为限制性。
液体重烃材料
本发明涉及“液体重烃材料”的加工,根据本发明,其为粘性液体或半固体碳质材料,所述材料在环境条件下是可流动液体,或可在高温条件(作为本方法的进料条件使用)下使之流动的液体(在以下进一步详细论述),以致材料可被分散在本发明方法中使用的气态载体中。
液体重烃材料的非限制性实例包括真空残油;常压残油;重的和还原的石油原油;柏油、沥青和石油沥青(天然存在的和由石油炼制过程得到的);沥青砂油;页岩油;催化裂解方法的塔底油;煤液化塔底油和其它含有显著量的重的或粘性材料比如石油蜡馏分的烃进料流。
液体重烃材料可固有地含有少量的固体碳质材料,比如石油焦炭和/或固体沥青烯,其一般分散在液体重烃基体内,而且在作为本方法的进料条件使用的高温条件下仍为固体。
另外,可将少量的固体碳质材料添加到在本发明中使用的液体重烃材料中。这类固体碳质材料的非限制性实例包括石油焦炭、固体沥青烯、煤和生物质。再循环/替代浸渍碱金属的碳质载体也可为添加到液体重烃材料中的固体碳质材料。通常,固体碳质材料应具有适合于分散在液体重烃基体内的粒径,但也可部分使用涂有液体重烃材料的颗粒形式,只要得到的材料可分散在用于制备分散的重烃进料的气态载体中。
分散的液体重烃进料的碳质内容物应主要包含液体重烃材料。
总的方法信息
在本发明的实施方案中,如图1和2所说明,使液体重烃材料流(10)与气态载体流(15)在混合容器或装置(120)中结合,其中将液体重烃材料分散在气态载体中以产生分散的重烃进料流(20)。在一个实施方案中,将液体重烃材料在气态载体中雾化以产生雾化的重烃进料流。
分散可通过传统装置进行,例如在具有静态混合器的在线混合器中,将以具体速率流动的进料流与适量的喷射蒸汽混合以产生富蒸汽的进料分散体,或者分散体可通过作为反应器(100/200)的进料入口(116)一部分的注射喷嘴产生。
合适的气态载体包括例如蒸汽、二氧化碳、合成气(含有一氧化碳和氢气的混合物)、惰性气体比如氮气和上述的混合物。通常,气态载体为蒸汽,或具有任选的少量一种或多种上述其它气体的主要或实质部分的蒸汽的混合物。在一个实施方案中,气态载体流为与二氧化碳混合的蒸汽,期望在这种条件下二氧化碳超临界。
气态载体流(15)通常是过热的,且液体重烃材料流(10)要加热到一定温度,以致在组合后,该温度使得到的分散的重烃流(20)在适合注入反应器(100/200)的高温下,无需另外加热,但是若有需要,可通过使用传统装置另外加热。分散的重烃进料流(20)在分散的重烃流进入反应器(100/200)的进料点(116)的温度通常为约900℉(约482℃)或更小,或约850℉(约454℃)或更小,以帮助使焦炭过早形成和可能的进料点(116)堵塞最小化。
分散的重烃进料流(20)的压力还应高于分散的重烃流进入反应器(100/200)的进料点(116)的压力。必要时,分散的重烃进料流(20)可通过传统装置在混合容器(120)之后,在注入反应器(100/200)之前(按需)压缩。
期望地,如上所述,当二氧化碳用作气态载体流(15)或作为气态载体流(15)的组分时,分散的重烃进料流(20)的温度和压力条件使得二氧化碳为超临界状态。
补充或补偿催化剂还可作为分散的重烃进料流(20)的一部分包括在内。
图1的反应器(100)含有浸渍碱金属的碳质载体的竖直床(110),分散的重烃进料流(20)注入其中。图2的反应器(200)含有浸渍碱金属的碳质载体的水平床(210),分散的重烃进料流(20)进料至其上。
浸渍碱金属的碳质载体是含有碱金属催化剂和任选的一种或多种共催化剂材料的碳载体。合适的浸渍碱金属的碳质载体的实例包括例如在US3958957和US2010/0121125A1中公开的那些。以下提供进一步的细节。
将包含蒸汽和任选氢气和一氧化碳的过热气流(25)同样注入反应器(100/200)。在一个实施方案中,过热气流(25)包含氢气和一氧化碳。如下所述,过热气流(25)的氢气和一氧化碳内容物可在合成气产生器中产生,合成气产生器也可用于使过热气流(25)或其它过程流比如气态载体流(15)和/或分散的重烃进料流(20)过热。
在反应器(100/200)中,分散的重烃碳进料与蒸汽、氢气和一氧化碳接触,并与床(110/210)接触(在浸渍碱金属的碳质载体的存在下),在床内认为发生了许多化学和物理过程。
结果是产生粗气态混合物,其包含甲烷、乙烯和丙烯的一种或两种(通常为两种的混合物)、乙烷和丙烷的一种或两种(通常为两种的混合物)以及少量的分子量增加的另外的烃材料(饱和的和/或不饱和的),和以下讨论的其它任选的组分和污染物。
反应器(100/200)的温度为约1100℉(约593℃)、或约1200℉(约649℃)、约1250℉(约677℃),至约1400℉(约760℃),或至约1350℉(约732℃)。
反应器(100/200)中的压力将提高(超过大气压),通常为约50 psig(约446 kPa)、或约100 psig(约791 kPa)、或约250 psig(约1825 kPa)、或约450 psig(约3204 kPa),至约1000 psig(约6996 kPa)、或至约600 psig(约4238 kPa)、或至约550 psig(约3894 kPa)。
反应器(100/200)中的温度和压力条件似乎对最终的产品混合物(乙烯相对于丙烯,乙烷相对于丙烷)具有显著影响;因此期望的产品混合物是决定反应器(100/200)的运行温度和压力条件的显著因素。
除粗气态混合物的产生外,进料的一部分碳成分似乎沉积在碳质载体上成为固体例如成为焦炭。同样,反应器(100/200)中的温度和压力条件似乎对焦炭形成的量(相对于转化成粗气态混合物)具有显著影响,这同样影响最终的粗气态混合物。
同样取决于反应器(100/200)的条件,来自碳质载体材料的一部分碳成分(原始的或沉积的焦炭)以及重烃进料,似乎气化为合成气混合物(一氧化碳和氢气)或加氢甲烷化成为富甲烷合成气(甲烷、一氧化碳和氢气),其可进一步甲烷化或在反应器(100/200)中转化为粗气态混合物的一部分。如以下讨论,气化/加氢甲烷化可在反应器(100/200)中得到促进,例如在床(110/210)的一部分(未描述)或反应器(100/200)的单独区域(未描述),或在单独的反应器(未描述)中。
期望地,反应器(100/200)中的反应的平衡在于,在碳质载体材料上沉积的碳质材料的量实质上与从碳质载体材料除去的材料的量相平衡。但是实际上,浸渍碱金属的碳质载体材料要定期从反应器(100/200)中除去,例如通过溢出流(35),且新的和/或再生的浸渍碱金属的碳质载体材料要注入反应器(100/200)中,比如通过催化剂进料线路(40)。如以下讨论,浸渍碱金属的碳质载体材料的再生可在例如单独的气化/加氢甲烷化反应器中进行。
不旨在受限于任何特别的理论,人们相信所有这些机理(包括以下提到的任选的部分氧化以及可能的其它)有助于最终的粗气态混合物组合物,所述组合物除烃组分以外,通常还含有未转化的蒸汽,以及其它任选的组分比如氢气、一氧化碳、二氧化碳、硫化氢和氨,这取决于反应条件以及液体重烃材料和碳质载体的组成。
反应器(100/200)中的液体重烃材料的转化总体是吸热的。另外,会有过程热损失,包括由于在低于反应器(100/200)的运行温度的温度下可对反应器(100/200)提供的任意进料进行任意所需原位加热的那些。因此,热能必须添加到反应器(100/200)中和/或原位产生以保持热平衡。如以上限定,必须添加到反应器(100/200)中以保持热平衡的热能的量是反应的热量需求。
如以下讨论,还可任选将富氧流(30)注入反应器(100/200)中,例如来帮助温度控制,和/或来原位提供另外的氢气和一氧化碳。
得到的气态粗产品流(50)通常要经受一个或多个下游加工步骤,包括比如冷却/淬火和热量回收、夹带固体分离、组分分离(例如回收烯烃成分、氨和氢气去除)、组分改进(例如酸气去除、脱硫、转移和/或甲烷化)和组分消耗(比如用于产生功率/蒸汽/热量的燃烧,和/或用于产生合成气/热量/蒸汽的部分氧化)。
以下提供另外的细节和实施方案。
反应器
(100/200)
几个气化反应器类型的任意种类均可用于反应器(100/200)。合适的反应器包括具有反应室(其为逆流固定床、并流固定床、流化床或夹带流动床反应室或移动床反应室)的那些。
图1的反应器(100)是竖直结构,且通常是流化床反应器。反应器(100)比如可以是“向下流”的逆流结构(如图1具体描述),其中使分散的重烃进料(20)在较高的点引入以致一些较重组分向下流过床(110),气体(比如过热气体进料流(25))在向上方向上流动并在高于流化床的去除点(118)去除,且较重组分(比如“用过的”催化剂颗粒)在接近或低于床(110)的点(比如溢出管线(35))去除。或者,反应器(100)可为“向上流”的并流结构,其中分散的重烃进料(20)在较低点进料以致液流连同气体(比如过热气体进料流(25))沿床(110)向上。
在反应器(100)的这两种结构类型中,通常在反应器(100)底部存在用于未流化的较大颗粒的收集区(112),和在反应器(100)顶部的分离区(114),以帮助使颗粒物质与粗气态混合物(在将其从反应器(100)取出时)分离。
图2的反应器(200)为具有床(120)的水平结构,所述床(120)为移动床。通常在这类结构中,分散的重烃进料流(20)、过热气体进料流(25)和催化剂进料管线(40)在反应器(200)的一端进料,且气态粗产品流(50)和催化剂溢出流(35)在反应器(200)的另一端取出。
因为反应器(100/200)在高压和高温下运转,所以催化剂床去除和补给需要在压力下向/从反应器(100/200)的反应室引入和取出适当的碳质载体。本领域技术人员熟悉向/从具有高压和/或高温环境的反应室供应和取出碳质载体的进料入口和出口,包括星形进料器、螺杆进料器、旋转活塞和锁式料斗。应理解入口和出口可包括两个或更多个压力-平衡元件,比如交替使用的锁式料斗。在有些情况下,碳质载体可在高于反应器(100/200)的运行压力的压力条件下制备或再生,因此碳质载体可直接通入反应器(100/200)和从反应器(100/200)中去除,而不进一步加压/减压。用于加压的气体可为惰性气体比如氮气,或更通常为过热蒸汽和/或二氧化碳的气流。
反应器(100/200)中的气流速度达到在反应器中可宽泛变化的期望的停留时间。
在某些实施方案中,反应器(100/200)中的气流速度、分散的重烃进料(20)进入反应器(100/200)的进料点(116)、和气态粗产品流(50)离开反应器(100/200)的去除点(118),使得蒸汽相从任意进料点(116)到任意去除点(118)的停留时间为短时期,比如少于约2秒、或约1.5秒或更少、或约1秒或更少、或约0.5秒或更少。为达到这种短停留时间,气流速度通常为约50英尺/秒(约15.2 m/秒)或更高、或约60英尺/秒(约18.3 m/秒)或更高。
在某些实施方案中,可使用较长停留时间,且反应器(100/200)中的典型的气流速度可为约0.1英尺/秒(约0.03 m/秒)、或约0.5英尺/秒(约0.15 m/秒)、或约1英尺/秒(约0.3 m/秒),至约2.0英尺/秒(约0.6 m/秒)、或至约1.5英尺/秒(约0.45 m/秒)。
在另一个实施方案中,存在多个用于分散的重烃进料的进料点,其中蒸汽相从至少一个进料点到任意去除点的停留时间为短时期,比如少于约2秒、或约1.5秒或更少、或约1秒或更少、或约0.5秒或更少。
当将富氧气流(30)也注入反应器(100/200)中时,来自碳质载体和可能的重烃进料的碳成分的一部分也可在氧化/燃烧反应中消耗,产生补充的热能以及一氧化碳和氢气。改变向反应器(100/200)供应的氧的量可提供有利的过程控制。增加氧的量将增加氧化/燃烧,因此增加原位的热量和合成气产生。减少氧的量将相反地减小原位的热量和合成气产生。
当使用时,可通过任何合适的方法比如将纯氧、氧气-空气混合物、氧气-蒸汽混合物或氧气-惰性气体混合物直接注入反应器内,将富氧气流(30)注入反应器(100/200)。参见例如US4315753和Chiaramonte等, Hydrocarbon Processing(烃的加工), 1982年9月, 255-257页。
富氧气流(30)通常通过标准空气-分离技术产生,并可作为高纯度氧气流(约95%或更大的体积百分数的氧,干基重)进料。但是通常,富氧气流作为与蒸汽的混合物提供,并在约400℉(约204℃)、或约450℉(约232℃)、或约500℉(约260℃),至约750℉(约399℃)、或至约700℉(约371℃)、或至约650℉(343℃)的温度和在至少稍高于反应器(100/200)存在压力的压力下引入。
当被提供给竖直流化床反应器比如反应器(100)时,富氧气流(30)通常在低于床(110)的点引入以免在反应器中形成热点,并避免气态产物的燃烧。富氧气流(30)可以例如有利地被引入反应器(100)的收集区(112),其中非流化颗粒收集通常在反应器的底部(比如低于反应器(100)底部的栅格或板(未描述)),以致非流化颗粒中的碳优先消耗,不同于反应器(100)中的不同区域的碳。
当被提供给反应器(200)时,富氧气流(30)通常在底部床(210),在具有良好颗粒流动的点引入,以免在反应器(200)中形成热点。
不旨在通过任何特定的操作理论限制,在与本发明有关而使用的操作条件下,一些水平的加氢甲烷化/气化似乎也在反应器(100/200)中发生。加氢甲烷化/气化可涉及几个不同的反应,包括比如:
蒸汽碳:C+H2O→CO+H2 (I)
水煤气转换:CO+H2O→H2+CO2 (II)
CO甲烷化:CO+3H2→CH4+H2O (III)
氢-气化:2H2+C→CH4 (IV)。
在加氢甲烷化反应中,头三个反应(I-III)占主导,引起以下总反应:
2C+2H2O→CH4+CO2 (V)。
在加氢甲烷化中,一氧化碳和氢气在相对平衡中产生和消耗,所以加氢甲烷化反应本身将产生富甲烷合成气。
在标准的蒸汽气化反应中,反应(I)占主导。若氧气是可用的,部分燃烧/氧化也可发生。
如上所述,加氢甲烷化是一个催化过程,似乎在浸渍碱金属的碳质载体的存在下发生至某种程度。标准气化通常是非催化性的(热过程),但是反应(I)可通过碱金属催化剂的存在而促进。
在反应器(100/200)中的温度和压力条件下,加氢甲烷化一般在床(110/210)中相对于常规气化占主导。加氢甲烷化条件一般公开于以下“催化剂床再循环/再生”部分结合的各个参考文献中。
期望地,反应器(100/200)中的条件使得浸渍碱金属的碳质载体的至少一部分碳成分(最初的碳成分,或更期望沉积在载体上的焦炭)加氢甲烷化以增加粗气态混合物的甲烷含量,并最终将气态粗产品流(50)从反应器(100/200)中取出。
在某些实施方案中,期望反应条件使得,碳材料在浸渍碱金属的碳质载体上的沉积,和碳从浸渍碱金属的碳质载体的消耗(通过气化、加氢甲烷化、燃烧和/或部分氧化),是实质上平衡的。
在其它实施方案中,期望反应条件使得碳材料在浸渍碱金属的碳质载体上的沉积大于碳从浸渍碱金属的碳质载体的消耗。在这种情况下,浸渍碱金属的碳质载体可通过溢出管线(35)从反应器(100/200)除去,在溢出管线(35)中其可通过比如在单独的反应器(未描述)中碳从浸渍碱金属的碳质载体的气化、加氢甲烷化、燃烧和/或部分氧化而再生,比如在以下“催化剂床再循环/再生”部分结合的多个参考文献中公开的单独的加氢甲烷化反应器中。
如上所述,反应器(100/200)中发生的反应具有合成气需求、蒸汽需求和热量需求。这些条件相组合是决定反应器(100/200)以及本方法其它部件的操作条件的重要因素。
通常,供应到反应器(100/200)的蒸汽:液体重烃进料的总重量比为约0.5或更大、或约0.75或更大、或约1或更大、或约1.5(或更大),至约6(或更小)、或至约5(或更小)、或至约4(或更小)、或至约3(或更小)、或至约2(或更小)。蒸汽需求应由分散重烃流(20)、过热气体进料流(25)和(若存在)富氧流(30)中的蒸汽满足;但是,若有需要,除这些气流外,还可将另外的蒸汽添加到反应器(100/200)中。
有利地,用于本方法的蒸汽由其它过程操作产生,通过过程热量捕获(比如在废热锅炉中产生,一般称为“过程蒸汽”或“过程-产生蒸汽”),而在一些实施方案中仅作为过程-产生蒸汽供应。例如,由换热器单元或废热锅炉产生,和/或来自其它下游气体加工步骤(比如转移和/或甲烷化可能存在于气态粗产品流(50)中的合成气成分)的过程蒸汽流,可最终注入反应器(100/200)中。
在某些实施方案中,本文描述的全过程至少实质上为蒸汽中性的,以致反应的蒸汽需求(压力和量)可通过与其中不同阶段的过程热的热交换满足;或是蒸汽阳性,以致生产并可以使用过量的蒸汽(例如用于发电)。期望地,过程-产生蒸汽占加氢甲烷化反应蒸汽需求的大于约95 wt%、或大于约97 wt%、或大于约99 wt%、或约100 wt%或更大。
同样如上所述,热量必须添加到反应器(100/200)中,因为反应器(100/200)中的反应是吸热的,加上会有过程热量损失。添加过热进料气流(25)和分散重烃流(20),加上碳在氧(其由富氧气流(30)(若存在)引入反应器(100/200))存在下的任选部分原位燃烧/氧化,应足以实质上满足反应的热量需求。
反应器(100/200)中的温度,可通过例如控制供应到反应器(100/200)的过热进料气流(25)的量和温度,以及任选的氧或单独供应的过热蒸汽的量(如上所述)控制。
全过程的结果是粗产品,其可从反应器(100/200)取出,为气态粗产品流(50),其通常包含超过痕量的甲烷、乙烷、丙烷、乙烯和丙烯,以及未反应的蒸汽、夹带的细粉,和任选的其它组分和污染物比如氢气、二氧化碳、一氧化碳、硫化氢和氨,这取决于进料和碳质载体使用的碳质材料的性质。
离开反应器(100/200)时,气态粗产品流(50)通常包含至少约30摩尔%(干基重)的低级烷烃(甲烷+乙烷+丙烷),和/或至少约8摩尔%的低级烯烃(乙烯+丙烯)。
浸渍碱金属的碳质材料和床
(110/210)
用于床(110/210)的浸渍碱金属的碳质材料是颗粒状碳质载体材料比如颗粒状生物质和/或非生物质,其含有有效催化反应器(100/200)中发生的反应的碱金属量,使得甲烷、乙烷、丙烷、乙烯和丙烯是反应得到的主要烃气态产物。
根据本领域已知的任何方法比如冲击粉碎和湿磨或干磨以产生一种或多种碳质颗粒,可通过粉碎和/或磨碎一种或多种碳质材料(单独或一起)来制备碳质载体。根据粉碎和/或磨碎碳质材料来源使用的方法,得到的碳质颗粒可以经过筛选(即根据尺寸分离)以提供用于反应器(100/200)的适当碳质载体。
本领域技术人员已知的任何方法皆可用于筛选颗粒。例如,筛选可通过过筛或使颗粒穿过一个筛子或数个筛子进行。筛选设备可包括铁格筛、棒条筛和金属丝网筛。筛子可静止或结合摇动或振动筛子的装置。或者,可使用分粒(classification)来分离碳质颗粒。分粒设备可包括矿石分选器、气体旋流器、旋液分离器、耙式分粒器、旋转滚筒筛或流化分粒器。碳质材料也可在磨碎和/或粉碎之前筛选或分粒。
通常,碳质载体按平均粒径为约25微米、或约45微米,至最多约2500微米、或最多约500微米的精细颗粒供应。本领域技术人员可容易确定碳质颗粒的适当粒径。例如,当使用流化床反应器时,这类碳质颗粒可具有以下的平均粒径,所述平均粒径可允许流化床反应器中使用的气体流速下碳质材料的初始流化。
期望的床(110)的粒径范围为Geldart A和Geldart B范围(包括两者间的重叠部分),这取决于流化条件,通常具有有限量的细(低于约25微米)材料和粗(大于约250微米)材料。
期望的床(210)的粒径范围为约40微米、或约200微米、或约400微米,至最多约2000微米、或最多约1000微米、或最多约800微米的范围,通常具有有限量的细材料和粗材料。
浸渍碱金属的碳质材料也可比如为加氢甲烷化炭副产品,比如由先前结合的参考文献中公开的各种加氢甲烷化过程产生。参见例如先前结合的US2010/0121125A1。
当使用新的碳颗粒(比如活性碳载体)时,催化剂可负载到材料上,如先前结合的US3958957所公开的,或对制备用于加氢甲烷化过程的颗粒状碳质材料所述的那样。参见例如US2009/0048476A1、US2010/0168495A1和US2010/0168494A1。
通常,存在于催化的颗粒中的碱金属为以下量,该量足以提供碱金属原子与碳原子在催化的颗粒中的比值范围为约0.01、或约0.05、或约0.1、或约0.2,至约1、或至约0.8、或至约0.6、或至约0.5。
合适的碱金属为锂、钠、钾、铷、铯及其混合物。特别有用的为钾源。合适的碱金属化合物包括碱金属碳酸盐、重碳酸盐、甲酸盐、草酸盐、酰胺、氢氧化物、醋酸盐或类似的化合物。例如,催化剂可包含碳酸钠、碳酸钾、碳酸铷、碳酸锂、碳酸铯、氢氧化钠、氢氧化钾、氢氧化铷或氢氧化铯的一种或多种,且特别是碳酸钾和/或氢氧化钾。
可使用任选的共催化剂或其它催化剂添加剂,比如以下在“催化剂床再循环/再生”部分结合的加氢甲烷化参考文献中公开的那些。
催化剂床再循环/再生
在流化床反应器比如反应器(100)中,由于污染物发生累积,通常需要时不时地去除和替换床(110)的一部分。床翻新的量和频率主要是有多少焦炭沉积和保持在碳质载体上的因素。其它因素包括,比如可沉积在载体颗粒上或“捆绑”催化剂组分的液体重烃进料的灰分和其它污染物成分的量。
在移动床反应器比如反应器(200)中,将床(210)的一部分除去并再循环。同样,床翻新的量和频率主要是有多少焦炭沉积和保持在碳质载体上的因素。
碳质载体可通过出口比如锁式料斗系统从反应器(100/200)定期或连续取出,不过本领域技术人员已知其它方法。
如上所述,从碱金属碳质载体除去焦炭沉积的一种方法是使碳从载体颗粒加氢甲烷化为富甲烷合成气和炭副产品。炭副产品可从加氢甲烷化反应器(未描述)除去并通过催化剂进料管线(40)再循环回反应器(100/200)。
催化气化/加氢甲烷化过程和条件公开于比如US3828474、US3998607、US4057512、US4092125、US4094650、US4204843、US4468231、US4500323、US4541841、US4551155、US4558027、US4606105、US4617027、US4609456、US5017282、US5055181、US6187465、US6790430、US6894183、US6955695、US2003/0167961A1、US2006/0265953A1、US2007/0000177A1、US2007/0083072A1、US2007/0277437A1、US2009/0048476A1、US2009/0090056A1、US2009/0090055A1、US2009/0165383A1、US2009/0166588A1、US2009/0165379A1、US2009/0170968A1、US2009/0165380A1、US2009/0165381A1、US2009/0165361A1、US2009/0165382A1、US2009/0169449A1、US2009/0169448A1、US2009/0165376A1、US2009/0165384A1、US2009/0217582A1、US2009/0220406A1、US2009/0217590A1、US2009/0217586A1、US2009/0217588A1、US2009/0218424A1、US2009/0217589A1、US2009/0217575A1、US2009/0229182A1、US2009/0217587A1、US2009/0246120A1、US2009/0259080A1、US2009/0260287A1、US2009/0324458A1、US2009/0324459A1、US2009/0324460A1、US2009/0324461A1、US2009/0324462A1、US2010/0121125A1、US2010/0120926A1、US2010/0071262A1、US2010/0168495A1、US2010/0168494A1、US2010/0292350A1、US2010/0287836A1、US2010/0287835A1、US2011/0031439A1、US2011/0062012A1、US2011/0062722A1、US2011/0064648A1、US2011/0088896A1、US2011/0088897A1、WO2010/048493A2和GB1599932;美国专利申请序列号12/970,105(代理人明细号FN-0057 US NP1,题为INTEGRATED ENHANCED OIL RECOVERY PROCESS(综合提高原油采收率的方法))和12/970,111(代理人明细号FN-0058 US NP1,题为INTEGRATED ENHANCED OIL RECOVERY PROCESS(综合提高原油采收率的方法)),它们各自提交于2010年12月16日;美国专利申请序列号13/031,486(代理人明细号FN-0059 US NP1,题为INTEGRATED HYDROMETHANATION FUEL CELL POWER GENERATION(综合加氢甲烷化燃料电池发电)),提交于2011年2月21日;美国专利申请序列号13/039,995(代理人明细号FN-0060 US NP1,题为INTEGRATED HYDROMETHANATION FUEL CELL POWER GENERATION(综合加氢甲烷化燃料电池发电)),提交于2011年3月3日;和美国专利申请序列号13/094,438(代理人明细号FN-0061 US NP1,题为HYDROMETHANATION OF A CARBONACEOUS FEEDSTOCK WITH VANADIUM RECOVERY(具有钒回收的碳质进料的加氢甲烷化)),提交于2011年4月26日。
加工后的富甲烷合成气可用作比如下述合成气产生器的进料,或可如以上结合的加氢甲烷化参考文献所述,另外纯化/处理/利用。
焦炭沉积也可通过热气化从碱金属碳质载体中除去,比如先前结合的US3816298所公开的那样。
由加氢甲烷化和热气化两者产生的固体是热的,并可再循环回反应器(100/200)作为热固体。这样做将减小反应器(100/200)中的反应的热量需求。
气体加工
离开反应器(100/200)的气态粗产品流(50)处于与反应器(100/200)近似的工作温度和压力下。
通常,气态粗产品流(50)将首先淬火至终止可消耗烯烃的反应的温度,比如低于约1100℉(约593℃),然后经受固体分离以除去夹带的固体。淬火和固体除去可以相关领域普通技术人员已知的任何方式进行,比如在结合到反应器(100/200)和/或在反应器(100/200)外部的细粉除去单元(未描绘)中进行。淬火可通过热交换发生,且固体除去可通过与水性(蒸汽或水)和/或有机介质(比如热解油或另外的残油进料)接触而在比如单个或多级旋流器中发生,得到的经淬火的气态粗产品流被送至进一步加工,而淬火介质和经分离的固体返回反应器(100/200)进一步加工。
在淬火之后可进行另外的细粉除去阶段,比如在另外的旋风分离器中,任选随后为文丘里洗涤器。
另外的热能可通过一个或多个换热器单元从经淬火的气态粗产品流中除去,且回收的热能可用于生成用于本过程其他地方的蒸汽。
取决于期望的最终产品,经淬火的气态粗产品流可经受本领域普通技术人员一般已知的另外的加工步骤,比如烯烃分离、脱硫、酸气去除、水/气转变和甲烷化。
在一个实施方案中,将烯烃和酸气体从经淬火的气态粗产品流中除去,并将至少一部分得到的降酸气流注入合成气产生器比如部分氧化反应器,以重组/部分氧化烃成分为另外的氢气和一氧化碳成分和热能,其可用于生成过热气体进料流(25)。一部分得到的降酸气流也可用于生成热能(比如通过燃烧或外部甲烷化)用于过热和/或蒸汽生成。
在一个实施方案中,合成气产生器使用气体-进料部分氧化/重组工艺,比如非催化气态部分氧化、催化自热重组或催化流-甲烷重组工艺。这些工艺一般在相关领域公知。参见比如,Rice和Mann,“ Autothermal Reforming of Natural Gas to Synthesis Gas, Reference: KBR Paper #2031(天然气到合成气的自热重组,参考文献:KBR Paper #_2031),” Sandia国家实验室公开号SAND2007-2331(2007); 和Bogdan,“ Reactor Modeling and Process Analysis for Partial Oxidation of Natural Gas(天然气部分氧化的反应器建模和过程分析)”,Febodruk, B.V. 出版, ISBN : 90-365-2100-9(2004)。
潜在的适合与本发明一起使用的技术和反应器可由以下市售可得:Royal Dutch Shell plc、Siemens AG、General Electric Company、Lurgi AG、Haldor Topsoe A/S、Uhde AG、KBR Inc.等。
在非催化气态部分氧化和自热重组中,富氧气流与气体进料流一起注入合成气产生器。蒸汽也可任选注入到合成气产生器中。在蒸汽-甲烷重组中,蒸汽与气体进料流一起注入反应器。有时,少量的其它气体比如二氧化碳、氢气和/或氮气也可注入合成气产生器。
各种反应器和技术的反应和其它工作条件、以及设备和结构一般为相关领域普通技术人员已知,在广义上对本发明并不至关重要。
除生成合成气以外,合成气产生器中的反应还产生热能。如上所述,一部分该热能可任选回收并用于比如由锅炉进水产生过程蒸汽或者加热/过热其它过程流。
多系列工艺
在本发明的方法中,每个过程可在一个或多个加工单元中进行。例如,可向一个或多个反应器供应来自一个或多个进料制备单元操作的进料。类似地,由一个或多个反应器产生的粗产品气流可在一个或多个气体加工单元中单独或通过它们的组合加工或纯化。
在某些实施方案中,所述方法使用两个或更多个反应器(例如2–4个反应器)。在这类实施方案中,在向多个反应器最终提供进料和过热气流的反应器之前,所述方法可含有发散性加工单元(即少于反应器的总数)或会聚性加工单元(即少于反应器的总数);和/或发散性或会聚性加工单元跟随用于加工由多个反应器产生的粗气态产品流的反应器。
当系统含有会聚性加工单元时,每个会聚性加工单元可选择为具有接受大于向会聚性加工单元的总进料流的1/n部分的能力,其中n为会聚性加工单元的数目。类似地,当系统含有发散性加工单元时,每个发散性加工单元可选择为具有接受大于供应会聚性加工单元的总进料流的1/m部分的能力,其中m为发散性加工单元的数目。
具体实施方案的实施例
本方法的一个具体实施方案是以下方法,其中方法为连续过程,其中步骤(a)、(b)、(d)和(e)以连续方式操作。
另一具体实施方案是以下方法,其中将液体重烃材料在一个或多个进料点注入反应器,将气态粗产品流在一个或多个取出点从反应器取出,并且从进料点到取出点的蒸气停留时间少于约2秒。
另一具体实施方案是以下方法,其中气态载体主要包含,或实质上包含,过热蒸汽或过热蒸汽与二氧化碳的混合物。
在另一具体实施方案中,过热气流包含来自基于气体的合成气产生器的一氧化碳和氢气,比如所述合成气产生器为利用非催化部分氧化过程或自热重组过程的产生器,其中将富氧气流与含甲烷的进料一起注入合成气产生器。在一个实施方案中,含甲烷的进料包含来自气态粗产品流的甲烷。在另一个实施方案中,加工气态粗产品流以除去实质部分的烯烃含量,以产生耗尽烯烃的产品流,并将至少一部分耗尽烯烃的产品流作为含甲烷的进料注入合成气产生器。
另一具体实施方案如下,其中将富氧气流周期或连续供应到反应器,且提供的氧的量随过程控制变化,以比如辅助控制反应器的温度。随着氧气供应到反应器,碳被部分氧化/燃烧以产生热能(以及通常一些量的一氧化碳和氢气)。供应到反应器的氧的量可增大或减小以增加消耗的碳量,并因此增加在反应器中原位产生的热能的量。在这种情况下,该原位产生的热能减小反应的热量需求,因此减小在过热气体进料流中供应的热能的量。
另一具体实施方案如下,其中将至少一部分热能从气态粗产品流回收,且至少一部分回收的热能用于生成本方法使用的蒸汽。
另一个具体实施方案如下,其中将床的溢出流从反应器取出,并将溢出流加氢甲烷化以生成富集甲烷的合成气流和副产品炭。在一个实施方案中,至少一部分富集甲烷的合成气用作用于合成气产生器的含甲烷的进料。在另一个实施方案中,将至少一部分副产品炭返回反应器作为再循环催化剂床。
另一个具体的实施方案如下,其中将床的溢出流从反应器取出,并将溢出流气化以生成包含氢气、一氧化碳和热能的合成气流。在一个实施方案中,过热气体进料流包含至少一部分合成气流。
实施例
使2英寸内径,4英尺高的柱装满浸渍钾催化剂的碳炭(900g)。所述炭来自粉河盆地(PRB)煤,并含有约0.29的K/C含量。也用未催化的活性碳作为床材料进行一个试验。
使用具有以下大致组成的石油残留物:C=89.3%;H=8.6%;S=1.8%;N=0.4%;V=80 ppm。
通过使蒸汽、氢气、一氧化碳和氮气的过热气体混合物流入柱的底部使碳炭在床中流化。
使石油残留物通过与过热蒸汽混合而雾化,并在1300℉下注入柱中。
反应器中的温度为约1300℉,且气体速度为约0.4-1.25英尺/秒,引起雾化的残留物进料的停留时间为约1秒。
由于进料注射口因焦炭形成导致的堵塞,每个试验持续约2小时。
在每个试验后,使用红外光谱分析法(IR)和气相色谱法(GC)分析获得的气体的烃种类。在回收气体和床材料上也进行碳平衡。通常,达到的碳平衡>90%。
实施例1
第一个试验在1300℉和150 psig下进行以比较催化床相对于未催化的床的效果。表1提供了结果。
从结果可以看出,床材料中催化剂的存在对进料向低级烯烃和烷烃的转化具有显著影响。
实施例2
四个试验在上述条件下用催化床进行,但是压力改为–50 psig、150 psig、295 psig和500 psig。
表2和3提供了结果。
从结果可以看出,压力对产品分布具有显著影响。有利地,较高压力似乎导致减少的焦炭形成,因此导致较高的总期望产品产率/单位进料(轻烷烃和烯烃)。
Claims (11)
1.由液体重烃材料生成气态粗产品流的方法,所述方法包含以下步骤:
(a)将液体重烃材料分散在气态载体中以生产分散的重烃进料;
(b)将包含热能和蒸汽,以及任选的一氧化碳和氢气,的过热气体进料流引入含有浸渍碱金属的碳载体床的反应器中;
(c)任选将富氧流引入反应器中以产生热能,并任选原位产生一氧化碳和氢气;
(d)在浸渍碱金属的碳载体床的存在下,使分散的重烃进料与蒸汽、一氧化碳和氢气在高压和1100℉-1400℉的温度下接触,以生成粗气态混合物,其包含甲烷、乙烯和丙烯的一种或两种、乙烷和丙烷的一种或两种;和
(e)从反应器中取出粗气态混合物流作为气态粗产品流,
其中步骤(d)的反应有合成气需求,且合成气需求至少实质上由可存在于过热气体进料流的一氧化碳和氢气,和可在步骤(c)中生成的一氧化碳和氢气满足。
2.权利要求1的方法,其特征在于将液体重烃材料在一个或多个进料点注入反应器,将气态粗产品流在一个或多个取出点从反应器中取出,且从进料点到取出点的蒸气停留时间小于2秒。
3.权利要求1的方法,其特征在于粗气态产物流包含至少30摩尔%的甲烷+乙烷+丙烷(干基重)和至少8摩尔%的乙烯+丙烯(干基重)。
4.权利要求1的方法,其特征在于将液体重烃材料在气态载体中雾化以生产分散的重烃进料。
5.权利要求1的方法,其特征在于气态载体主要包含过热蒸汽。
6.权利要求1的方法,其特征在于高压最多1000psig。
7.权利要求1的方法,其特征在于将富氧气流注入反应器。
8.权利要求1的方法,其特征在于反应器在反应器底部包含收集区,并将富氧气流注入收集区。
9.权利要求1的方法,其特征在于将床的溢出流从反应器取出,并将溢出流加氢甲烷化以生成富集甲烷的合成气流和副产品炭。
10.权利要求9的方法,其特征在于将至少一部分副产品炭返回反应器作为再循环催化剂床。
11.权利要求1-10中任一项的方法,其特征在于所述液体重烃材料包括选自真空残油;常压残油;重的和还原的石油原油;柏油、沥青和石油沥青;沥青砂油;页岩油;催化裂解方法的塔底油;和煤液化塔底油。
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AU2011258204B2 (en) | 2013-11-07 |
JP5559428B2 (ja) | 2014-07-23 |
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KR20130014578A (ko) | 2013-02-07 |
KR101506381B1 (ko) | 2015-03-26 |
US8653149B2 (en) | 2014-02-18 |
JP2013527296A (ja) | 2013-06-27 |
WO2011150217A2 (en) | 2011-12-01 |
CA2793893A1 (en) | 2011-12-01 |
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