CN116731756A - 重质船用燃料油组合物 - Google Patents

重质船用燃料油组合物 Download PDF

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Publication number
CN116731756A
CN116731756A CN202310459703.XA CN202310459703A CN116731756A CN 116731756 A CN116731756 A CN 116731756A CN 202310459703 A CN202310459703 A CN 202310459703A CN 116731756 A CN116731756 A CN 116731756A
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iso
oil
marine fuel
fuel oil
heavy
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Inventor
伯特兰·R·克鲁斯曼
迈克尔·J·摩尔
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Magema Technology LLC
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Magema Technology LLC
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Publication of CN116731756A publication Critical patent/CN116731756A/zh
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/04—Liquid carbonaceous fuels essentially based on blends of hydrocarbons
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    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
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Abstract

一种用于减少符合ISO 8217标准的原料重质船用燃料油(原料)中的环境污染物的方法，所述方法包括：将一定量的所述原料与一定量的活化气体混合物混合，得到原料混合物；使所述原料混合物与一种或多种催化剂接触以由所述原料混合物形成工艺混合物；将所述工艺混合物的产品重质船用燃料油液体(产品)组分与所述工艺混合物的气态组分和副产品烃类分离，和排出所述产品。所述产品符合对于残渣船用燃料油的ISO标准，并且最大硫含量在0.05％wt至0.50％wt的范围内。所述产品可用作符合标准的低硫或超低硫重质船用燃料油或者用作其共混料。还公开了用于执行所述方法的装置。

Description

重质船用燃料油组合物
本申请为2018年02月12日提交的申请号为201880019191.2且发明名称为“重质船用燃料油组合物”的专利申请的分案申请。
背景技术
有两种船用燃料油类型，基于馏分油的船用燃料油和基于残渣油的船用燃料油。基于馏分油的船用燃料油也称为船用瓦斯油(Marine Gas Oil，MGO)或船用柴油(MarineDiesel Oil，MDO)，包括在炼油厂通过蒸馏工艺中从原油中分离的石油馏分。瓦斯油(也称为中等柴油)是沸程和粘度在含有C10-19烃的混合物的煤油和润滑油之间的石油馏分中间物。瓦斯油(用于家用供暖，以及用于重型设备，如起重机、推土机、发电机、bobcat、拖拉机和联合收割机。通常，从渣油中最大化回收瓦斯油是炼油厂对材料的最经济的使用，因为其可以将瓦斯油裂化成有价值的汽油和馏分油。柴油与瓦斯油非常相似，柴油主要含有C10-19烃的混合物，其包含约64％的脂族烃、1-2％的烯烃和35％的芳烃。船用柴油机可含有高达15％的残渣工艺流，和任选地多至不大于5％体积的多环芳烃(沥青质)。柴油燃料主要用作陆地运输燃料和作为与煤油的共混组分以形成航空喷气燃料。
基于渣油的燃料油或重质船用燃料油(HMFO)包括工艺渣油—即使在真空条件下也不会沸腾或蒸发的馏分的混合物，并且沥青质含量在3至20重量百分比(％wt)的范围内。沥青质是大而复杂的多环烃，具有形成复杂和蜡状沉淀物的倾向。一旦沥青质沉淀出来，其非常难以再溶解，并且在海运业和船用仓储燃料业被描述为燃料箱污泥。
大型远洋轮船依靠HMFO为大型二冲程柴油发动机提供动力超过50年。HMFO是原油精炼过程中产生的芳烃、馏分油和渣油的共混物。HMFO制剂中包含的典型流包括：常压塔底物(即常压渣油)、真空塔底物(即减压渣油)、减粘裂化炉渣油、FCC轻循环油(LCO)、FCC重循环油(HCO)(也称为FCC底物)、FCC淤浆油、重质瓦斯油和延迟裂化油(DCO)、多环芳烃、回收的陆地运输机油和小部分(小于20％体积)的切削油、煤油或柴油，以达到期望的粘度。HMFO的芳烃含量高于上述船用馏分燃料。HMFO组合物是复杂的并且随着原油来源和用于从原油桶中提取最大价值的炼油工艺而变化。组分的混合物通常表征为粘性的、高硫和金属含量和高沥青质，使HMFO成为每桶的价值低于原料原油本身的炼油工艺的一种产品。
行业统计表明，约90％的销售的HMFO含有3.5重量％的硫。估计全球每年的HMFO消费量为约3亿吨，航运业每年的二氧化硫年产量估计超过2100万吨。HMFO在船上燃烧产生的排放对全球空气污染和当地空气污染水平的影响很大。
颁布了由国际海事组织(IMO)执行的国际防止船舶造成污染公约MARPOL来防止船舶造成污染。1997年，MARPOL增加了新附则：船舶空气污染防治条例—附则VI，以尽量减少船舶的气载排放(SOx、NOx、ODS、VOC)及其对空气污染的危害。2008年10月通过了修订后的附则VI，其包括严格的排放限制，自2010年7月1日起生效(以下简称附则VI(修订版)或简称附则VI)。
MARPOL附则VI(修订版)对指定的排放控制区域(ECA)的船舶运营制定了一套严格的排放限制。MARPOL附则VI(修订版)下的ECA是：i)波罗的海区域-如MARPOL附则I中所限定的-仅SOx；ii)北海区域-如MARPOL附则V中所限定的-仅SOx；iii)北美-如MARPOL附则VI附录VII中所限定的-SOx、NOx和PM；和iv)美国加勒比海区域-如MARPOL附则VI附录VII所限定的-SOx、NOx和PM。
附则VI(修订版)根据美国船舶污染防治法令(APPS)编纂。在APPS的授权下，美国环境保护署(EPA)与美国海岸警卫队(USCG)协商颁布了一些法规，其通过引用并入了MARPOL附则VI(修订版)的全文。参见40C.F.R.§1043.100(a)(1)。2012年8月1日，在美国水域/ECA运行的船舶上使用的所有船用燃料油的最大硫含量不得超过1.00％wt(10,000ppm)，并且在2015年1月1日，北美ECA中使用的所有船用燃料油的最大硫含量降至0.10％wt(1,000ppm)。在实施时，美国政府表示船舶经营者必须大力为0.10％wt(1,000ppm)US ECA船用燃料油硫标准做准备。为了鼓励符合标准，EPA和USCG拒绝将符合标准的低硫燃料油的成本视为声称无法购买符合标准的燃料油的有效基础。在过去五年中，为满足海洋行业对低硫HMFO的要求，有着非常强大的经济刺激，但技术上可行的方案尚未实现。对制造符合MARPOL附则VI排放要求的低硫HMFO的工艺和方法存在持续和迫切的需求。
由于ECA，在这些ECA外部和内部运行的所有远洋船舶必须以不同的船用燃料油运行，以符合各自的限制并实现最大的经济效益。在这种情况下，在进入ECA之前，船舶必须完全转换为使用符合ECA标准的船用燃料油，并具有在船上实施的书面程序来说明如何进行。类似地，直到离开ECA之后才进行从使用符合ECA标准的燃油回到HMFO的转换。每次转换时，都要求记录船上符合ECA标准的燃油的量，以及船舶在进入这些区域之前完成转换或在离开之后开始转换的日期、时间和位置。这些记录应在船旗国规定的日志中，在没有任何具体要求的情况下记录被做出，例如在船舶附件I油类记录簿中。
附则VI(修订版)还对船舶废气和颗粒物的硫氧化物和氮氧化物的排放设定了全球限制，并禁止故意排放臭氧消耗物质，例如氢氯氟烃(hydro-chlorofluorocarbon)。根据经修订的MARPOL附则VI，HMFO的全球硫含量降至3.50％wt，自2012年1月1日生效；然后进一步降低至0.50％wt，自2020年1月1日生效。这项规定一直是海运业和船用仓储燃料业讨论的主题。在全球限制下，所有船舶必须使用硫含量不大于0.50％wt的HMFO。IMO多次向海运业表示，无论符合标准的燃料的可用性或符合标准的燃料的价格如何，符合的HMFO的0.50％wt的硫限制将在2020年1月1日生效，并且IMO希望燃料油市场解决这个要求。为满足国际海洋行业对低硫HMFO的需求，已有非常强大的经济刺激，但技术上可行的解决方案尚未实现。对制造符合MARPOL附则VI排放要求的低硫HMFO的工艺和方法存在持续和迫切的需求。
IMO第14条规定了需要遵守的限值和手段。这些可以分为称为初级(其中避免形成污染物)或二级(其中形成污染物但在将废气流排出到大气之前除去)的方法。没有关于任何初级方法的指南(其可能包括例如船上共混液体燃料油或双燃料(气体/液体)的使用)。在二级控制方法中，已经对废气净化系统采用了指南(MEPC.184(59))；在使用这种安排时，除了系统认证之外，对仓储的燃料油的含硫量没有限制。由于众多技术和经济原因，二级控制已被大部分航运公司拒绝，并且并未在海运业广泛采用。二级控制的使用不被海运业视为实用的方案。
初级控制方案：符合MARPOL要求的初级控制方案的重点是基于用替代燃料代替HMFO来降低燃烧前船用燃料组分中的硫含量。然而，从HMFO到替代燃料的切换给船舶经营者带来了一系列问题，其中许多仍然不为航运业或炼油业所理解。由于当船舶切换燃料时船舶推进系统(即燃料系统，发动机等)的潜在风险，所以必须安全有效地完成转换过程以避免任何技术问题。然而，在适应基于海运业所使用的HMFO的数十年的航运基础设施和油仓系统中，每种替代燃料在经济和技术上均面临困难。
LNG：航运业中最普遍的初级控制方案是采用LNG作为主要或HMFO的添加剂燃料。越来越多的船舶使用液化天然气(LNG)作为主要燃料。天然气作为燃气涡轮机和柴油发动机的船用燃料导致可忽略不计的硫氧化物排放。2015年采用的由IMO开发的使用气体和其他低闪点燃料船舶国际规则(IGF规则)中已经认识到天然气的好处。然而，LNG为海运业带来了经营挑战，包括：在海洋环境中在船上储存低温液体将需要对船舶的油仓燃料储存和燃料输送系统进行大量翻新和更换；LNG的供应远达不到在世界主要港口普遍存在的程度；需要在出海前更新船员资格和操作LNG或双燃料发动机的培训。
无硫生物燃料：另一个提出的符合MARPOL要求的初级方案是用无硫生物燃料代替HMFO。生物柴油在代替石油衍生柴油中的成功有限，但供应依然受到限制。甲醇已被用于北海ECA的一些短途海运服务，用于渡轮和其他沿岸船舶。生物燃料(例如生物柴油或甲醇)的广泛采用给船的所有者和船用燃料行业带来了许多挑战。这些挑战包括：需要燃料系统兼容性和现有燃料系统的适应性；在甲醇和生物柴油的长期储存中由水和生物污染造成的污染；每吨甲醇和生物柴油的热含量远低于HMFO；并且甲醇具有高蒸汽压并且存在严重的闪火安全问题。
用船用瓦斯油或船用柴油替代重质燃料油：第三种提出的初级方案是简单地用船用瓦斯油(MGO)或船用柴油(MDO)代替HMFO。第一个主要困难是占MGO和MDO的超过90％的馏分材料的全球供应的限制。据报道，生产MGO的有效备用产能每年不到1亿公吨，导致每年船用燃料每年超过2亿公吨的缺口。炼油厂不仅缺乏增加MGO产量的能力，而且没有经济动力，因为从陆地运输系统(即卡车、火车、公共交通系统、重型建筑设备等)的超低硫柴油可以获得更高的价值和更高的利润。
共混：另一种初级方案是将HMFO与低硫含量燃料如低硫船用柴油(0.1％wt硫)共混，以获得硫含量为0.5％wt的产品HMFO。在直接共混方法(基于线性共混)中，每1吨HSFO(3.5％硫)需要7.5吨具有0.1％wt S的MGO或MDO材料以达到0.5％wt HMFO的硫含量。燃料共混领域的技术人员将立即理解，共混会损害HMFO的关键性质，特别是粘度和密度大幅改变。此外，共混过程会导致具有可变粘度和密度的燃料，其可能不再满足HMFO的要求。
当将共混的HMFO引入不是为共混HMFO设计的燃料仓储基础设施和船载系统时，可能会出现进一步的复杂情况。当两种燃料混合时存在不兼容的真实风险。将主要为链烷烃型的馏分燃料(MGO或MDO)与具有高芳烃含量的HMFO共混通常与沥青质的差溶解性相关。共混燃料可能导致沥青质和/或高度链烷烃材料从馏分油材料中沉淀，形成难处理的燃料箱污泥。燃料箱污泥导致过滤器和分离器、输送泵和管线的堵塞，储存罐中的污泥堆积，燃料喷射泵的粘连(柱塞和桶上的沉积物)以及堵塞的燃料喷嘴。对于主推进系统的这种风险是公海的货船不可接受的。
最后将HMFO与海洋馏分油产品(MGO或MDO)共混在经济上是不可行的。搅拌机将采用高价值产品(0.1％ S船用瓦斯油(MGO)或船用柴油(MDO))并将其以7.5比1与低价值高硫HMFO混合，以产生最终符合IMO/MARPOL标准的HMFO(即0.5％wt S低硫重质船用燃料油-LSHMFO)。预计LSHMFO将以比单独两种共混料的价值低的每吨价格出售。
渣油加工。在过去的几十年里，炼油行业集中在重油(原油、劣质油(distressedoil)或渣油)加工相关的研究工作的努力方向在于提升这些低价值炼油工艺油的性能，以产生具有更高价值的轻油。挑战在于原油、劣质油和渣油可能不稳定并含有高含量的硫、氮、磷、金属(尤其是钒和镍)和沥青质。大部分镍和钒难以去除与卟啉的螯合物。钒和镍卟啉和其他金属有机化合物是炼油厂中催化剂污染和腐蚀问题的原因。去除硫、氮和磷，因为它们是常压或真空蒸馏塔下游工艺中使用的贵金属(铂和钯)催化剂的众所周知的毒物。
处理大气或真空渣油流的困难已为人所知多年，并且已成为大量研究和调查的主题。已经开发了许多渣油转化方法，其目标是相同的，1)产生更有价值的，优选馏分油范围的烃产物；2)将污染物如硫、氮、磷、金属和沥青质浓缩成一种形式(焦炭、重质焦化器渣油、FCC淤浆油)，以从炼油厂流中除去。炼油行业众所周知和公认的做法是提高反应强度(升高的温度和压力)，以生产更轻并且更纯的烃产品，延长催化剂的使用寿命，并从炼油厂流中去除硫、氮、磷、金属和沥青质。
在这些方法中还众所周知的是，原料的性质对所生产的产品、催化剂寿命以及最终该方法的经济可行性具有显著影响。在代表性的技术论文Residual-Oil HydrotreatingKinetics for Graded Catalyst Systems:Effects of Original and TreatedFeedstocks中，陈述了“取决于用于测试的原料，结果显示了活性的显著变化。本研究证明了正确选择用于渣油加氢处理的分级催化剂体系的候选催化剂的性能评价和筛选中使用的原料的重要性”。由此，本领域技术人员将理解，常压渣油的成功加氢处理所需的条件不适于减压渣油的成功加氢处理，减压渣油的成功加氢处理不适于减粘裂化炉渣油的成功加氢处理，以此类推。成功的反应条件取决于原料。因此，现代复杂的炼油厂具有多个加氢处理单元，每个单元针对特定的烃流，目的是产生期望的和有价值的轻质烃，并提供下游工艺可接受的产品。
处理重质油残余物和其他重质烃的另一个困难是每种炼油厂中间物流固有的不稳定性。本领域技术人员理解，将每种炼油厂流分开处理有许多实际原因。其中一个原因是每个流中包含的沥青质的不可预测性。沥青质是大而复杂的烃，倾向于从炼油厂烃流中沉淀出来。本领域技术人员知道，即使组分或物理条件(温度、压力)的微小变化也会使沥青质沉淀，否则沥青质溶解在溶液中。一旦从溶液中沉淀出来，沥青质可能快速阻塞重要管线、控制阀、涂覆关键传感装置(即温度和压力传感器)，并且通常导致严重且高花费的破坏和关闭单元或整个炼油厂。由于这个原因，炼油厂长期实践是不共混中间产物流(例如常压渣油、减压渣油、FCC淤浆油等)，并在不同的反应器中处理每个流。
总之，自MARPOL标准宣布降低HMFO的全球硫含量以来，原油炼油厂尚未进行技术努力以产生HMFO的低硫替代品。尽管具有强的政府和经济激励以及国际海运业的需求，但炼油厂几乎没有经济理由解决从HMFO中去除环境污染物的问题。相反，全球炼油工业一直致力于通过产生轻质烃(即柴油和汽油)并将环境污染物浓缩到越来越低价值的流(即渣油)和产物(石油焦炭，HMFO)中来从每桶石油中产生更大的价值。航运公司专注于短期方案，例如安装洗涤装置，或采用更昂贵的低硫船用柴油和船用瓦斯油的有限使用作为HMFO的替代品。在公海上，大多数(如果不是所有)主要航运公司继续使用最经济可行的燃料，即HMFO。对于从HMFO中去除环境污染物(即硫、氮、磷、金属，尤其是钒和镍)而不改变使HMFO成为为远洋船舶提供动力的最经济实用手段的品质和特性的工艺和装置仍然存在长期和未满足的需求。此外，对于也符合可销售的ISO 8217HMFO所需的主要性质的符合IMO的低硫(即0.5％wt硫)或超低(0.10％wt硫)HMFO仍存在长期和未满足的需求。
发明内容
一般目标是在使HMFO的期望性质的变化最小化和使不必要的副产品烃(即轻质烃(C1-C8)和野生石脑油(C5-C20))的产生最小化的方法中减少重质船用燃料油(HMFO)中的环境污染物。
第一方面和说明性实施方案包括减少原料重质船用燃料油中的环境污染物的方法，所述方法包括：将一定量的原料重质船用燃料油与一定量的活化气体混合物混合，得到原料混合物；使所述原料混合物与一种或多种催化剂接触以由原料混合物形成工艺混合物；接收所述工艺混合物并将所述工艺混合物的产品重质船用燃料油液体组分与所述工艺混合物的气态组分和副产品烃组分分离，和排出所述产品重质船用燃料油。
第二方面和说明性实施方案包括在本文中称为重质船用燃料组合物的烃燃料组合物，其基本上由至少大部分体积，优选85体积％，更优选至少90体积％，并且最优选至少95体积％的产品重质船用燃料油组成，所述产品重质船用燃料油由所公开的用于减少原料重质船用燃料油中的环境污染物的方法产生，或者任选地由体现所述方法的装置产生。重质船用燃料成分中的余量(balance)体积可以是与产品HMFO一起的稀释剂材料，但不会导致混合物不符合对于残渣船用燃料的主要性质的ISO 8217:2017标准，并实现硫含量低于全球MARPOL标准的0.5％wt硫(ISO 14596或ISO 8754)。
第三方面和说明性实施方案包括用于减少原料HMFO中的环境污染物并生产产品HMFO的装置。该说明性装置包括第一容器，与第一容器流体连通的第二容器和与第二容器流体连通的第三容器，和来自第三容器的用于排出产品HMFO的排出管线。第一容器接收与一定量的活化气体混合物混合的一定量的原料HMFO，并在某些工艺条件下使所得混合物与一种或多种催化剂接触以形成工艺混合物。第二容器从第一个容器接收工艺混合物，使工艺混合物中的液体组分与大部分气态组分分离。大部分气态组分被输送用于进一步处理。液体组分送至第三容器，其从加工的产品HMFO中分离出任何残留的气态组分和任何副产品烃组分(主要是轻质烃和野生石脑油)，产品HMFO随后被排出。
附图说明
图1是用于生产产品HMFO的方法的过程流程图。
图2是用于生产产品HMFO的设备的基本示意图。
具体实施方式
如本文所述的发明构思利用了本领域技术人员应该熟知的术语，但是使用了具有特定预期含义的某些术语，并且这些术语定义如下：
重质船用燃料油(HMFO)是除了环境污染物的浓度水平外符合对于残渣船用燃料的主要性质的ISO 8217:2017标准的石油产品燃料。
环境污染物是在燃烧时会导致形成SOx、NOx和颗粒物质的HMFO的有机和无机成分。
原料HMFO是除了环境污染物的浓度外符合对于残渣船用燃料的主要性质的ISO8217:2017标准的石油产品燃料，优选地原料HMFO的硫含量大于全球MARPOL标准的0.5％wt硫，并且优选地硫含量(ISO 14596或ISO 8754)在5.0％wt至1.0％wt的范围内。
重质船用燃料组合物是基本上由至少85体积％的产品HMFO和不大于15体积％的稀释剂材料组成的烃燃料组合物，其符合对于残渣船用燃料的主要性质的ISO 8217:2017标准，并且硫含量低于全球MARPOL标准的0.5％wt硫(ISO 14596或ISO 8754)。
稀释剂材料是混合或组合或添加到产品HMFO中的烃材料或非烃材料，或者悬浮在产品HMFO中的固体，其存在不会导致混合物不符合对于残渣船用燃料的主要性质的ISO8217:2017标准并且不会导致硫含量大于全球MARPOL标准的0.5％wt硫(ISO 14596或ISO8754)。
产品HMFO是一种石油产品燃料，其符合对于残渣船用燃料的主要性质的ISO8217:2017标准，并且实现了硫含量低于全球MARPOL标准的0.5％wt硫(ISO 14596或ISO8754)，并且优选地最大硫含量(ISO 14596或ISO 8754)在0.05％wt至1.0％wt的范围内。
活化气体：是在该方法中与催化剂结合使用以从原料HMFO中除去环境污染物的气体混合物。
流体连通：是将流体(液体、气体或其组合，其可具有悬浮的固体)从第一个容器或位置转移到第二容器或位置的能力，这可能包括由管(也称为管线)、阀芯(spool)、阀、中间储罐或缓冲罐(也称为桶)构成的连接。适售品质：是残渣船用燃料油的品质水平，使得燃料适合其意图服务的一般目的(即用作船舶的残渣燃料来源)，并且可以作为重质或残渣海用船舱燃料商业销售，并且可与重质或残渣海用船舱燃料互换。
Bbl或bbl：是油的标准体积量度；1bbl＝0.1589873m3；或1bbl＝158.9873升；或1bbl＝42.00US液体加仑。
Bpd：是每天Bbl的缩写。
SCF：是气体的标准立方英尺的缩写；标准立方英尺(在14.73psi和60℉下)等于0.0283058557标准立方米(在101.325kPa和15℃下)。
在参考附图的本描述中更详细地说明了本发明构思，其中图1示出了根据第一说明性实施方案的用于减少原料HMFO中的环境污染物并生产产品HMFO的一般方框化工艺流程。将预定体积的原料HMFO(2)与预定量的活化气体(4)混合，得到原料混合物。除了环境污染物外，所使用的原料HMFO通常符合在其他方面符合ISO 8217:2017标准的残渣船用燃料油的主要物理和某些关键化学性质。更具体地，当环境污染物是硫时，原料HMFO中的硫浓度可以在5.0％wt至1.0％wt的范围内。原料HMFO应具有符合ISO 8217:2017标准的HMFO所需的主要物理性质：180mm2/s至700mm2/s范围内的50℃下的最大运动粘度(ISO 3104)，991.0kg/m3至1010.0kg/m3范围内的15℃下的最大密度(ISO 3675)，780至870的CCAI，和不低于60.0℃的闪点(ISO 2719)。与颗粒材料(PM)的形成相关的原料HMFO的其他性质包括：0.10％wt的最大总沉积物-老化(ISO 10307-2)，18.00％wt至20.00％wt的范围内的最大碳残留-微量法(ISO 10370)，和60mg/kg的最大铝和硅(ISO 10478)含量。可能存在于原料HMFO中的超过ISO要求的除硫之外的潜在环境污染物可包括钒、镍、铁、铝和硅，其通过本发明的方法显著减少。然而，本领域技术人员将理解，钒含量用作这些其他环境污染物的一般指标。在一个优选的实施方案中，钒含量符合ISO标准，因此原料MHFO的最大钒含量(ISO14597)在350mg/kg至450mg/kg的范围内。
至于活化气体的性质，活化气体应选自氮气、氢气、二氧化碳、气态水和甲烷的混合物。活化气体中的气体混合物应具有大于活化气体混合物的总压力(P)的80％的理想的氢气分压(pH2)，更优选地其中活化气体具有大于活化气体混合物的总压力(P)的95％的理想的氢气分压(pH2)。本领域技术人员将理解，活化气体的摩尔含量是另一个标准，活化气体应具有为活化气体混合物的总摩尔数的80％至100％的氢摩尔分数，更优选地，其中活化气体具有为活化气体混合物总摩尔数的80％至99％的氢摩尔分数。
将原料混合物(即原料HMFO与活化气体的混合物)升至温度和压力的工艺条件，并引入第一容器，优选反应器容器，然后使原料混合物与一种或多种催化剂(8)接触，以由原料混合物形成工艺混合物。
选择工艺条件，使得活化气体的量与原料HMFO的量的比率为250scf气体/bbl原料HMFO至10,000scf气体/bbl原料HMFO；优选在2000scf气体/bbl原料HMFO之间；1至5000scf气体/bbl原料HMFO，更优选在2500scf气体/bbl原料HMFO至4500scf气体/bbl原料HMFO之间。选择工艺条件，使得第一容器中的总压力为250psig至3000psig；优选1000psig至2500psig，更优选1500psig至2200psig。选择工艺条件，使得第一容器内的指示温度在500℉至900℉之间，优选在650℉至850℉之间，更优选在680℉和800℉之间。选择工艺条件，使得第一容器内的液时空速在0.05油/小时/m3催化剂至1.0油/小时/m3催化剂之间；优选在0.08油/小时/m3催化剂至0.5油/小时/m3催化剂之间；更优选在0.1油/小时/m3催化剂至0.3油/小时/m3催化剂之间，以实现脱硫，其中产品硫含量低于0.5％wt。
本领域技术人员将理解，确定工艺条件以考虑单元的液压容量。处理单元的示例性液压容量可以为100bbl原料HMFO/天至100,000bbl原料HMFO/天，优选1000bbl原料HMFO/天至60,000bbl原料HMFO/天，更优选5,000bbl原料HMFO/天至45,000bbl原料HMFO/天，甚至更优选10,000bbl原料HMFO/天至30,000bbl原料HMFO/天。
该方法可以使用选自由以下组成的组的一种或多种催化剂体系：沸腾床(ebulliated bed)负载的过渡金属多相催化剂，固定床负载的过渡金属多相催化剂，和沸腾床负载的过渡金属多相催化剂和固定床负载的过渡金属多相催化剂的组合。本领域技术人员将理解，固定床负载的过渡金属多相催化剂在技术上最容易实施并且是优选的。过渡金属多相催化剂包含多孔无机氧化物催化剂载体和过渡金属催化剂。多孔无机氧化物催化剂载体是选自由氧化铝、氧化铝/氧化硼载体、含有含金属硅铝酸盐的载体、氧化铝/磷载体、氧化铝/碱土金属化合物载体、氧化铝/二氧化钛载体和氧化铝/氧化锆载体组成的组的至少一种载体。催化剂的过渡金属组分是选自由周期表第6、8、9和10族组成的组的一种或多种金属。在优选和说明性实施方案中，过渡金属多相催化剂是多孔无机氧化物催化剂载体和过渡金属催化剂，其中优选的多孔无机氧化物催化剂载体是氧化铝，并且优选的过渡金属催化剂是Ni—Mo、Co—Mo、Ni—W或Ni-Co—Mo。
将工艺混合物(10)从第一容器(8)中取出并不与一种或多种催化剂接触，并通过流体连通输送至第二容器(12)，优选气液分离器或热分离器和冷分离器，用于将工艺混合物的液体组分(14)与工艺混合物的大部分气态组分(16)分离。在本方法的界区(batterylimit)外处理气态组分(16)。这样的气态组分可包含活化气组分和作为来自该方法的副产品烃的一部分而不可避免地形成的较轻烃(主要是甲烷、乙烷和丙烷，但还有一些野生石脑油)的混合物。
液体组分(16)通过流体连通送至第三容器(18)，优选燃料油产品汽提塔系统，用于将任何残余气态组分(20)和副产品烃组分(22)与产品HMFO(24)分离。残余气态组分(20)可以是选自由氮气、氢气、二氧化碳、硫化氢、气态水、C1-C5轻质烃组成的组的气体的混合物。该残余气体在本方法的界区外进行处理，与从第二容器(12)中的工艺混合物(10)中除去的其他气态组分(16)组合。在方法中不可避免地形成的液体副产品烃组分(22)是可冷凝烃，可以是选自由C5-C20烃(野生石脑油)(石脑油-柴油)和其他可冷凝轻质液体(C4-C8)烃组成的组的混合物，其可用作发动机燃料混合池的一部分使用，或作为汽油和柴油混合组分在公开市场上出售。
作为旁注，残余气态组分是选自由氮气、氢气、二氧化碳、硫化氢、气态水、轻质烃组成的组的气体的混合物。胺洗涤器将有效地除去硫化氢含量，其然后可以使用本领域技术人员熟知的技术和方法处理。在一个优选的说明性实施方案中，使用熟知的Claus方法将硫化氢转化为元素硫。一个替代实施方案利用专有方法将硫化氢转化为氢硫酸。无论哪种方式，在船舶发动机中燃烧HMFO之前，硫都不会进入环境。经净化的气体可以排放、燃烧或更优选地再循环回用作活化气体。
副产品烃组分是C5-C20烃(野生石脑油)(石脑油-柴油)的混合物，可以直接进入发动机燃料混合池，或穿过围栏出售给相邻的炼油厂，或甚至用于燃烧加热器和燃气轮机为方法提供热量和动力。这些由加氢裂化反应产生的副产品烃应小于总工艺质量平衡的10％wt，优选小于5％wt更优选小于2％wt。
产品HMFO(24)通过流体连通排放到本方法界区外的储罐中。
产品HMFO由所公开的说明性方法得到的产品HFMO具有作为重质船用燃料油(也称为残渣船用燃料油或重质船用燃料)销售和使用的适售品质，并具有产品HMFO作为符合ISO标准(即ISO 8217:2017)的残渣船用燃料油所要求的主要物理性质，其表现出以下主要性质：在50℃下的最大运动粘度(ISO 3104)为180mm2/s至700mm2/s；在15℃下的最大密度(ISO3675)为991.0kg/m3至1010.0kg/m3；CCAI为780至870；闪点(ISO 2719)不低于60.0℃；最大总沉积物-老化(ISO 10307-2)为0.10％wt；最大碳残留-微量法(ISO 10370)为18.00％wt至20.00％wt，并且最大铝和硅(ISO 10478)含量为60mg/kg。
产品HMFO的硫含量(ISO 14596或ISO 8754)小于0.5％wt，优选小于0.1％wt，更优选小于0.05％wt，并且完全符合IMO附则VI(修订版)对低硫、优选超低硫HMFO的要求。也就是说，与原料HMFO相比，产品HMFO的硫含量降低了约90％或更多。类似地，产品重质船用燃料油的钒含量(ISO 14597)小于原料重质船用燃料油的最大钒含量的10％，更优选地小于1％。本领域技术人员将理解，原料HMFO的硫和钒含量的显著降低表明已经实现了来自原料HMFO的环境污染物的显著减少的方法；同样重要的是，这是在保持符合ISO 8217:2017标准的HMFO的期望特性的同时实现的。
产品HMFO不仅符合ISO 8217:2017标准(并且可作为残渣船用燃料油或船用燃料销售)，而且产品HMFO的最大硫含量(ISO 14596或ISO 8754)在0.05％wt至1.0％wt之间，优选地硫含量(ISO 14596或ISO 8754)在0.05％wt至0.5％wt之间，并且更优选地硫含量(ISO14596或ISO 8754)在0.1％wt至0.05％wt之间。产品HMFO的钒含量完全在ISO 8217:2017残渣船用燃料油要求的最大钒含量(ISO 14597)范围内，表现为钒含量低于450mg/kg，优选地钒含量(ISO 14597)低于300mg/kg，并且更优选地钒含量(ISO 14597)在50mg/kg至100mg/kg的范围内。
海运燃料的船用燃料共混、仓储燃料制剂和燃料物流要求领域的技术人员将容易理解，无需进一步的组成变化或共混，产品HMFO可以作为低硫符合MARPOL附则VI标准的重质(残渣)船用燃料油销售和使用，其是目前使用的高硫重质(残渣)船用燃料油或重质船用燃料的直接替代品。一个说明性实施方案是符合ISO 8217:2017标准的低硫重质船用燃料油，其包含(和优选地基本上由以下组成)100％加氢处理的符合ISO 8217:2017标准的高硫重质船用燃料油，其中加氢处理的符合ISO 8217:2017标准的高硫重质船用燃料油的硫含量大于0.5％wt，并且其中符合ISO 8217:2017标准的低硫重质船用燃料油的硫含量小于0.5％wt。另一个说明性实施方案是符合ISO 8217:2017标准的超低硫重质船用燃料油，其包含(和优选地基本上由以下组成)100％加氢处理的符合ISO 8217:2017标准的高硫重质船用燃料油，其中加氢处理的符合ISO 8217:2017标准的高硫重质船用燃料油的硫含量大于0.5％wt，并且其中符合ISO 8217:2017标准的低硫重质船用燃料油的硫含量小于0.1％wt。
作为本发明的结果，可以实现对船舶加油和海运业的多种经济和物流益处。更具体地说，益处包括：对现有重型船用燃料仓储基础设施(储存和转移系统)的最小改变；需要船舶系统的最小变化以符合MARPOL附则VI(修订版)的排放要求；不需要为船员提供额外的培训或认证等可实现的益处。炼油厂也将实现多种经济和物流益处，包括：不需要改变或重新平衡炼油厂运营和产品流以满足对低硫或超低硫HMFO的新市场需求；炼油厂不需要额外的单元以及附加额外的氢或硫容量，因为示例的方法可以作为独立的单元进行；炼油厂的运营可以继续专注于从接收的原油中产生最大价值的那些产品(即生产石化产品、汽油和馏分油(柴油)；炼油厂可以继续使用现有的原油状态而无需改用更低硫或更轻的原油以满足HMFO产品的环保要求；仅举几例。
重质船用燃料组合物本发明构思的一个方面是燃料组合物，其包含以下，但优选基本上由以下组成：由所公开的方法得到的产品HMFO，并且可任选地包含稀释剂材料。如上所述，产品HMFO本身的主要性质符合ISO 8217:2017标准，并符合全球IMO附则VI关于最大硫含量的要求(ISO 14596或ISO 8754)。在需要超低硫含量的程度上，本发明的方法实现了这一点，并且船用燃料共混领域的技术人员将理解，低硫或超低硫产品HMFO可用作主要共混原料，以形成符合全球IMO附则VI标准的低硫重质船用燃料组合物。这种低硫重质船用燃料组合物将包含以下(并且优选基本上由以下组成)：a)产品HMFO和b)稀释剂材料。在一个实施方案中，重质船用燃料组合物的大部分体积是产品HMFO，余量材料是稀释剂材料。优选地，重质船用燃料组合物为至少75体积％、优选至少80体积％、更优选至少90体积％、进一步优选至少95体积％的产品HMFO，余量为稀释剂材料。
稀释剂材料可以是混合或组合或添加到产品HMFO中的基于烃或非烃的材料，或者悬浮在产品HMFO中的固体颗粒。稀释剂材料可有意或无意地改变产品HMFO的组成，但是不得使得所得混合物不符合对于残渣船用燃料的主要性质的ISO 8217:2017标准，或者硫含量不低于全球MARPOL标准的0.5％wt硫(ISO 14596或ISO 8754)。被认为是基于烃的材料的稀释剂材料的实例包括：原料HMFO(即高硫HMFO)；基于馏分油的燃料，例如道路柴油、瓦斯油、MGO或MDO；切削油(其目前用于配制残渣船用燃料油)；可再生油和燃料，例如生物柴油、甲醇、乙醇等；基于气液技术的合成烃和油，例如；Fischer-Tropsch衍生油，全合成油，例如基于聚乙烯、聚丙烯、二聚物、三聚物和聚丁烯等的那些；炼油厂渣油或其他烃油，例如常压渣油、减压渣油、流体床催化裂化器(FCC)淤浆油、FCC循环油、裂解瓦斯油、裂化轻瓦斯油(CLGO)、裂化重瓦斯油(CHGO)、轻循环油(LCO)、重循环油(HCO)、热裂化渣油、焦化器重馏分油、沥青、脱沥青重油、减粘裂化炉渣油、废油、沥青质油；使用过的或回收的机油；润滑油芳烃提取物和原油，例如重质原油、劣质原油和类似物质，它们原本可能被送到加氢裂化器或转移到共混池中以用于现有技术的高硫重质(残渣)船用燃料油。被认为是基于非烃的材料的稀释剂材料的实例包括：残留水(即从空气中的湿气吸收的水，或者(在某些情况下作为微乳液)混溶或溶解在本发明产品HMFO的烃中的水)，燃料添加剂，其可包括但不限于洗涤剂、粘度调节剂、倾点抑制剂、润滑性改性剂、除雾剂(de-hazer)(例如烷氧基化酚醛聚合物)、消泡剂(例如聚醚改性的聚硅氧烷)；点火改进剂；防锈剂(例如琥珀酸酯衍生物)；腐蚀抑制剂；抗磨损添加剂、抗氧化剂(例如酚类化合物和衍生物)、涂层剂和表面改性剂、金属钝化剂、静电消散剂、离子和非离子表面活性剂、稳定剂、化妆着色剂和添味剂和它们的组合。第三组稀释剂材料可包括由于产品HMFO或重质船用燃料组合物的处理、储存和运输而存在的悬浮固体或细颗粒材料，包括但不限于：碳或烃固体(例如，焦炭、石墨固体或微团聚沥青质)、铁锈和其他氧化腐蚀固体、细块金属颗粒、颜料或表面涂层颗粒、塑料或聚合物或弹性体或橡胶颗粒(例如由垫圈、阀门部件等降解产生)、催化剂细料、陶瓷或矿物颗粒、砂、粘土和其他土制颗粒、细菌和其他生物产生的固体，和这些的混合物，其可作为悬浮颗粒存在，但在别的方面却不会影响重质船用燃料组合物的作为符合ISO 8217:2017标准的重质(残渣)船用燃料的适售品质。
产品HMFO和稀释剂材料的共混物必须具有作为低硫重质(残渣)船用燃料的适售品质。也就是说，该混合物必须适合作为重质海洋船用燃料的预期用途，并且通常可代替作为远洋船舶的船用燃料。优选地，重质船用燃料组合物必须保持符合ISO 8217:2017标准的残渣船用燃料油所需的主要物理性质和低于全球MARPOL标准的0.5％wt硫(ISO 14596或ISO 8754)的硫含量，使材料符合MARPOL附则VI低硫重质船用燃料油(LS-HMFO)的要求。如上所述，产品HMFO的硫含量可显著低于0.5％wt(即低于0.1％wt硫(ISO 14596或ISO8754))以有资格作为MARPOL附则VI(修订版)超低硫重质船用燃料油(ULS-HMFO)，并且重质船用燃料成分同样可以配制成作为符合MARPOL附则VI标准的ULS-HMFO，以适合于用作ECA区域的海运燃料。为了获得ISO 8217:2017合格燃料的资格，本发明的重质船用燃料组合物必须满足国际公认的标准，包括：在50C下的最大运动粘度(ISO 3104)在180mm2/s至700mm2/s之间；在15℃下的最大密度(ISO 3675)在991.0kg/m3至1010.0kg/m3之间；CCAI在780至870的范围内；闪点(ISO 2719)不低于60.0℃；最大总沉积物-老化(ISO 10307-2)为0.10％wt；最大碳残留-微量法(ISO 10370)在18.00％wt至20.00％wt之间，并且最大铝和硅(ISO10478)含量为60mg/kg。
生产设备描述：现在转到生产设备的更详细的说明性实施方案，图2示出了实施上述用于减少原料HMFO中的环境污染物以生产根据第二说明性实施方案的产品HMFO的生产设备的示意图。其中使用多个反应器的生产设备的可选的实施方案在本发明的范围内，并且在共同未决的公开内容中描述。
在图2中，原料HMFO(A)从界区外(OSBL)进料到油进料缓冲罐(1)，后者从界区外(OSBL)接收进料并提供足够的缓冲体积以确保单元的平稳运行。从HMFO中除去进料中夹带的水，其中将水排出为流(1c)用于OSBL处理。
原料HMFO(A)通过供油泵(3)经管线(1b)离开油进料缓冲罐(1)，并加压至该工艺所需的压力。加压的HMFO(A’)然后通过管线(3a)进入油进料/产品热交换器(5)，在那里加压的HMFO进料(A’)被产品HMFO(B)部分加热。产品HMFO(B)是硫含量小于5000ppmw，优选小于1000ppmw的烃流。原料HMFO和产品HMFO中的烃为C12至C70+，并且沸程在350℉至1110+F之间。通过管线(5a)的加压的原料HMFO(A’)在反应器进料/流出物热交换器(7)中被来自反应器系统的流出物(E)进一步加热。
然后将管线(7a)中的经加热和加压的原料HMFO(A”)与通过管线(23c)提供的活化气体(C)在混合点(X)混合，以形成原料混合物(D)。混合点(X)可以是本领域技术人员公知的任何公知的气/液混合系统或夹带机构。
原料混合物(D)通过管线(9a)到达反应器进料炉(9)，在那里将原料混合物(D)加热到指定的工艺温度。反应器进料炉(9)可以是火焰加热炉或本领域技术人员已知的任何其他种类或类型的加热器，只要其将原料混合物的温度升高到工艺条件的期望温度即可。
完全加热的原料混合物(D’)通过管线9b离开反应器进料炉(9)并供给至反应器系统(11)中。完全加热的原料混合物(D’)进入反应器系统(11)，在那里从完全加热的原料混合物的原料HMFO组分中优先除去环境污染物，例如硫、氮和金属。反应器系统含有催化剂，该催化剂通过使原料HMFO组分中的硫化合物与活化气体中的氢气反应形成硫化氢而优先除去原料HMFO组分中的硫化合物。反应器系统还将实现脱金属、脱氮和一定量的复杂芳烃和沥青质的开环氢化，但是烃加氢裂化的发生应该最低化。将氢分压、反应压力、温度和通过时空速度测量的停留时间的工艺条件优化以实现所需的最终产物品质。关于反应器系统、催化剂、工艺条件和该工艺的其它方面的更详细讨论包含在下面的“反应器系统描述”中。
反应器系统流出物(E)通过管线(11a)离开反应器系统(11)并在反应器进料/流出物交换器(7)中与加压的原料HMFO(A’)进行交换热并部分地加热原料HMFO(A’)。然后，部分冷却的反应器系统流出物(E’)经管线(11c)流到热分离器(13)。
热分离器(13)将反应器系统流出物的气态组分(F)与反应器系统流出物的液体组分(G)分离，将反应器系统流出物的气态组分(F)引导到管线(13a)，将反应器系统流出物的液体组分(G)引导到管线(13b)。管线(13a)中的反应器系统流出物的气态组分在热分离器蒸汽空气冷却器(15)中相对于空气冷却，然后通过管线(15a)流到冷分离器(17)。
冷分离器(17)进一步使反应器系统流出物的冷却的气态组分(F’)中任何剩余的气态组分与液体组分分离。来自冷分离器的气态组分(F”)被引导至管线(17a)并供给至胺吸收塔(21)上。冷分离器(17)还使管线(17b)中的任何剩余的冷分离器烃液体(H)与任何冷分离器冷凝液态水(I)分离。冷分离器冷凝液态水(I)通过管线(17c)送入OSBL进行处理。
管线(13b)中的来自热分离器的反应器系统流出物的烃液体组分(G)与管线(17b)中的冷分离器烃液体(H)合并，并被供给至油产品汽提塔系统(19)。油产品汽提塔系统(19)从产品HMFO(B)中除去任何残留的氢和硫化氢，产品HMFO(B)在管线(19b)中排放以在OSBL储存。管线(19a)中的来自油产品汽提塔的排气流(M)可以被送到OSBL的燃气系统或火炬系统。有关油产品汽提塔系统的更详细讨论包含在“油产品汽提塔系统描述”中。
管线(17a)中来自冷分离器的气态组分(F”)含有氢气、硫化氢和轻质烃(主要是甲烷和乙烷)的混合物。该蒸汽流(17a)供给至胺吸收塔(21)，在那里其与由OSBL通过管线(21a)提供至胺吸收塔(21)的贫胺(J)接触，以从构成活化气体再循环流(C’)的气体中除去硫化氢。吸收了硫化氢的富胺(K)离开胺吸收塔(21)的底部，并通过管线(21b)送入OSBL，用于胺再生和硫回收。
管线(21c)中的胺吸收塔顶部蒸汽优选通过再循环压缩机(23)和管线(23a)作为再循环活化气体(C’)再循环到工艺中，在那里其与从OSBL通过管线(23b)提供的补充活化气体(C”)混合，循环活化气体(C’)与补充活化气体(C”)的这种混合物形成活化气体(C)，其如上所述通过管线(23c)在所述方法中被利用。洗涤的净化气流(H)从胺吸收塔顶部蒸气管线(21c)移除并通过管线(21d)送至OSBL以防止轻质烃或其他不可冷凝物的积聚。
反应器系统描述：图2中所示的反应器系统(11)包括装载有工艺催化剂的单个反应器容器以及本领域技术人员容易理解的足够的控制器、阀门和传感器。
其中不止一个反应器容器可以并联使用或级联串联使用的可选反应器系统可以很容易地替代图2所示的单反应器容器反应器系统(11)。在这样的实施方案中，多个反应器容器中的每一个并联并且类似地装载有工艺催化剂，并且可以通过共用管线提供加热的进料混合物(D’)。来自三个反应器中的每一个的流出物在共用管线中重新组合并形成合并的反应器流出物(E)，用于如上所述的进一步处理。说明性布置将允许三个反应器并联地执行该过程，从而有效地倍增了整个反应器系统的液压容量。控制阀和隔离阀可用于阻止进料进入一个反应器容器但不阻止进入另一个反应器容器。以这种方式，一个反应器可以被绕过并处于离线以便维护和重新加载催化剂，而剩余的反应器继续接收加热的原料混合物(D’)。本领域技术人员将理解，这种并联布置的反应器容器不限于三个，而是可以添加多个另外的反应器容器。对并联反应器容器数量的唯一限制是布局间距和向每个活性反应器提供加热的原料混合物(D’)的能力。
在另一个说明性实施方案中，级联反应器容器装载有对待去除的金属、硫或其他环境污染物具有相同或不同活性的工艺催化剂。例如，一个反应器可以装载高活性的脱金属催化剂，第二后续或下游反应器可以装载经平衡的脱金属/脱硫催化剂，和第二反应器下游的第三反应器可以装载高活性脱硫催化剂。这样可以在工艺条件(温度、压力、空间流速等)中实现更好的控制和平衡，因此可以为每种催化剂进行定制。以这种方式，可以根据供给至特定反应器的材料/催化剂组合来优化每个反应器中的参数，并使加氢裂化反应最小化。与前面的说明性实施方案一样，可以并联使用多个级联反应器系列，并且以这种方式利用上述这种布置的优点(即允许一个系列“在线”而另一个系列“离线”用于维护或允许增加的设备产能)。
形成反应器系统的反应器可以是固定床、沸腾床或淤浆床或这些类型反应器的组合。如所设想的，固定床反应器是优选的，因为它们更易于操作和维护。
反应器系统中的反应器容器装载有一种或多种工艺催化剂。工艺催化剂体系的确切设计取决于原料性质、产品要求和操作限制，并且本领域普通技术人员可以通过常规试验和误差来进行工艺催化剂的优化。
工艺催化剂包含选自由各自属于元素周期表第6、8、9和10族的金属组成的组的至少一种金属，更优选使用混合过渡金属催化剂，例如Ni—Mo、Co—Mo、Ni—W或Ni—Co—Mo。金属优选负载在多孔无机氧化物催化剂载体上。多孔无机氧化物催化剂载体是选自由氧化铝、氧化铝/氧化硼载体、含有含金属硅铝酸盐的载体、氧化铝/磷载体、氧化铝/碱土金属化合物载体、氧化铝/二氧化钛载体和氧化铝/氧化锆载体组成的组的至少一种载体。优选的多孔无机氧化物催化剂载体是氧化铝。载体上的孔径和金属负载量可以随所需的原料和工艺条件而系统地改变并进行测试，以优化产品HMFO的性质。这些活动对于本领域技术人员来说是公知的和常规的。固定床反应器中的催化剂可以是致密负载的或袜式负载的(sock-loaded)。
通过设计催化剂装载方案，可以使反应器系统内使用和装载的催化剂选择优先脱硫，使得原料混合物首先接触具有优先脱金属的催化剂的催化剂床，然后下游是具有用于脱金属和脱硫的混合活性的催化剂床，然后下游是具有高脱硫活性的催化剂床。实际上，具有高脱金属活性的第一床充当脱硫床的保护床。
反应器系统的目标是以满足产品HMFO规范所需的严格程度处理原料HMFO。当工艺条件优化时，脱金属、脱氮和烃加氢反应也可在一定程度上发生，因此反应器系统的性能达到所需的脱硫水平。优选使加氢裂化最小化以减少作为工艺副产品烃形成的烃的体积。该方法的目的是从原料HMFO中选择性地除去环境污染物并使不必要的副产品烃(C1-C8烃)的形成最小化。
每个反应器容器中的工艺条件取决于原料、所用催化剂和期望产品HMFO的期望的最终性能。本领域普通技术人员可以预期条件的变化，并且这些变化可以通过该方法的中试设备测试和系统优化来确定。考虑到这一点，发现操作压力、指示的操作温度、活化气体与原料HMFO的比率、活化气体中氢气的分压和空间速度都是需要考虑的重要参数。反应器系统的操作压力应在250psig至3000psig的范围内，优选在1000psig至2500psig之间，更优选在1500psig至2200psig之间。反应器系统的指示操作温度应为500℉至900℉，优选在650℉至850℉之间，更优选在680℉至800℉之间。活化气体的量与原料HMFO的量的比率应在250scf气体/bbl原料HMFO至10,000scf气体/bbl原料HMFO的范围内；优选在2000scf气体/bbl原料HMFO至5000scf气体/bbl原料HMFO之间，更优选在2500scf气体/bbl原料HMFO至4500scf气体/bbl原料HMFO之间。活化气体应选自氮气、氢气、二氧化碳、气态水和甲烷的混合物，因此活化气体具有大于活化气体混合物的总压力(P)的80％的理想的氢气分压(pH2)，并且优选地其中活化气体具有大于活化气体混合物的总压力(P)的95％的理想的氢气分压(pH2)。活化气体可具有为活化气体混合物的总摩尔数的80％之间的氢摩尔分数，并且更优选地，其中活化气体具有为活化气体混合物总摩尔数的80％至99％的氢摩尔分数。反应器系统内的液时空速应在0.05油/小时/m3催化剂至1.0油/小时/m3催化剂之间；优选在0.08油/小时/m3催化剂至0.5油/小时/m3催化剂之间；更优选0.1油/小时/m3催化剂至0.3油/小时/m3催化剂之间，以实现脱硫，其中产品硫含量低于0.1％wt。
反应器系统的液压容量率应在100bbl原料HMFO/天至100,000bbl原料HMFO/天之间，优选在1000bbl原料HMFO/天至60,000bbl原料HMFO/天之间，更优选在5,000bbl原料HMFO/天至45,000bbl原料HMFO/天之间，甚至更优选在10,000bbl原料HMFO/天至30,000bbl原料HMFO/天之间。可以在单个反应器容器反应器系统或多反应器容器反应器系统中实现期望的液压容量。
油产品汽提塔系统描述：油产品汽提塔系统(19)包括从产品HMFO中除去氢气、硫化氢和比柴油更轻的轻质烃所需的汽提塔和辅助设备和设施。这种系统是本领域技术人员公知的，本文提供了一般性的功能描述。来自热分离器(13)和冷分离器(7)的液体供给至油产品汽提塔(19)。可以通过再沸器、新蒸汽或其他汽提介质实现氢气和硫化氢以及比柴油轻的轻质烃的汽提。油产品汽提塔系统(19)可以设计有顶部系统，包括顶部冷凝器、回流罐和回流泵，或者其可以设计成没有顶部系统。可以优化油产品汽提塔的条件以控制产品HMFO的主要性质，更具体地粘度和密度。
胺吸收塔系统描述：胺吸收塔系统(21)包括从冷分离器蒸汽进料中除去酸性气体(即硫化氢)所需的气液接触塔和辅助设备和设施，使得得到的洗涤气体可以在循环并且用作活化气体。这种系统是本领域技术人员公知的，本文提供了一般性功能描述。来自冷分离器(17)的蒸汽供给至接触塔/系统(19)。从OSBL提供的贫胺(或其他合适的酸性气体汽提流体或系统)用于洗涤冷分离器蒸汽，从而有效地除去硫化氢。胺吸收塔系统(19)可设计有气体干燥系统以除去夹带在再循环活化气体(C’)中的任何水蒸气。
以下实施例将为本领域技术人员提供了用于进行本文公开的方法的更具体的说明性实施方案。
实施例1
概述：中试试验的目的是证明原料HMFO可以在特定条件下通过装载有市售催化剂的反应器进行处理，以从HMFO中除去环境污染物，特别是硫和其他污染物，从而生产符合MARPOL标准的HMFO产品，即生产低硫重质船用燃料油(LS-HMFO)或超低硫重质船用燃料油(USL-HMFO)。
中试单元设置：中试单元将设置两个串联排列的434cm3反应器，以处理原料HMFO。前置反应器装载有市售的加氢脱金属(HDM)催化剂和市售的加氢过渡(hydro-transition，HDT)催化剂的混合物。本领域技术人员将理解，可以使用HDM和HDS催化剂的混合物与惰性材料的组合来形成和优化HDT催化剂层，以实现期望的中间/过渡活性水平。第二反应器将装载市售的加氢过渡(HDT)和市售加氢脱硫(HDS)的共混物。可选地，第二反应器可以简单地装载商业加氢脱硫(HDS)催化剂。本领域技术人员将理解，原料HMFO的特定进料性质可影响反应器系统中HDM、HDT和HDS催化剂的比例。使用相同进料测试不同组合的系统过程将产生针对任何原料和反应条件的优化的催化剂组合。对于该实施例，第一反应器将装载2/3加氢脱金属催化剂和1/3加氢过渡催化剂。第二反应器将装载所有加氢脱硫催化剂。每个反应器中的催化剂将与玻璃珠(约50体积％)混合以改善液体分布并更好地控制反应器温度。对于该中试试验，应使用这些市售催化剂：HDM：Albemarle KFR 20系列或同等产品；HDT：Albemarle KFR 30系列或同等产品；HDS：Albemarle KFR 50或KFR 70或同等产品。一旦完成中试单元的设置，可以使用二甲基二硫醚(DMDS)以本领域技术人员熟知的方式通过使催化剂硫化来活化催化剂。
中试单元操作：在完成活化步骤后，中试单元准备好接收原料HMFO和活化气体进料。对于本实施例，活化气体可以是工业级或更好的氢气。将混合的原料HMFO和活化气体按照规定的速率和操作条件提供给中试设备：供油速率：108.5ml/h(空速＝0.25/h)；氢/油比：570Nm3/m3(3200scf/bbl)；反应器温度：372℃(702℉)；反应器出口压力：13.8MPa(g)(2000psig)。
本领域技术人员将知道，可以根据进料性质系统地调节和优化速率和条件，以达到期望的产品要求。对于每种条件，单元将处于稳定状态，并采集完整样品，以便完成分析测试。在进入下一个条件之前，应关闭每个条件的材料平衡。
对原料HMFO性质的预期影响是：硫含量(wt％)：减少至少80％；金属含量(wt％)：减少至少80％；MCR/沥青质含量(wt％)：减少至少30％；氮含量(wt％)：减少至少20％；C1-石脑油产率(wt％)：不大于3.0％，优选不大于1.0％。
可以根据表4系统地调整中试单元中的工艺条件，以评估工艺条件的影响并优化所用特定催化剂和原料HMFO的工艺性能。
以这种方式，可以优化中试单元的条件以实现小于0.5％wt硫的产品HMFO，优选0.1％wt硫的产品HMFO。制备ULS-HMFO(即0.1％wt硫的产品HMFO)的条件是：原料HMFO进料速率：65.1ml/h(空速＝0.15/h)；氢/油比：620Nm3/m3(3480scf/bbl)；反应器温度：385℃(725℉)；反应器出口压力：15MPa(g)(2200psig)。
表5总结了对HMFO关键性质的预期影响。
表6列出了进行用于表征原料HMFO和产品HMFO的分析测试。分析测试包括ISO对原料HMFO和产品HMFO要求的那些以获得作为符合ISO标准残渣船用燃料的资格并销售。提供了额外的参数使得本领域技术人员将能够理解和领会本发明方法的有效性。
表7包含本发明方法预期的原料HMFO分析测试结果和产品HMFO分析测试结果，其表明产生LS HMFO。本领域技术人员将注意到，在这些条件下，烃裂化的水平将最小化至基本上低于总质量平衡的10％，更优选地小于5％，甚至更优选地小于1％的水平。
通过系统改变工艺参数，例如通过较低的空速或通过使用具有较低初始硫含量的原料HMFO，通过本发明方法生产的产品HMFO将达到ULS HMFO限值(即0.1％wt硫的产品HMFO)。
实施例2：RMG-380HMFO
中试单元设置：如上述实施例1中所述设置中试单元，具有以下变化：第一反应器装载有：70体积％的Albemarle KFR 20系列加氢-脱金属催化剂作为与原料接触的第一(上)层，和30体积％的Albemarle KFR 30系列加氢过渡催化剂作为第二(下)层。第二反应器装载有：20％的Albemarle KFR 30系列加氢过渡催化剂作为第一(上)层，和80体积％的加氢脱硫催化剂作为第二(下)层。使用二甲基二硫醚(DMDS)以本领域技术人员熟知的方式通过使催化剂硫化来活化催化剂。
中试单元操作：在完成活化步骤后，中试单元准备好接收原料HMFO和活化气体进料。活化气体可以是工业级或更好的氢气。除了高硫含量(2.9wt％)之外，原料HMFO是市售且适售的符合ISO 8217:2017标准的HMFO。将混合的原料HMFO和活化气体以下表8中规定的速率和条件提供给中试设备。改变条件以优化产品HMFO材料中的硫含量。
以下提供了原料HMFO的代表性样品和产品HMFO的代表性样品的分析数据：
如上表7中所述，原料HMFO和产品HMFO均表现出与对于适售残渣船用燃料油的ISO8217:2017一致的主要性质，不同之处在于如上所述，与原料HMFO相比，产品HMFO的硫含量显著降低。
本领域技术人员将理解，通过本发明方法生产的上述产品HMFO不仅实现了符合ISO 8217:2017标准的LS HMFO(即0.5％wt硫)，而且还实现了符合ISO 8217:2017标准的ULS HMFO限制(即0.1％wt硫)的产品HMFO。
实施例3：RMK-500HMFO
将上述实施例2中使用的中试反应器的原料改变为市售且适售的符合ISO 8217:2017RMK-500标准的HMFO，不同之处在于其具有高环境污染物(即硫(3.3wt％))。RMK-500原料高硫HMFO的其他主要特征如下：
将混合的原料(RMK-500)HMFO和活化气体以下表中的速率和条件提供给中试设备，且所得到的硫水平如下表所示。
如上表所示，得到的产品(RMK-500)HMFO表现出与原料(RMK-500)HMFO一致的观察到的主要性质，不同之处在于硫含量显著降低。
本领域技术人员将理解，通过本发明方法生产的上述产品HMFO已经实现了LSHMFO(即0.5％wt硫)产品HMFO，其具有符合ISO 8217:2017标准的RMK-500残渣燃料油的主要特征。还应理解，该方法可在非加氢裂化条件(即较低的温度和压力)下成功进行，这显著降低了原料的加氢裂化。应当注意，当条件增加到更高的压力时(实施例E)，实现了具有更低硫含量的产品，但是观察到轻质烃和野生石脑油产量增加。
本领域技术人员将理解，在不脱离其广泛的发明构思的情况下，可以对上述说明性实施方案进行改变。因此，应理解，所公开的发明构思不限于所公开的说明性实施方案或实施例，而是旨在覆盖由权利要求限定的发明构思的范围内的修改。

Claims (16)

1.一种低硫重质船用燃料油，基本上由在加氢脱硫和加氢脱金属以及小于总质量平衡的10％wt的加氢裂化的条件下加氢处理的高硫重质船用燃料油组成，其中在加氢处理之前，所述高硫重质船用燃料油在其他方面符合ISO 8217:2017标准作为表2残渣船用燃料油但是具有大于0.5％wt的硫含量(ISO 14596或ISO 8754)，并且其中所述低硫重质船用燃料油符合ISO 8217:2017标准作为表2残渣船用燃料油，具有作为残渣船用燃料油的适售品质且具有小于0.5％wt的硫含量(ISO 14596或ISO 8754)。
2.根据权利要求1所述的组合物，其中所述高硫重质船用燃料油的硫含量(ISO 14596或ISO 8754)在1.0％wt至5.0％wt的范围内，并且所述低硫重质船用燃料油的硫含量(ISO14596或ISO 8754)在0.5％wt至0.05％wt的范围内。
3.根据权利要求1所述的组合物，其中所述低硫重质船用燃料油的硫含量(ISO 14596或ISO 8754)小于0.1％wt。
4.根据权利要求1所述的组合物，其中低硫重质船用燃料油具有180mm2/s至700mm2/s的范围内的50C下的最大运动粘度(ISO 3104)；991.0kg/m3至1010.0kg/m3的范围内的15℃下的最大密度(ISO 3675)；780至870的范围内的CCAI；不低于60.0℃的闪点(ISO 2719)；0.10％wt的最大总沉积物-老化(ISO 10307-2)；18.00％wt至20.00％wt的范围内的最大碳残留-微量法(ISO 10370)，和60mg/kg的最大铝和硅(ISO 10478)含量。
5.一种低硫烃燃料组合物，基本上由大部分体积的在加氢脱硫和加氢脱金属以及小于总质量平衡的10％wt的加氢裂化的条件下加氢处理的高硫残渣船用燃料油和小部分体积的稀释剂材料组成，其中在加氢处理之前，所述高硫重质船用燃料油在其他方面符合ISO8217:2017标准作为表2残渣船用燃料油但是具有大于0.5％wt的硫含量(ISO 14596或ISO8754)；并且其中所述低硫重质船用燃料油符合ISO 8217:2017标准作为表2残渣船用燃料油并且具有小于0.5％wt的硫含量(ISO 14596或ISO 8754)；并且其中所述稀释剂材料选自由烃材料；非烃材料；和固体材料和它们的组合组成的组，并且其中所述低硫烃燃料组合物符合ISO 8217:2017表2。
6.根据权利要求5所述的组合物，其中所述100％加氢处理的高硫残渣船用燃料油占所述组合物的至少75体积％，并且所述稀释剂材料占所述组合物的不大于25体积％。
7.根据权利要求5所述的组合物，其中所述100％加氢处理的高硫残渣船用燃料油占所述组合物的至少90体积％，并且所述稀释剂材料占所述组合物的不大于10体积％。
8.根据权利要求5所述的组合物，其中所述烃材料选自由以下组成的组：硫含量(ISO14596或ISO 8754)大于0.5wt的重质船用燃料油；基于馏分油的燃料；柴油；瓦斯油；船用瓦斯油；船用柴油；切削油；生物柴油；甲醇、乙醇；基于气液技术的合成烃和油；Fischer-Tropsch衍生油；基于聚乙烯、聚丙烯、二聚物、三聚物和聚丁烯的合成油；常压渣油；减压渣油；流体床催化裂化器(FCC)淤浆油；FCC循环油；裂解瓦斯油；裂化轻瓦斯油(CLGO)；裂化重瓦斯油(CHGO)；轻循环油(LCO)；重循环油(HCO)；热裂化渣油；焦化器重馏分油；沥青；脱沥青重油；减粘裂化炉渣油；废油；沥青质油；使用过的或回收的机油；润滑油芳香提取物；原油；重质原油；劣质原油；和它们的组合；并且其中所述非烃材料选自由以下组成的组：残留水；洗涤剂；粘度调节剂；倾点抑制剂；润滑性调节剂；除雾剂；消泡剂；点火改进剂；防锈剂；腐蚀抑制剂；抗磨损添加剂、抗氧化剂(例如酚类化合物和衍生物)、涂层剂和表面改性剂、金属钝化剂、静电消散剂、离子和非离子表面活性剂、稳定剂、化妆着色剂和添味剂和它们的组合；并且，其中所述固体材料选自由以下组成的组：碳或烃固体；焦炭；石墨固体；微团聚沥青质，铁锈；氧化腐蚀固体；块状金属颗粒；油漆颗粒；表面涂层颗粒；塑料颗粒或聚合物颗粒或弹性体颗粒橡胶颗粒；催化剂细料；陶瓷颗粒；矿物颗粒；砂；粘土；土制颗粒；细菌；生物产生的固体；和它们的组合。
9.根据权利要求4所述的组合物，其中低硫重质船用燃料油具有180mm2/s至700mm2/s的范围内的50C下的最大运动粘度(ISO 3104)；991.0kg/m3至1010.0kg/m3的范围内的15℃下的最大密度(ISO 3675)；780至870的范围内的CCAI；不低于60.0℃的闪点(ISO 2719)；0.10％wt的最大总沉积物-老化(ISO 10307-2)；18.00％wt至20.00％wt的范围内的最大碳残留-微量法(ISO 10370)，和60mg/kg的最大铝和硅(ISO 10478)含量。
10.一种低硫船用燃料油，基本上由包括以下步骤的方法的产物组成：
将预定量的硫含量大于0.5％wt但在其他方面符合ISO 8217:2017标准作为表2残渣船用燃料油的重质船用燃料油与预定量的活化气体混合，形成原料混合物；
使所述原料混合物在至少一个反应器容器中与一种或多种催化剂体系接触，所述一种或多种催化剂体系选自由固定床负载的过渡金属多相催化剂；沸腾床负载的过渡金属多相催化剂；惰性催化剂材料；以及它们的组合组成的组，其中所述接触在加氢脱硫和加氢脱金属，并且加氢裂化至小于总质量平衡的10％wt的反应性工艺条件下进行，以形成工艺混合物；
将所述工艺混合物从与所述至少一个反应器容器中的所述一种或多种催化剂体系的接触中移除；
通过流体连通将所述工艺混合物从所述至少一个反应器容器转移到至少一个液气分离容器中；
在所述至少一个液气分离容器中将所述工艺混合物分离成所述工艺混合物的液体组分和所述工艺混合物的气体组分；
通过流体连通将所述工艺混合物的所述液体组分从所述至少一个液气分离容器转移到至少一个烃分馏容器；和
从所述工艺混合物的所述液体组分中分离低硫船用燃料油组分；
将所述低硫船用燃料油组分作为所述低硫船用燃料油从所述至少一个烃分馏容器中排出，其中所述低硫船用燃料油符合ISO 8217:2017标准作为表2残渣船用燃料油，而无需额外处理。
11.根据权利要求10所述的低硫船用燃料油，其中所述高硫重质船用燃料油的硫含量(ISO 14596或ISO 8754)在1.0％wt至5.0％wt的范围内，并且所述低硫重质船用燃料油的硫含量(ISO 14596或ISO 8754)在0.5％wt至0.05％wt的范围内。
12.根据权利要求10所述的低硫船用燃料油，其中所述低硫重质船用燃料油的硫含量(ISO 14596或ISO 8754)小于0.1％wt。
13.根据权利要求10所述的低硫船用燃料油，其中低硫重质船用燃料油具有180mm2/s至700mm2/s的范围内的50C下的最大运动粘度(ISO 3104)；991.0kg/m3至1010.0kg/m3的范围内的15℃下的最大密度(ISO 3675)；780至870的范围内的CCAI；不低于60.0℃的闪点(ISO2719)；0.10％wt的最大总沉积物-老化(ISO 10307-2)；18.00％wt至20.00％wt的范围内的最大碳残留-微量法(ISO 10370)，和60mg/kg的最大铝和硅(ISO 10478)含量。
14.根据权利要求10中所述的方法的产物，其中所述方法还包括步骤i)将至少75体积％的符合ISO 8217:2017标准作为表2残渣船用燃料油的所述低硫船用燃料油与不超过25体积％的稀释剂材料共混，从而形成符合ISO 8217:2017作为表2残渣船用燃料油的低硫船用燃料组合物。
15.根据权利要求14中所述的方法的产物，其中所述稀释剂材料选自由烃材料；非烃材料；和固体材料及它们的组合组成的组，并且进一步地其中所述烃材料选自由以下组成的组：硫含量(ISO 14596或ISO 8754)大于0.5wt的重质船用燃料油；基于馏分油的燃料；柴油；瓦斯油；船用瓦斯油；船用柴油；切削油；生物柴油；甲醇、乙醇；基于气液技术的合成烃和油；Fischer-Tropsch衍生油；基于聚乙烯、聚丙烯、二聚物、三聚物和聚丁烯的合成油；常压渣油；减压渣油；流体床催化裂化器(FCC)淤浆油；FCC循环油；裂解瓦斯油；裂化轻瓦斯油(CLGO)；裂化重瓦斯油(CHGO)；轻循环油(LCO)；重循环油(HCO)；热裂化渣油；焦化器重馏分油；沥青；脱沥青重油；减粘裂化炉渣油；废油；沥青质油；使用过的或回收的机油；润滑油芳香提取物；原油；重质原油；劣质原油；和它们的组合。
16.根据权利要求14中所述的方法的产物，其中低硫船用燃料油具有180mm2/s至700mm2/s的范围内的50C下的最大运动粘度(ISO 3104)；991.0kg/m3至1010.0kg/m3的范围内的15℃下的最大密度(ISO 3675)；780至870的范围内的CCAI；不低于60.0℃的闪点(ISO2719)；0.10％wt的最大总沉积物-老化(ISO 10307-2)；18.00％wt至20.00％wt的范围内的最大碳残留-微量法(ISO 10370)，和60mg/kg的最大铝和硅(ISO 10478)含量。
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