CN103827261A - 生产沥青和脱硫油的一体化方法 - Google Patents
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Abstract
提供了一种一体化方法以生产沥青和脱硫油。将重质石油馏分中所含的硫分子,包括有机硫分子(在某些实施方案中为有机氮分子)氧化。极性的经氧化硫化合物由油相转移至沥青相中。
Description
相关申请
本申请要求于2011年7月31日提交的美国临时专利申请第61/513,621号的权益,其公开内容通过引用全部并入本文。
发明背景
发明领域
本发明涉及用于生产沥青以及脱硫和脱沥青油的方法和***。
相关技术描述
原油包含影响原油馏分的精炼加工的量的杂原子如硫、氮、镍、钒等。轻质原油或冷凝物包含低达0.01重量%(W%)的硫,相反,重质原油包含高达5-6W%的硫。类似地,原油的氮含量为0.001-1.0W%。各种沙特***原油的杂原子含量在表1中给出。可以看出,在重度提高时,同一族内的原油的杂原子含量随API比重的降低而增大。原油馏分的杂原子含量还随着沸点的提高而增大(表2)。
表1
性能 | ASL | AEL | AL | AM | AH |
比重,° | 51.4 | 39.5 | 33.0 | 31.1 | 27.6 |
硫,W% | 0.05 | 1.07 | 1.83 | 2.42 | 2.94 |
氮,ppmw | 70 | 446 | 1064 | 1417 | 1651 |
RCR,W% | 0.51 | 1.72 | 3.87 | 5.27 | 7.62 |
Ni+V,ppmw | <0.1 | 2.9 | 21 | 34.0 | 67 |
ASL—***超轻油
AEL—***特级轻油
AL—***轻油
AM—***中质油
AH—***重油
表2
馏分,℃ | 硫,W% | 氮,ppmw |
C5-90 | 0.01 | |
93-160 | 0.03 | |
160-204 | 0.06 | |
204-260 | 0.34 | |
260-315 | 1.11 | |
315-370 | 2.00 | 253 |
370-430 | 2.06 | 412 |
430-482 | 2.65 | 848 |
482-570 | 3.09 | 1337 |
原油馏分中的污染物(有毒化合物)如硫、氮、多核芳族化合物影响下游工艺,包括加氢处理、加氢裂化和流化催化裂化(FCC)。所述污染物以不同的结构和浓度存在于原油馏分中。在精炼期间必须除去这些杂质以满足对于最终产品(如汽油、柴油、燃料油)或对于需要加工以进一步升级如重整异构化的中间精炼料流的环境规定。
在常规精炼方案中,首先将原油在常压塔蒸馏以分离酸气和轻质烃,包括甲烷、乙烷、丙烷、丁烷和硫化氢、石脑油(36-180℃)、煤油(180-240℃)、瓦斯油(240-370℃);以及常压塔底渣油包括沸点高于370℃的烃。
来自常压蒸馏塔的常压渣油用作燃料油或者送至真空蒸馏单元,这取决于炼油厂的设置。在其中将渣油进一步在真空蒸馏塔中蒸馏的设置中,获得的产物包括具有沸点为370-520℃的烃的真空瓦斯油和具有沸点高于520℃的烃的真空渣油。
随着石油馏分的沸点升高,油的品质下降,且对下游加工单元产生不利影响。表3和表4提供了源自不同原油来源的常压渣油(沸点高于370℃)和真空渣油(沸点高于520℃)的品质。这些表中清楚显示出常压渣油或真空渣油被杂原子高度污染和具有高碳含量,且品质随着沸点升高而变劣。
表3
来源 | 名称 | API比重,° | 硫,W% | Ni+V,ppmw | CCR,W% |
中东 | ***轻油 | 16.80 | 3.14 | 550.00 | 7.60 |
中东 | ***重油 | 12.70 | 4.30 | 125.00 | 13.20 |
南亚 | Mina | 26.40 | 0.15 | 16.00 | 4.20 |
南亚 | Duri | 17.50 | 0.22 | 17.00 | 9.30 |
中国 | Shengli | 18.70 | 1.23 | 19.00 | 8.60 |
中国 | Taching | 25.10 | 0.13 | 4.00 | 4.00 |
拉丁美洲 | Maya | 8.30 | 4.82 | 494.00 | 17.40 |
拉丁美洲 | Isthmus | 13.90 | 2.96 | 53.00 | 8.20 |
表4
来源 | 名称 | API比重,° | 硫,W% | Ni+V,ppmw | CCR,W% |
中东 | ***轻油 | 6.90 | 4.34 | 141.00 | 20.30 |
中东 | ***重油 | 3.00 | 6.00 | 269.00 | 27.70 |
南亚 | Mina | 17.30 | 0.19 | 44.00 | 10.40 |
南亚 | Duri | 13.00 | 0.25 | 32.00 | 15.20 |
中国 | Shengli | 11.70 | 1.66 | 28.00 | 16.40 |
中国 | Taching | 18.70 | 0.18 | 9.00 | 9.50 |
拉丁美洲 | Maya | -0.10 | 5.98 | 835.00 | 29.60 |
拉丁美洲 | Isthmus | 4.00 | 4.09 | 143.00 | 21.10 |
对来自原油或其它天然来源如页岩油、沥青和沥青砂的石脑油、煤油和瓦斯油料流进行处理以脱除其量超过规定值的主要为硫的污染物。加氢处理是最常用的脱除这些污染物(对其它工艺/催化剂具有毒性的化合物)的精炼技术。将真空瓦斯油在氢化裂化单元中加工以生产汽油和柴油,或者在FCC单元中加工以主要生产汽油和生产作为副产物的LCO和HCO。前者用作柴油池或燃料油中的混合组分,而后者被直接送至燃料油池中。对于真空渣油馏分而言,存在若干加工选择,包括加氢处理、焦化、减粘裂化、气化和溶剂脱沥青。
在其它设置中,可在沥青单元中对真空渣油进行处理从而通过空气氧化生产沥青。沥青氧化是使空气在氧化塔容器中鼓泡通过进料或沥青以氧化含硫化合物的过程。其是将硫分子从油相中转移至沥青相中的非催化过程。
如上所述,在一些精炼设置中,可在溶剂脱沥青单元中对真空渣油进行处理以分离溶剂可溶性馏分(脱沥青油)和不溶性油(沥青质)馏分。
溶剂脱沥青是一种沥青分离工艺,其中借助极性而非借助沸点(像真空蒸馏工艺中的那样)分离渣油。溶剂脱沥青工艺制得了富含链烷属分子的低污染物脱沥青油(DAO)。然后可将这些馏分在常规转化单元如FCC单元或氢化裂化单元中进一步加工。溶剂脱沥青工艺通常采用链烷属C3-C7溶剂在临界条件或低于临界条件下进行。
与溶剂脱沥青有关的其它材料可见于美国专利4,816,140、4,810,367、4,747,936、4,572,781、4,502,944、4,411,790、4,239,616、4,305,814、4,290,880、4,482,453和4,663,028,其全部通过引用并入本文。
尽管单独和独立的沥青氧化和溶剂脱沥青工艺已充分开发且适于其预期目的,然而本领域仍需要更经济和有效的方法以由重质馏分如常压渣油获得产品。
发明简述
上述目的和其它优点由用于生产脱沥青和脱硫的油和沥青的***和方法提供。提供了一种一体化方法以用于生产沥青和脱硫油。使重质石油馏分中所含的硫分子(包括有机硫分子)和在某些实施方案中重质石油馏分中的有机氮分子氧化。极性的经氧化硫化合物由油相转移至沥青相中。有利地,本发明的方法和***可一体化至现有的溶剂脱沥青单元中,从而以相对较低的成本脱除杂质。
尽管单独和独立的沥青氧化和溶剂脱沥青方法已被充分开发,然而先前并未提出将所述两种方法一体化以通过氧化使常压渣油进料脱硫并通过溶剂脱沥青法提纯所述经氧化的进料来生产脱硫油和沥青产品。
附图简述
下文将参照附图进一步详细描述本发明,在所述附图中:
图1为一体化的沥青氧化和溶剂脱沥青的工艺流程图。
发明详述
提供了一种一体化方法以生产沥青和脱硫油。在本文所述的方法中,将存在于重质石油馏分(例如常压渣油)中的硫分子(在某些实施方案中为氮分子)氧化。通常不溶于该方法所用的溶剂中的经氧化极性硫化合物,在某些实施方案中的经氧化的氮化合物由可溶性油相转移至不溶性沥青相中。有利地,本发明的方法和***可一体化至现有的炼油厂溶剂脱沥青单元中,从而以相对较低的成本脱除杂质。
将常压渣油馏分(例如沸点为370℃或更高)通入沥青单元中以在存在或不存在催化剂下空气氧化。将沥青单元的产品引入溶剂脱沥青单元中以将包含降低含量的有机化合物,在某些实施方案中还包含降低含量的有机氮化合物的油馏分与沥青产物分离,这是因为与沥青相相比,油相相对较轻。
所述方法包括如下步骤:
提供沸点为36-1500℃,在某些实施方案中高于约370℃,在其它实施方案中高于约520℃的烃进料,所述烃进料包含杂质,所述杂质包括硫、氮化合物、镍、钒、铁、钼,典型地来源于原油源;
任选将均相催化剂添加至所述进料。将活性物质为Mo(VI)、W(VI)、V(V)、Ti(IV),具有高路易斯酸性和弱氧化电位的均相过渡金属催化剂用作催化剂;
在沥青氧化单元入口处将气态氧化剂与进料混合。气态氧化剂为空气或氧气或一氧化二氮或臭氧。氧与油之比为1-50V:V%,在某些实施方案中为3-20V:V%,或者对除氧气之外的气态氧化剂而言为等量的。沥青单元在100-300℃,在某些实施方案中为150-200℃的入口温度和150-400℃,在某些实施方案中为250-300℃的氧化区温度下,且在环境压力至60巴,在某些实施方案中为环境压力至30巴的压力下操作;
将沥青反应器的出料在容器中与C3-C7链烷属溶剂,在某些实施方案中为C4正丁烷和异丁烷的混合物,在低于溶剂的临界压力和温度的压力和温度下混合,由此破坏沥青质在石油脂(maltene)溶液中的平衡并使固体沥青质颗粒絮凝。链烷属溶剂的临界温度和压力在表5中给出,其它溶剂性能在表6中给出;
任选将吸附剂用于溶剂脱沥青工段中以进一步选择性分离氮、硫和多芳族化合物,例如如美国专利7,566,634所述(通过引用将其并入本文);
在第一分离容器中将固体相沥青质与液相分离,并将底部产物转移至沥青池中,将上层液体层转移至第二分离容器;和
在第二分离容器中分离脱沥青油并回收所述链烷属溶剂以将其再循环至混合容器。
表5
碳数 | 临界温度,℃ | 临界压力,巴 |
C3 | 97 | 42.5 |
C4 | 152 | 38.0 |
C5 | 197 | 34.0 |
C6 | 235 | 30.0 |
C7 | 267 | 27.5 |
表6
参照图1,其提供了用于生产沥青和脱硫油的一体化装置8的工艺流程图。一体化装置8包括氧化单元10(如氧化塔容器)和溶剂脱沥青单元18,所述溶剂脱沥青单元18包括第一分离容器20、第二分离容器30、脱沥青/脱硫油分离器40、溶剂流汽提容器50、沥青分离容器60、沥青汽提容器70和再循环溶剂容器80。
氧化单元10可为将渣油进料12中的有机硫化合物,在某些实施方案中的有机氮化合物有效转化成不溶于脱沥青单元溶剂中的其氧化物的任何合适的氧化装置。在某些实施方案中,氧化单元10可为氧化塔容器,其包括用于接受渣油进料12(一个或多个换热器的下游,未示出)和任选的催化剂14的入口15、用于接受保护蒸气的入口16、气态氧化剂入口18和经氧化的渣油出口22。
第一分离容器20(例如主沉降槽)包括与氧化塔容器10的出口22流体连通的入口24、用于排出沥青相的出口28和用于排出脱沥青/脱硫油相的出口32。还将补充溶剂流26、再循环的溶剂流62和第二分离容器底部料流78经由任选的混合容器90装入第一分离容器20。
第二分离容器30(例如次沉降槽)包括与第一沉降容器20的脱沥青/脱硫油32流体连通的入口34、用于排出脱沥青/脱硫油相的出口36和用于排出沥青相的出口38。
脱沥青/脱硫油分离器40典型地为用于回收溶剂的闪蒸器,其包括与第二分离容器30的顶部出口36流体连通的入口42、用于排出脱沥青/脱硫油分离器底部产物的出口46和用于排出再循环溶剂的出口44。
溶剂蒸气气提容器50包括与脱沥青/脱硫油分离器40的出口46流体连通的入口48、用于排出蒸气和过量溶剂的出口52和用于排出适于进一步精炼处理的脱沥青/脱硫油产物流的出口54。
沥青分离容器60包括与第一分离容器20的沥青相出口28流体连通的入口64、用于排出沥青分离容器底部产物的出口68和用于将再循环溶剂排至再循环溶剂容器80中的出口66。
沥青汽提容器70包括与沥青分离容器60的底部出口68流体连通的入口72、用于排出溶剂的出口76和用于排出沥青产物的出口74。
再循环溶剂容器80包括与脱沥青油分离器40的顶部出口44流体连通的入口56和与沥青分离容器60的出口66流体连通的导管84。再循环溶剂容器80的出口58与导管62流体连通,从而与进料混合。
在通过一个或多个换热器(未示出)之后,将渣油进料引入氧化塔容器10的入口12。在某些实施方案中,可经由导管14引入均相催化剂。保护蒸气经由入口16连续注入氧化塔容器10中。将压缩(压缩器未示出)后的气态氧化剂料流18通入分离鼓(未示出)中,并导至分布器中,例如位于所述氧化塔底部的上方。将渣油进料氧化并经由出口22排出。
所述气态氧化剂为空气或氧气或一氧化二氮或臭氧。氧气与油之比为1-50V:V%,优选为3-20V:V%,或者对其它气态氧化剂而言为等量的。所述氧化单元在150-200℃的入口温度、250-300℃氧化区温度和环境压力至30巴的压力下操作。
沥青氧化用于通过将氧原子加成至重烃分子而提高沥青质组分的分子尺寸。这导致比真空塔底沥青进料(针入度为230-250mm)更稠且更致密的沥青产物(针入度为60-70mm)。在本发明的方法中,使用进料如常压渣油来选择性氧化含硫和含氮的有机化合物,从而将其转移至沥青相中。因此,所述一体化沥青氧化和溶剂脱沥青单元的主要目的是生产脱硫油,并生产作为副产物的沥青。
将来自氧化塔容器10的出口22的经氧化渣油进料与补充溶剂26和再循环溶剂62混合,例如借助一个或多个在线混合器(未示出)或任选的混合容器90。
将沥青氧化反应器的出料与C3-C7链烷溶剂,在某些实施方案中与C4正丁烷和异丁烷的混合物在低于该溶剂的临界压力和温度的温度和压力下混合,由此破坏沥青质在石油脂溶液中的平衡并使固体沥青质颗粒絮凝。所述链烷属溶剂的临界温度和压力在表5中给出,其它溶剂性能在表6中给出。混合可在一个或多个混合容器中进行和/或借助一个或多个在线混合器进行。
任选地,在溶剂脱沥青工段中使用吸附剂以进一步选择性分离氮、硫和多芳族化合物,例如如美国专利7,566,634所述(通过引用将其并入本文)。
将所述混合物通入第一分离容器20(例如溶剂脱沥青单元的主沉降槽)的入口24中,在该容器中相分离成经由出口32排出的脱沥青/脱硫油相和经由出口28排出的沥青相。所述渣油进料的氧化部分具有极性,这导致由于其在所述溶剂中的不溶特性而转移至沥青相中。主沉降槽的压力和温度为所述溶剂的临界性质或更低。主沉降器的温度低,从而从经氧化的渣油出料中回收大部分脱沥青/脱硫油。由主沉降槽收集(例如经由收集管)的溶剂可溶性脱沥青/脱硫油相包含大部分的溶剂和脱沥青/脱硫油以及较小部分的沥青。所回收(例如经由一个或多个沥青收集管)的溶剂不溶性沥青相包含大部分的沥青、较小部分的溶剂、油相和经氧化的有机硫化合物(在某些实施方案中为经氧化的有机氮化合物)。
将脱沥青/脱硫油通入第二分离容器30(例如溶剂脱沥青单元的次沉降槽)的入口34中,分离成经由出口36(例如立式收集管)排出的脱沥青/脱硫油相和经由出口38(例如一个或多个沥青收集管)排出的沥青相。包含经氧化的有机硫化合物(在某些实施方案中为经氧化的有机氮化合物)的剩余沥青混合物在次沉降容器30中由于相对于主沉降槽的操作温度为提高的温度而作为沥青相脱除。所述次沉降槽典型地在或接近所述溶剂的临界温度的温度下操作,且能在底部形成包含较少量溶剂的沥青相和再循环回到主沉降容器20中的脱沥青油。经由出口38排出的脱沥青/脱硫油相包含大部分溶剂和脱沥青/脱硫油,并将其经由导管78再循环至主沉降容器20中以回收脱硫油。
将来自第二分离容器出口36的脱沥青/脱硫油相通入分离器40的入口42中,分离成脱沥青/脱硫油产物料流46和溶剂再循环料流44。将经由出口44的再循环溶剂通入再循环溶剂容器80中并返回至主沉降容器20中(例如经由混合容器90)。所述脱沥青/脱硫油分离器40的设置和尺寸允许进行快速和有效的闪蒸。
将包含大部分脱沥青/脱硫油以及小部分溶剂和蒸气的脱沥青/脱硫油产物料流46输送至容器50的入口48中以蒸气汽提所述溶剂,例如采用150psig的干蒸气。所述脱沥青/脱硫油经由出口54回收,蒸气与过量溶剂的混合物经由出口52排出。
将经由出口28排出的主沉降槽沥青相通入沥青分离容器60的入口64中,以闪蒸分离成经由出口68排出的沥青相和经由出口66排出的再循环溶剂。将包含大部分沥青和小部分溶剂的沥青相68输送至沥青汽提容器70的入口72中以蒸气汽提所述溶剂,例如采用150psig的干蒸气。溶剂经由出口76回收(可将其再循环,未示出),而包含经氧化的有机硫化合物(在某些实施方案中为经氧化的有机氮化合物)的沥青产物经由出口74回收,其可被送至沥青池中。
将来自沥青分离容器60的出口66的再循环溶剂经由导管84与来自第二分离容器40的再循环溶剂44一起通入再循环溶剂容器80中。根据需要,将再循环的溶剂经由管58输送以与来自出口22的经氧化渣油进料混合,例如在混合容器90中和/或在一个或多个在线混合器中。根据需要,可引入一个或多个中间溶剂鼓。
在主沉降槽20中,脱沥青油相包含大部分溶剂和脱沥青的油,与少量从主沉降槽顶部(出口32)排出的沥青。包含40-50液体体积%溶剂的沥青相离开该容器的底部(出口28)。在次沉降槽30中,来自主沉降槽20的包含一些沥青的脱沥青油相进入该容器中。从次沉降槽脱除的沥青包含较少量的溶剂和脱沥青油。在脱沥青油分离器40中,引入所述沉降槽中的溶剂的大于90W%进入脱沥青油分离器,其中回收超过95重量%的溶剂。来自脱沥青油分离器且包含痕量溶剂的脱沥青油进入脱沥青油汽提器50中。基本上所有溶剂均通过蒸气汽提从脱沥青油中移除。沥青分离器60允许对沥青和溶剂进行闪蒸分离。所述沥青相包含40-50体积%的溶剂。来自所述沥青分离器的沥青进入沥青汽提器70中,在其中通过蒸气汽提从沥青中移除残余溶剂。将约95%在高压***中回收的循环溶剂与在低压***中回收的循环溶剂的余量合并在一起并进入高压溶剂鼓80中。
进料通常为沸点高于370℃的常压渣油。在某些实施方案中,所述进料可为全部原油,其在初始进料12的上游具有一个或多个分离步骤。进料可来源于一种或多种天然源,如原油、沥青、重油、页岩油和/或来自于一个或多个精炼工艺单元(包括加氢处理、氢化加工、流体床催化裂化、焦化、减粘裂化或煤液化)的底部产物。
在一个或多个实施方案中,可任选与所述混合物一起在入口24处引入第二进料。在一个或多个实施方案中,可将某些中间馏分油或沥青料流再循环至氧化单元10中。
有利地,通过一体化沥青氧化和溶剂脱沥青工艺,采用现有单元对常压渣油进料脱硫,从而以比常规高压脱硫工艺更低的成本获得脱硫油和沥青。例如,可对常压渣油进行脱硫,从而在某些实施方案中回收40W%的脱硫油,剩余部分进入沥青相中,这也是有价值的产品。
上文和附图已对本发明的方法和***进行了描述;然而,其改进对本领域技术人员而言是显而易见的,本发明的保护范围由下文权利要求来限定。
Claims (10)
1.一种用于分离进料中的油和沥青的一体化方法,其包括:
将所述进料与有效量的氧化剂一起装入氧化单元中以产生包含经氧化的有机硫化合物的中间装料;和
将所述中间装料与有效量的溶剂一起通入溶剂脱沥青单元中以产生脱沥青/脱硫的油相和包含经氧化的有机硫化合物的沥青相。
2.根据权利要求1的方法,其中所述氧化单元为沥青氧化器。
3.根据权利要求1的方法,其中所述中间装料包含经氧化的有机硫化合物和经氧化的有机氮化合物。
4.根据权利要求3的方法,其中所述经氧化的有机硫化合物和经氧化的有机氮化合物不溶于溶剂脱沥青单元中所用的溶剂中,由此转移至所述沥青相中。
5.根据权利要求1的方法,其中所述氧化单元在100-300℃的入口温度下操作。
6.根据权利要求1的方法,其中所述氧化单元在150-200℃的入口温度下操作。
7.根据权利要求1的方法,其中所述氧化单元在150-400℃的温度下操作。
8.根据权利要求1的方法,其中所述氧化单元在250-300℃的温度下操作。
9.根据权利要求1的方法,其中所述氧化单元在环境压力至60巴的压力下操作。
10.根据权利要求1的方法,其中所述氧化单元在环境压力至30巴的压力下操作。
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Also Published As
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JP2014527560A (ja) | 2014-10-16 |
WO2013019509A1 (en) | 2013-02-07 |
US10125319B2 (en) | 2018-11-13 |
US20130026075A1 (en) | 2013-01-31 |
JP6215826B2 (ja) | 2017-10-18 |
KR101955702B1 (ko) | 2019-03-07 |
CN107446620A (zh) | 2017-12-08 |
US20190136139A1 (en) | 2019-05-09 |
EP2737009A1 (en) | 2014-06-04 |
KR20140064800A (ko) | 2014-05-28 |
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