CN1245485C - 制备蜡状萃余液的方法 - Google Patents

制备蜡状萃余液的方法 Download PDF

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CN1245485C
CN1245485C CNB028074203A CN02807420A CN1245485C CN 1245485 C CN1245485 C CN 1245485C CN B028074203 A CNB028074203 A CN B028074203A CN 02807420 A CN02807420 A CN 02807420A CN 1245485 C CN1245485 C CN 1245485C
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G·R·B·杰迈恩
D·J·韦德洛克
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Abstract

通过以下步骤制备蜡状萃余液产物的方法，(a)氢化裂解/加氢异构化费-托衍生原料，其中在费-托产物中，具有至少60个或更多碳原子的化合物以及具有至少30个碳原子的化合物的重量比为至少为0.2，并且在费-托衍生原料中，至少30wt%的化合物具有至少30个碳原子，(b)从步骤(a)的产物中分离蜡状产物，所述产物的T10wt%沸点介于200-450℃之间，T90wt%沸点介于400-650℃之间。

Description

制备蜡状萃余液的方法
本发明涉及一种从费-托产物制备蜡状萃余液(waxy raffinate)的方法。已经发现，用该方法得到的蜡状萃余液可以用作制备润滑基油的原料。所述基油的制备和蜡状萃余液的制备可以在不同的地点进行。蜡状萃余液的制备适合在制备费-托产物的地点进行，而润滑基油的制备适合在邻近这些产物的主要市场的地点进行。这些地点通常是不同的，导致蜡状萃余液产物必须通过，例如船舶，运送至润滑基油的生产地点。这种制备基油的方式是有利的，因为只需将一种产物航运至潜在的基油和润滑剂市场，而无需运输由蜡状萃余液产物制备的各种级别的基油。本申请人现已发现了一种制备所述蜡状萃余液产物的方法，所述产物是可运输的，并且从中可以制得一种新等级的基油。
例如，在WO-A-0014179、WO-A-0014183、WO-A-0014187和WO-A-0014188中描述的现有技术的基油含有至少95wt％非环异链烷烃。WO-A-0118156描述了一种从环烷含量低于10％的费-托产物衍生的基油。已经发现，在本申请人的专利申请EP-A-776959或EP-A-668342中公开的基油含有低于10wt％环烷。申请人重复了EP-A-776959的实施例2和3，由蜡状费-托合成产物得到了基油，其中基油分别由96wt％和93wt％异-和正-链烷烃组成。本申请人还使用根据EP-A-668342的教导制备的含合成镁碱沸石(ferrierite)和铂的催化剂，通过将Shell MDS Waxy Raffinate(得自Shell MDS Malaysia SdnBhd)催化脱蜡，制备倾点为-21℃的基油，并且发现异-和正链烷烃的含量约为94％。因此，现有技术中这些由费-托合成产物衍生的基油中，环烷的含量至少低于10wt％。此外，如申请WO-A-9920720的实施例所公开的基油中，环烷的含量将不会很高。这是由于在所述实施例中使用的原料和制备方法与用于制备基于EP-A-776959和EP-A-668342的现有技术样品的原料和制备方法非常类似。
本申请人已经发现了一种制备蜡状萃余液产物的方法，由所述产物可以制备与现有基油相比，环烷含量更高并且溶解力得以改善的润滑基油。这一发现对于，例如含有大量本发明基油的工业制剂，诸如汽轮机油和液压机油是有利的。此外，与现有技术的基油相比，本发明的基油组合物将导致，例如发动机中密封圈更加膨胀。这是有利的，在特定用途中可以观察到所述膨胀使得润滑剂损失更少。本申请人已经发现，所述基油是具有改进的溶解力特性的优异的API III族基油。
本发明涉及以下方法，通过以下步骤制备蜡状萃余液产物：
(a)氢化裂解/加氢异构化费-托衍生原料，其中在费-托产物中，具有至少60个或更多碳原子的化合物以及具有至少30个碳原子的化合物的重量比至少为0.2，并且其中在费-托衍生原料中，至少30wt％的化合物具有至少30个碳原子，
(b)从步骤(a)的产物中分离蜡状萃余液产物，所述产物的T10wt％沸点介于200-450℃之间，T90wt％沸点介于400-650℃之间。
本申请人发现，使用相对重质的原料进行氢化裂解/加氢异构化步骤，得到的蜡状萃余液产物可制备有用的产物，诸如本申请所述的基油产物。另一个优点是，适用于制备基油的，诸如汽油的燃料，以及蜡状萃余液产物是在一个氢化裂解/加氢异构化反应步骤中进行的。
本发明的方法还生产出具有特别良好的冷流特性的中间馏分油。这些优异的冷流特性也许可以由异/正比相对较高以及尤其是二-和/或三甲基化合物的量相对较高而解释。然而，柴油馏分的十六烷值远远超出60是非常优异的，通常是得到70或更高的值。此外，硫含量非常低，一般小于50ppmw，通常小于5ppmw，大部分情况下，硫含量是零。而且，尤其是柴油馏分的密度低于800kg/m3，大部分情况下观察到密度为765-790kg/m3之间，通常约780kg/m3(在100℃下，这样一个样品的粘度约为3.0cSt)。芳族化合物事实上不存在，即低于50ppmw，这使得粒子发射量非常低。聚芳族化合物的含量甚至比芳族化合物的含量还低，通常低于1ppmw。结合了上述特性的T95低于380℃，一般低于350℃。
上述方法得到的中间馏分油具有非常良好的冷流特性。例如，任何柴油馏分的浊点通常低于-18℃，甚至常常低于-24℃。CFPP通常低于-20℃，经常是-28℃或更低。倾点通常低于-18℃，通常低于-24℃。
用于步骤(a)的相对重质的费-托衍生原料中，具有至少30个碳原子的化合物的含量至少为30wt％，优选至少50wt％，更优选至少55wt％。此外，费-托衍生原料中，具有至少60个或更多碳原子的化合物与具有至少30个碳原子的化合物的重量比至少是0.2，优选至少是0.4，更优选至少是0.55。费-托衍生原料优选衍生自包含ASF-α值(Anderson-Schulz-Flory链增长因子)至少是0.925，优选至少是0.935，更优选至少是0.945，更加优选至少是0.955的C20+馏分的费-托产物。
费-托衍生原料的初始沸点最高为400℃，但优选低于200℃。优选在将费-托合成产物用作步骤(a)的费-托衍生原料之前，至少从费-托合成产物中分离出任何具有4个或更少碳原子的化合物以及任何沸点在上述范围的化合物。以上详细描述的费-托衍生原料将大部分由费-托合成产物组成，所述费-托合成产物并未进行过本发明定义的氢化转化步骤。因此在费-托合成产物中，非支链化合物的含量将超过80wt％。除了该费-托产物之外，其它馏分也可以构成费-托衍生原料的一部分。适合的其它馏分可以是在步骤(b)中得到的不能航运至润滑油制造厂的任何高沸点馏分，或任何剩余的蜡状萃余液产物。通过循环该馏分，可以制备额外的中间馏分油。
通过生产出相对重质的费-托产物的费-托法得到的所述费-托衍生原料是适合的。不是所有的费-托法均能生产所述重质产物。在WO-A-9934917和AU-A-698392中描述了适合的费-托法的例子。这些方法可以生产出上述费-托产物。
费-托衍生原料和所得蜡状萃余液产物中，不含或仅含非常少量的含硫和氮的化合物。这对于由使用几乎不含杂质的合成气的费-托反应所衍生的产物而言是常见的。硫和氮的含量通常低于检测范围，目前硫的检测范围是5ppm，而氮是1ppm。
任选将费-托衍生原料进行温和的加氢处理步骤，以除去费-托反应的反应产物中的任何含氧物质并使烯烃化合物饱和。在EP-B-668342中描述了这样的加氢处理。氢化处理步骤的温和程度是以该步骤中转化程度低于20wt％，更优选低于10wt％而表示的。此处的转化率定义为沸点高于370℃的原料中，反应为沸点低于370℃的馏分的重量百分比。在所述温和的加氢处理之后，优选在将流出物用于步骤(a)之前，从中除去具有4个或更少碳原子的低沸点化合物以及沸点在上述范围的其它化合物。
步骤(a)的氢化裂解/加氢异构化反应优选在氢气和催化剂的存在下进行的，其中催化剂选自本领域技术人员已知适用于该反应的催化剂。在步骤(a)中使用的催化剂通常含有酸性官能度以及氢化/脱氢官能度。优选的酸性官能度是耐火(refractory)金属氧化物载体。适合的载体材料包括二氧化硅、氧化铝、二氧化硅-氧化铝、氧化锆、二氧化钛及其混合物。在本发明方法中使用的催化剂中，优选的载体材料是二氧化硅、氧化铝和二氧化硅-氧化铝。特别优选的催化剂含有负载于二氧化硅-氧化铝载体上的铂。如果需要，可以向载体上施加卤素部分，特别是氟，或亚磷部分，以增强催化剂载体的酸度。在WO-A-0014179、EP-A-532118、EP-A-666894以及较早引用的EP-A-776959中描述了适合的氢化裂解/加氢异构化反应和适合的催化剂的例子。
优选的氢化裂解/加氢异构化官能度是VIII族非贵金属，例如镍和钴，任选与钼或铜结合，以及VIII族贵金属，例如钯，更优选铂或铂/钯合金。催化剂中，贵金属氢化/脱氢活性组分的含量是0.005-5重量份，优选0.02-2重量份/每100重量份载体材料。特别优选用于加氢转化步骤的催化剂中，铂的含量是0.05-2重量份，更优选0.1-1重量份/每100重量份载体材料。催化剂还含有粘合剂，以增强催化剂的强度。粘合剂可以是非酸性的。例如粘土和本领域技术人员已知的其它粘合剂。
在步骤(a)中，原料与氢气在催化剂的存在下，于升高的温度和压力下接触。温度通常在175-380℃的范围内，优选高于250℃，并且更优选300-370℃。压力通常在10-250bar，优选20-80bar的范围内。氢气以100-10000Nl/l/hr，优选500-5000Nl/l/hr的气体时空速供应。烃进料以0.1-5kg/l/hr，优选高于0.5kg/l/hr，更优选低于2kg/l/hr的重时空速提供。氢气与烃进料之比值在100-5000Nl/kg，优选250-2500Nl/kg的范围内。
步骤(a)的转化率定义为沸点高于370的原料中反应转化为沸点低于370的馏分的重量百分比，其至少为20wt％，优选至少25wt％，但优选不超过80wt％，更优选不超过70wt％。在上述定义中使用的进料是步骤(a)的总烃进料，因此，也可以是在步骤(b)得到的高沸点馏分的任选循环馏分。
在步骤(b)中，步骤(a)的产物被分离为一种或多种粗柴油馏分、蜡状萃余液产物，该蜡状萃余液产物具有200-450℃之间的T10wt％沸点，以及400-650℃之间的T90wt％沸点，更优选T90wt％沸点低于550℃。根据步骤(a)的转化率和步骤(a)的总进料特性，在步骤(b)中还可以得到一个较高沸点的馏分。
步骤(b)中的分离优选通过在约大气压条件，优选在1.2-2bar的压力下的第一蒸馏进行，其中从步骤(a)产物的高沸点馏分中分离粗柴油产物和低沸点馏分，诸如石脑油和煤油馏分。其中至少95wt％沸点高于370℃的高沸点馏分随后在真空蒸馏步骤中进一步分离，其中得到真空粗柴油馏分、蜡状萃余液产物和高沸点馏分。真空蒸馏适合在0.001-0.05bar的压力下进行。
步骤(b)的真空蒸馏优选在这样的条件下操作：得到的所需蜡状萃余液产物的沸点在特定范围内，并且在100℃下的运动粘度优选为3-10cSt。
在上述方法中得到的蜡状萃余液产物所具有的特性，诸如倾点和粘度使其适于通过船舶运输至润滑基油的生产场所。优选在无氧下储存和运输蜡状萃余液，以避免蜡转萃余液中存在的链烷烃分子被氧化。在所述储存和运输过程中，施加氮气保护气是合适的。优选蜡状萃余液具有的倾点高于0℃。这使得可以例如通过将产物保持在室温，以固体形式运输蜡状萃余液。运输固体状态的产物是有利的，因为进一步限制了氧气的吸入并因此避免了氧化。在卸料装置中将产物液化的方法是存在的。优选在储罐中存在间接加热装置，诸如蒸汽加热盘管，这样，可以在从储罐卸料之前将产物液化。运输管线中也优选配备将产物保持液态的装置。
蜡状萃余液产物可用于各种应用。最适合的应用是使用蜡状萃余液产物作为原料，通过对蜡状萃余液产物进行倾点下降步骤，以制备润滑基油。任选在对蜡状萃余液产物进行倾点下降步骤之前，使蜡状萃余液产物与疏松石蜡掺合，以提高疏松石蜡与硫、氮和饱和物含量有关的特性。
倾点下降处理被理解为以下每一种方法，其中基油的倾点下降超过10℃，优选超过20℃，更优选超过25℃。
倾点下降处理可以通过所谓溶剂脱蜡法或催化脱蜡法的方法而进行。溶剂脱蜡法是一种本领域技术人员熟知的方法，包括将一种或多种溶剂和/或蜡沉淀剂与蜡状萃余液产物混合，并将混合物的温度冷却至-10℃至-40℃，优选-20℃至-35℃的范围内，以从油中分离蜡。通常将含蜡的油通过可以由诸如棉的纺织纤维制备的滤布、多孔金属布或由合成材料制备的滤布进行过滤。在溶剂脱蜡法中使用的溶剂的例子是C3-C6酮(例如甲基乙基酮、甲基异丁基酮及其混合物)、C6-C10芳族烃(例如甲苯)、酮和芳族烃的混合物(例如甲基乙基酮和甲苯)、自冷溶剂，诸如液化的通常为气体的C2-C4烃，诸如丙烷、丙烯、丁烷、丁烯及其混合物。通常优选甲基乙基酮和甲苯或甲基乙基酮和甲基异丁基酮的混合物。在Lubricant Base Oil and Wax Processing，Avilino Sequeira，Jr，Marcel Dekker Inc.，New York，1994，第7章中描述了这些和其它适合的溶剂脱蜡法的例子。
优选的倾点下降法是催化脱蜡法。已经发现，当以本发明的蜡状萃余液产物为原料时，使用该方法制备的基油甚至具有低于-40℃的倾点。
催化脱蜡法可以通过以下任何方法制备：其中在催化剂和氢气存在下，蜡状萃余液产物的倾点下降至上述定义的范围。适合的脱蜡催化剂是含有分子筛和任选结合的具有氢化官能的金属，诸如VIII族金属的多相催化剂。在催化脱蜡条件下，分子筛，以及更适合的中孔尺寸沸石显示出降低蜡状萃余液产物倾点的良好催化活性。优选中孔尺寸沸石具有的孔直径为0.35-0.8nm。适合的中孔尺寸沸石是丝光沸石、ZSM-5、ZSM-12、ASM-22、ASM-23、SSZ-32、ZSM-35和ZSM-48。另一组优选的分子筛是例如US-A-4859311中描述的磷酸硅铝材料(SAPO)，其中最优选SAPO-11。ZSM-5任选在无任何VIII族金属的存在下，以其HZSM-5形式使用。其它分子筛优选与加入的VIII族金属结合使用。适合的VIII族金属是镍、钴、铂和钯。可能的结合形式是，例如Pt/ZSM-35、Ni/ZSM-5、Pt/ZSM-23、Pd/ZSM-23、Pt/ZSM-48和Pt/SAPO-11。例如，在WO-A-9718278、US-A-4343692、US-A-5053373、US-A-5252527和US-A-4574043中描述了适合的分子筛和脱蜡条件的更多细节和例子。
脱蜡催化剂还适合含有粘合剂。粘合剂可以是合成或天然存在(无机)物质，例如粘土、二氧化硅和/或金属氧化物。天然存在的粘土是，例如蒙脱石和高岭土类。粘合剂优选是多孔粘合剂材料，例如耐火氧化物，例如氧化铝、二氧化硅-氧化铝、二氧化硅-氧化镁、二氧化硅-氧化锆、二氧化硅-氧化钍、二氧化硅-氧化铍，二氧化硅-二氧化钛以及三元组合物，例如二氧化硅-氧化铝-氧化钍、二氧化硅-氧化铝-氧化锆、二氧化硅-氧化铝-氧化镁和二氧化硅-氧化镁-氧化锆。更优选使用基本不合氧化铝的低酸度耐火氧化物粘合剂材料。这样的粘合剂材料的例子是，二氧化硅、氧化锆、二氧化钛、二氧化锗、氧化硼(boria)以及上述列举的这些例子的两种或多种的混合物。最优选的粘合剂是二氧化硅。
最优选的一类脱蜡催化剂包括上述的中孔沸石催化剂和上述基本不合铝的低酸度耐火氧化物粘合剂材料，其中硅铝酸盐沸石晶粒的表面已经通过将硅铝酸盐沸石晶粒进行表面脱铝处理而改性。优选的脱铝处理是，例如按照US-A-5157191或WO-A-0029511所述，将粘合剂和沸石的挤出物与氟硅酸盐的水溶液接触。例如按照WO-A-0029511和EP-B-832171所述，上述合适的脱蜡催化剂的例子是结合了二氧化硅并脱铝的Pt/ZSM-5，更优选结合了二氧化硅并脱铝的Pt/ZSM-23、结合了二氧化硅并脱铝的Pt/ZSM-12、结合了二氧化硅并脱铝的Pt/ZSM-22。
催化脱蜡条件是本领域已知的，通常包括在200-500℃、优选250-400℃的操作温度，10-200bar、优选40-70bar的氢气压力，0.1-10kg油/每升催化剂/每小时(kg/l/hr)、优选0.2-5kg/l/hr、更优选0.5-3kg/l/hr的重时空速(WHSV)以及100-2000升氢气/每升油的氢油比。通过在催化脱蜡步骤中，在40-70bar下，于275，优选315至375℃之间改变温度，可以制备出具有优选在-10至-60℃之间变化的不同倾点的基油。
例如，当流出物含有烯烃或当产物对氧化敏感或当需要提高色度时，任选将催化剂或溶剂脱蜡步骤的流出物或不同沸点的馏分进行额外的加氢步骤，称为加氢精制步骤。该步骤适合在180-380℃的温度、10-250bar、优选高于100bar、更优选在120-250bar的总压下进行。WHSV(重时空速)在0.3-2kg油/每升催化剂/每小时(kg/1.h)范围内。
氢化催化剂适合为含有分散的VIII族金属的载体催化剂。VIII族金属可以是钴、镍、钯和铂。含钴和镍的催化剂还可以含有VIB族金属，适合的是钼和钨。适合的载体和支持物材料是低酸度无定形耐火氧化物。适合的无定形耐火氧化物的例子包括无机氧化物，诸如氧化铝、二氧化硅、二氧化钛、氧化锆、氧化硼、二氧化硅-氧化铝、氟化氧化铝、氟化二氧化硅-氧化铝及其二种或多种的混合物。
适合的氢化催化剂的例子是含镍-钼的催化剂，诸如KF-847和KF-8010(AKZO Nobel)、M-8-24和M-8-25(BASF)以及C-424、DN-190、HDS-3和HDS-4(Criterion)；含镍-钨的催化剂，诸如NI-4342和NI-4352(Engelhard)和C-454(Criterion)；含钴-钼的催化剂，诸如KF-330(AKZO-Nobel)、HDS-22(Criterion)和HPC-601(Engelhard)。优选使用含铂的催化剂，更优选使用含铂和钯的催化剂。用于这些含钯和/或铂催化剂的优选载体是无定形二氧化硅-氧化铝。在WO-A-9410263zhong公开了适合的二氧化硅-氧化铝载体的例子。优选的催化剂含有优选负载于无定形二氧化硅-氧化铝载体上的钯和铂的合金，例如市场出售的Criterion CatalystCompany(Houston，TX)的催化剂C-624。
脱蜡产物适合通过蒸馏手段，任选结合初始闪蒸步骤，分离为一种或多种具有不同粘度的基油产物。分离为不同馏分的步骤适合在带有侧汽提器的真空蒸馏塔中进行，以从所述塔中分离馏分。发现按照该方式，可以由单一的蜡状萃余液产物同时得到例如，一种粘度为2-3cSt的基油、一种粘度为4-6cSt的基油以及一种粘度为7-10cSt的基油(粘度是在100℃下的运动粘度)。发现通过直接优化产物状态并使非基油中间馏分的量最小化，可以以高收率制备具有良好Noack挥发特性的基油。例如，得到的在100℃下具有3.5-6cSt的运动粘度的基油所具有的Noack挥发度为6-14wt％。
已经发现，以该蜡状萃余液产物为原料制备润滑基油，所述基油优选含有至少98wt％饱和物、优选至少99.5wt％饱和物以及最优选至少99.9wt％饱和物。基油中的所述饱和物馏分含有10-40wt％环烷。环烷含量优选低于30wt％，更优选低于20wt％。环烷含量优选至少为12wt％。独特和新颖的基油的特征还在于1-环环烷与具有二个或多个环的环烷的重量比为3，优选大于5。发现该比例小于15是合适的。
上述环烷含量是通过以下方法测定的。也可以使用能够得到类似结果的其它任何方法。首先通过使用高效液相色谱(HPLC)法IP368/01，将基油样品分离为极性(芳烃)相和非极性(饱和物)相，其中该方法强调使用戊烷代替己烷作为流动相。随后使用装配了场解吸/场致电离(FD/FI)界面的Finnigan MAT90质谱仪分析饱和物和芳烃馏分，其中FI(“软”电离技术)用于根据碳数目和氢缺乏进行的烃类型的半定量测定。根据形成的特征离子测定质谱中的化合物类型，并通常用“z数”分类。对于所有烃种类，可以给出通式CnH2n+z。因为饱和相是与芳烃相分别分析的，因此可以测定具有相同化学计量的不同(环)烷的含量。使用商用软件(poly 32；Sierra AnalyticsLLC，3453 Dragoo Park Drive，Modesto，California GA95350USA)处理质谱仪的结果，以测定各个烃类型的相对比例，以及饱和物和芳烃馏分的平均分子量和多分散性。
基油组合物中，芳烃含量优选低于1wt％，更优选低于0.5wt％，最优选低于0.1wt％，硫含量低于20ppm，氮含量低于20ppm。基油的倾点优选低于-30℃，更优选低于-40℃。粘度指数高于120。已经发现，新颖的基油通常具有低于140的粘度指数。
基油本身可以部分作为例如，Automatic Transmission Fluids(ATF)、内燃机(汽油机或柴油机)机油、汽轮机油、液压机油、电机机油或变压器油和冷冻机油。
使用以下非限制性实施例阐述本发明。
实施例1
通过将使用WO-A-9934917实施例III的催化剂，按照实施例VII得到的费-托产物的C5-C750℃+馏分连续进料至氢化裂解步骤(步骤(a))，得到蜡状萃余液产物。原料含有约60wt％的C30+产物。C60+/C30+的比例约为0.55。在氢化裂解步骤中，馏分与EP-A-532118的实施例1的氢化裂解催化剂接触。
连续蒸馏步骤(a)的流出物，得到轻质馏分、燃料和沸点370℃和以上的残余物“R”。在氢化裂解步骤中，基于新鲜进料的粗柴油馏分的收率是43wt％。将大部分残余物“R”循环至步骤(a)，并通过真空蒸馏将剩余部分分离为具有表1特性且沸点高于510℃的蜡状萃余液产物。
氢化裂解步骤(a)的条件为：新鲜进料的重量时空速(WHSV)为0.8kg/l.h，循环进料WHSV为0.2kg/l.h，氢气速率＝1000Nl/kg，总压＝40bar，反应器温度335℃。
                         表1
  70℃的密度(kg/m3)   779.2
  vK@100(cSt)   3.818
  倾点(℃)   +18
  在回收的wt％下，沸点的温度数据   5％355℃10％370℃50％419℃90％492℃95％504℃
实施例2
通过将实施例1的蜡状萃余液产物与如WO-A-0029511的实施例9所述，含0.7wt％Pt和30wt％ZSM-5的脱铝二氧化硅结合ZSM-5催化剂接触，而将产物脱蜡，以制备基油。脱蜡条件是氢气40bar、WHSV＝1kg/l.h和温度340℃。
将脱蜡油蒸馏分离为三种基油馏分：沸点介于378-424℃(基于脱蜡步骤进料的收率为14.2wt％)的馏分、介于418-455℃的馏分(基于脱蜡步骤进料的收率为16.3wt％)和沸点高于455℃(基于脱蜡步骤进料的收率为21.6wt％)的馏分。详细结果见表2。
                                  表2
  轻质馏分   中间馏分   重质馏分
  20℃下的密度   805.8   814.6   822.4
  倾点(℃)   ＜-63   ＜-51   -45
  40℃下的运动粘度(cSt)   19.06   35.0
  100℃下的运动粘度(cSt)   3.16   4.144   6.347
  VI   n.a   121   134
  Noack挥发度(wt％)   n.a.   10.8   2.24
  硫含量(ppm)   ＜1ppm   ＜1ppm   ＜5ppm
  饱和物(％w)   n.a   99.9   n.a
  环烷含量(wt％)(*)   n.a.   18.5   n.a.
  在-40℃通过CCS测定的动态粘度   n.a.   3900cP   n.a
(*)使用装配了场解吸/场致电离(FD/FI)界面的Finnigan MAT90质谱仪分析所述基油的饱和物馏分。
n.a.：不适用
n.d.：未测出
实施例3
重复实施例2，除了将脱蜡基油蒸馏分离为具有表3所示特性的三种不同基油产物。
                                  表3
  轻质馏分   中间馏分   重质馏分
  20℃下的密度   809.1   817.2   825.1
  倾点(℃)   ＜-63   ＜-51   -39
  40℃下的运动粘度(cSt)   23.32   43.01
  100℃下的运动粘度(cSt)   3.181   4.778   7.349
  VI   n.a   128   135
  Noack挥发度(wt％)   n.a.   7.7   n.a.
  硫含量(ppm)   ＜5ppm   ＜5ppm   ＜5ppm
  饱和物(％w)   99.0
  在-40℃通过CCS测定的动态粘度   5500cp
  基于催化脱蜡步骤进料的收率(wt％)   15.3   27.4   8.9
实施例4
重复实施例2，除了将脱蜡基油蒸馏分离为具有表4所示特性的三种不同基油产物和一种中间萃余液(I.R.)。
                                      表4
  轻质馏分   I.R.   中间馏分   重质馏分
  20℃下的密度   806   811.3   817.5   824.5
  倾点(℃)   ＜-63   -57   ＜-51   -39
  40℃下的运动粘度(cSt)   10.4   23.51   42.23
  100℃下的运动粘度(cSt)   2.746   3.501   4.79   7.24
  VI   103   127   135
  Noack挥发度(wt％)   n.a.   6.8   1.14
  硫含量(ppm)   ＜5ppm   ＜5ppm   ＜5ppm
  饱和物(％w)   n.d.   99.5
  在-40℃通过CCS测定的动态粘度   5500cP
  基于CDW进料的收率(wt％)   22.6   8.9   22.6   11.1
n.a.：不适用
n.d.：未测出
实施例2-4阐述了由通过本发明方法得到的蜡状萃余液产物，以高收率制备基油，并且该基油具有优异的粘度特性。

Claims (10)

1.通过以下步骤制备蜡状萃余液产物的方法，
(a)氢化裂解/加氢异构化费-托衍生原料，其中在费-托产物中，具有至少60个或更多碳原子的化合物以及具有至少30个碳原子的化合物的重量比至少为0.4，并且在费-托衍生原料中，至少30wt％的化合物具有至少30个碳原子，
(b)从步骤(a)的产物中分离蜡状萃余液产物，所述产物的T10wt％沸点介于200-450℃之间，T90wt％沸点介于400-650℃之间。
2.权利要求1的方法，其中费-托衍生原料中至少50wt％化合物具有至少30个碳原子。
3.权利要求1-2任一项的方法，其中费-托衍生原料衍生自包含ASF-α值(Anderson-Schulz-Flory链增长因子)至少是0.925的C20+馏分的费-托产物。
4.权利要求1-2任一项的方法，其中步骤(a)的转化率是25-70wt％。
5.权利要求1-2任一项的方法，其中蜡状萃余液产物的T90wt％沸点低于550℃。
6.权利要求1-2任一项的方法，其中蜡状萃余液产物在100℃的运动粘度为3-10cSt。
7.权利要求1-2任一项的方法得到的蜡状萃余液产物制备润滑基油的用途。
8.权利要求7的用途，其中基油是通过将蜡状萃余液产物催化脱蜡而制备的。
9.权利要求8的用途，其中润滑基油的饱和物馏分中，环烷含量是12-20wt％。
10.权利要求7的用途，其中蜡状萃余液产物具有高于0℃的倾点，并且蜡状萃余液产物以固体状态和在氮气保护下运输至润滑基油的生产场所。
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MY139353A (en) 2009-09-30
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BR0207891A (pt) 2004-03-23
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US7285206B2 (en) 2007-10-23
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