CN1608121A - 制备润滑基础油和粗柴油的方法 - Google Patents
制备润滑基础油和粗柴油的方法 Download PDFInfo
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Abstract
一种制备两种或多种润滑基础油级分和粗柴油的方法,所述方法通过(a)加氢裂化/加氢异构化费-托产品,其中在费-托产品中具有至少60个或更多碳原子的化合物与具有至少30个碳原子的化合物之间的重量比为至少0.2,并且其中在费-托产品中至少有30wt%的化合物具有至少30个碳原子,(b)将步骤(a)的产品分离成一种或多种粗柴油馏分和一种基础油前体馏分,(c)对步骤(b)中得到的基础油前体馏分进行倾点降低步骤,和(d)分离步骤(c)的流出物为两个或多个基础油级分。
Description
本发明涉及一种由费-托(Fischer-Tropsch)产品制备润滑基础油和粗柴油的方法。
这种方法可由EP-A-776959得知。该出版物描述了一种方法,其中费-托合成产品的高沸点馏分首先在被二氧化硅/氧化铝载带的Pd/Pt催化剂存在时进行加氢异构化。非环状异链烷烃含量超过80wt%的异构化产品随后进行倾点降低步骤。在其中的一个实施例中所公开的倾点降低步骤为在被二氧化硅载带的脱铝ZSM-23催化剂存在时在310℃下进行催化脱蜡步骤。
这种方法的一个缺点是仅制备了一个基础油级分。另一个缺点是加氢异构化步骤是针对费-托合成产品的窄沸程馏分进行的,其中加氢异构化步骤主要用来制备具有所希望特性的基础油前体馏分。如果进料还包括沸点更低的化合物,则加氢异构化处理步骤也可以产生除基础油前体馏分以外的有用的中间馏分。因此存在一种愿望,希望由蜡状链烷烃馏分来制备基础油,所述蜡状链烷烃馏分可以从加氢异构化处理步骤得到,而所述加氢异构化处理步骤产生中间馏分如石脑油、煤油和粗柴油以及非环状异链烷烃含量超过90wt%的蜡状链烷烃馏分。还存在一种愿望,希望找到一种灵活的方法来得到具有优良质量的具有不同粘度特性的两种或多种基础油。
本发明的目的是提供一种方法,其中可以达到粗柴油的高产率,并且其中由蜡状费-托产品制备具有不同粘度特性的两种或多种高质量的基础油。
这个目的通过下列过程来实现。该方法通过如下步骤来制备两种或多种润滑基础油级分和粗柴油:
(a)加氢裂化/加氢异构化费-托产品,其中在费-托产品中具有至少60个或更多碳原子的化合物和具有至少30个碳原子的化合物的重量比为至少0.2,并且其中在费-托产品中至少30wt%的化合物具有至少30个碳原子,
(b)将步骤(a)的产品分离成一种或多种粗柴油馏分和一种基础油前体馏分,
(c)对步骤(b)中得到的基础油前体馏分进行倾点降低步骤,以及
(d)分离步骤(c)的流出物为两个或多个基础油级分。
本申请人发现通过应用相对重的原料进行加氢裂化/加氢异构化步骤,可以得到按步骤(a)的进料计算的较高的粗柴油产率。另一优点是在一个加氢裂化/加氢异构化处理步骤中可以同时制备燃料如粗柴油和适于制备基础油的材料。这种生产路线比在如WO-A-0014179中所描述的对沸点主要在370℃以上的费-托蜡进行的专用于基础油的加氢裂化/加氢异构化步骤的生产路线来说要更简单。另一个优点是可以同时制备两个或多个具有不同动力学粘度即在100℃时为2cSt至12cSt以上的基础油级分。
另一优点是制备了环烷烃含量相对高的基础油,而这对实现所希望的溶解特性来说是有利的。在所得到的基础油的饱和馏分中环烷烃含量可以为5-40wt%。已经发现对于调配发动机润滑油来说饱和馏分中环烷烃含量为12-20wt%的基础油是很好的基础原料。
本发明的方法还产生具有非常好的冷流动特性的中间馏分。这些非常好的冷流动特性或许可以由相对高的异/正化合物特别是相对高的二和/或三甲基化合物的量来解释。但柴油馏分的十六烷值在远超过60的值时是更好的,经常得到的值为70或更高。另外,硫含量非常低,总是低于50ppmw,通常低于5ppmw,并且在大多数情况下硫含量为零。另外,柴油馏分的密度具体低于800kg/m3,在大多数情况下所观察到的密度值为765-790kg/m3,通常在780kg/m3左右(这种样品的粘度为约3.0cSt)。芳族化合物几乎没有即低于50ppmw,从而导致非常低的颗粒排放。聚芳族化合物含量甚至比芳族化合物含量还低,通常低于1ppmw。与上述特性相组合的T95低于380℃,通常低于350℃。
上述方法产生具有极好的冷流动特性的中间馏分。例如任何柴油馏分的浊点通常低于-18℃,甚至经常低于-24℃。CFPP.通常低于-20℃,经常为-28℃或更低。倾点通常低于-18℃,经常低于-24℃。
用于步骤(a)中的相对重的费-托产品具有至少30wt%,优选至少50wt%,并且更优选至少55wt%的化合物具有至少30个碳原子。另外,费-托产品的具有至少60个或更多碳原子的化合物与具有至少30个碳原子的化合物之间的重量比为至少0.2,优选为至少0.4,并且最优选为至少0.55。费-托产品优选包括ASF-α值(Anderson-Schulz-Flory链生长因子)为至少0.925的C20 +馏分,优选为至少0.935,更优选为至少0.945,甚至进一步优选为至少0.955。费-托产品的初始沸点优选低于200℃。在将费-托合成产品用于步骤(a)之前,优选将任何具有4个或更少碳原子的化合物和沸点在该范围内的任何化合物从该产品中分离出来。上面详细描述的费-托产品是没有进行本发明所定义的加氢转化步骤的费-托产品。因此在费-托产品中非支链化合物的含量将超过80wt%。除了费-托产品外,在步骤(a)中也可以附加地处理其它馏分。进料至步骤(a)的其它可能馏分可以适当地为不能在步骤(c)中被处理的基础油前体馏分的一部分和/或在步骤(d)得到的不合格基础油馏分。
这种费-托产品可以通过任何得到相对重的费-托产品的方法得到。并不是所有的费-托方法都得到这种重的产品。在WO-A-9934917和AU-A-698392中描述了合适的费-托方法的例子。这些方法可以得到上述费-托产品。
费-托产品将不含或含有非常少的含硫和含氮化合物。这对于由应用几乎不含杂质的合成气的费-托反应得到的产品来说是常见的。因此硫和氮含量通常分别低于1ppmw。
费-托产品可以通过使费-托反应的反应产品进行适度的加氢处理步骤,从而脱除任何氧化物以及使任何烯属化合物饱和而得到。在EP-B-668342中有描述了这种加氢处理。所述加氢步骤的适度程度优选表示为该步骤的转化程度低于20wt%,并且更优选低于10wt%。转化率在这里被定义为沸点高于370℃的进料的重量百分比,这些进料反应生成沸点低于370℃的馏分。经过这样一个适度的加氢处理后,当其作为上述的费-托产品而在步骤(a)中应用之前,具有四个或更少碳原子的沸点较低的化合物以及在该沸程的其它化合物优选从流出物中脱除。
步骤(a)的加氢裂化/加氢异构化反应优选在氢和适合于该反应过程的催化剂存在时进行,而所述催化剂对本领域熟练技术人员来说是已知的。用于步骤(a)中的催化剂通常包括酸性官能团和加氢/脱氢官能团。优选的酸性官能团为耐熔的金属氧化物载体。合适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。在本发明方法中应用的催化剂中包括的优选载体材料为二氧化硅、氧化铝和二氧化硅-氧化铝。特别优选的催化剂包括载带在二氧化硅-氧化铝载体上的铂。如果需要,向载体上施加卤素部分具体为氟或磷部分,可以提高催化剂载体的酸度。
优选的加氢/脱氢官能团为VIII族贵金属,例如钯,更优选为铂。以每100重量份载体材料为基准,催化剂可以包括其量为0.005-5重量份的加氢/脱氢活性组分,优选为0.02-2重量份。以每100重量份载体材料为基准,用于加氢转化阶段的特别优选的催化剂包括其量为0.05-2重量份的铂,更优选为0.1-1重量份。所述催化剂还可以含有粘结剂以提高催化剂的强度。所述粘结剂可以为非酸性的。其例子包括本领域熟练技术人员已知的粘土和其它粘结剂。在WO-A-0014179、EP-A-532118、EP-A-666894和更早参考的EP-A-776959中描述了适当的加氢裂化/加氢异构化方法的例子和适当的催化剂的例子。
在步骤(a)中所述进料在催化剂存在时在升高的温度和压力下与氢接触。所述温度范围通常为175-380℃,优选高于250℃,更优选为300-370℃。所述压力范围通常为10-250bara,优选为20-80bara。氢可以按气体小时空速为100-10000Nl/l/hr供给,优选为500-5000Nl/l/hr。烃进料可以按重量小时空速为0.1-5kg/l/hr供给,优选高于0.5kg/l/hr,更优选低于2kg/l/hr。氢与烃进料的比的范围可以为100-5000Nl/kg,并且优选为250-2500Nl/kg。
按单程反应生成沸点低于370℃的馏分的沸点高于370℃的进料的重量百分比定义,步骤(a)中的转化率为至少20wt%,优选为至少25wt%,但优选不超过80wt%,更优选不超过70wt%。上面定义中所应用的进料为进料至步骤(a)的全部烃进料,例如包括所有的循环物流。
在步骤(b)中,步骤(a)的产品被分离为一种或多种粗柴油馏分和一种基础油前体馏分。基础油馏分适当地具有初始沸点330-400℃。所述分离优选在约为大气压条件下通过精馏进行,所述压力优选为1.2-2bara,其中步骤(a)产品中的粗柴油产品和沸点较低的馏分如石脑油和煤油馏分与沸点较高的馏分分离。
在步骤(c)中,对步骤(b)中得到的基础油前体馏分进行倾点降低处理。对于倾点降低处理理解为在每种方法中基础油的倾点被降低10℃以上,优选为20℃以上,更优选为25℃以上。
倾点降低处理可以通过所谓的溶剂脱蜡过程或通过催化脱蜡过程进行。对本领域熟练技术人员来说,溶剂脱蜡是公知的,并且包括一种或多种溶剂和/或蜡沉淀剂与基础油前体馏分的混合物,并将混合物冷却至温度范围为-10℃至-40℃,优选为-20℃至-35℃,从而从油中分离出蜡。含有蜡的油通常通过滤布过滤,而所述滤布可以由织物纤维如棉布、多孔金属布、或由合成材料制成的布制成。在溶剂脱蜡过程中可以应用的溶剂的例子有C3-C6酮(例如甲基乙基酮、甲基异丁基酮及其混合物)、C6-C10芳烃(例如甲苯)、酮和芳烃的混合物(例如甲基乙基酮和甲苯)、自冷性溶剂如液化的、通常为气相的C2-C4烃如丙烷、丙烯、丁烷、丁烯及其混合物。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通常是优选的。这些和其它合适的溶剂脱蜡过程的例子在Lubricant Base Oil and Wax Processing,Avilino Sequeira,Jr,Marcel Dekker Inc.,New York,1994,Chapter 7中进行了描述。
步骤(c)优选通过催化脱蜡过程进行。已经发现利用这种过程当由本方法的步骤(b)中得到的基础油前体馏分开始时,可以制备倾点低于-40℃的基础油。
催化脱蜡过程可以通过任何过程来进行,其中在催化剂和氢存在时按上面所规定降低基础油前体馏分的倾点。合适的脱蜡催化剂为非均相催化剂,所述催化剂包括分子筛,任选组合有具有加氢功能的金属如第VIII族金属。分子筛以及更适当的中孔径的沸石,已经表现出很好的催化性能,从而在催化脱蜡条件下降低基础油前体馏分的倾点。中孔径的沸石优选具有0.35-0.8nm的孔径。合适的中孔径的沸石为ZSM-5、ZSM-12、ZSM-22、ZSM-23、SSZ-32、ZSM-35和ZSM-48。优选的另一组分子筛为二氧化硅-氧化铝磷酸盐(SAPO)材料,其中在US-A-4859311中所描述的SAPO-11是最优选的。ZSM-5可以任选在不存在任何第VIII族金属的情况下以其HZSM-5的形式应用。其它分子筛优选与所加入的第VIII族金属组合应用。适合的第VIII族金属为镍、钴、铂和钯。其可能组合的例子为Ni/ZSM-5、Pt/ZSM-23、Pd/ZSM-23、Pt/ZSM-48和Pt/SAPO-11。合适分子筛和脱蜡条件的进一步细节及其例子在WO-A-9718278、US-A-5053373、US-A-5252527和US-A-4574043中有述。
脱蜡催化剂还适当地包括粘结剂。所述粘结剂可以为合成的或天然存在的(无机)物质,例如粘土、二氧化硅和/或金属氧化物。天然存在的粘土例如有蒙脱土和高岭土系列。所述粘结剂优选为多孔粘结剂材料,例如耐熔的氧化物,其例子有氧化铝、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。更优选应用基本不含氧化铝的低酸度的耐熔氧化物粘合剂材料。这些粘结剂材料的例子有二氧化硅、氧化锆、二氧化钛、二氧化锗、氧化硼(boria)和上面所列的例子的两种或多种的混合物。最优选的粘结剂是二氧化硅。
优选的一类脱蜡催化剂包括如上文所述的中间沸石晶体以及上述的基本不含氧化铝的低酸度耐熔氧化物粘结剂材料,其中铝硅酸盐沸石晶体的表面已经通过使铝硅酸盐沸石晶体进行表面脱铝处理而进行了改性。优选的脱铝处理通过使粘结剂的挤出物和沸石与氟硅酸盐的水溶液接触来进行,正如US-A-5157191或WO-A-0029511中所述。上述脱蜡催化剂的合适例子为粘结二氧化硅且脱铝的Pt/ZSM-5、粘结二氧化硅且脱铝的Pt/ZSM-23、粘结二氧化硅且脱铝的Pt/ZSM-12、粘结二氧化硅且脱铝的Pt/ZSM-22,正如WO-A-0029511和EP-B-832171中所述。
催化脱蜡条件在本领域是已知的,并且通常包括范围为200-500℃的操作温度,适当地为250-400℃,氢的压力范围为10至200bar,优选为40至70bar,重量小时空速(WHSV)的范围为0.1-10kg油每升催化剂每小时(kg/l/hr),适当地为0.2-5kg/l/hr,更适当地为0.5-3kg/l/hr,并且氢油比的范围为100-2,000升氢每升油。通过在催化脱蜡步骤中在40-70bar下在275-375℃内且更优选在315-375℃内改变温度,有可能制备具有不同倾点规格的基础油,所述倾点适当地在-60至-10℃之间变化。
如果流出物含有烯烃或者当产品对氧化比较敏感或者当颜色需要改进时,在步骤(d)之前或进行步骤(d)之后,步骤(c)的流出物任选进行附加的加氢步骤,该步骤也称为加氢精制步骤。该步骤适当地在温度为180-380℃下,总压为10-250bar且优选高于100bar并且更优选在120-250bar下进行。WHSV(重量小时空速)范围为0.3-2kg油每升催化剂每小时(kg/l.h)。
所述加氢催化剂适当为含有分散的第VIII族金属的载带催化剂。可能的第VIII族金属有钴、镍、钯和铂。含有钴和镍的催化剂也可以包括第VIB族金属,适当地为钼和钨。合适的载体或载体材料为无定形耐熔氧化物。合适的无定形耐熔氧化物的例子包括无机氧化物,例如氧化铝、二氧化硅、二氧化钛、氧化锆、氧化硼(boria)、二氧化硅-氧化铝、氟化的氧化铝、氟化的二氧化硅-氧化铝以及这些物质中两种或多种的混合物。
合适的加氢催化剂的例子为含有镍-钼的催化剂,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-钨的催化剂如NI-4342和NI-4352(Engelhard)和C-454(Criterion);含钴-钼的催化剂如KF-330(AKZO-Nobel)、HDS-22(Criterion)和HPC-601(Engelhard)。优选应用含有铂的催化剂,并且更优选应用含有铂和钯的催化剂。对这些含有钯和/或铂的催化剂的优选载体为无定形二氧化硅-氧化铝。合适的二氧化硅-氧化铝载体的例子在WO-A-9410263中公开。一种优选的催化剂包括优选载带于无定形二氧化硅-氧化铝载体上的钯和铂合金,其中从criterion CatalystCompany(Houston,TX)商购得到的C-624催化剂是一个例子。
在步骤(d)中,优选通过精馏方法,并任选地与初始闪蒸步骤组合,首先适当脱除沸点较低的非基础油馏分。脱除这些沸点较低的化合物后,适当地通过精馏将脱蜡产品分离为两个或更多个基础油级分。为了符合所希望的粘度级别和各种基础油级分的挥发度要求,另外优选作为单独的馏分得到其沸点超过和/或低于所希望的基础油级分或在其之间的不合格馏分。如果这些馏分的初始沸点超过340℃,则它们可以有利地循环回到步骤(a)中。所得到的沸点在粗柴油范围或低于该范围的任何馏分可以适当地循环回到步骤(b)或另外直接与最终粗柴油产品混合。分离为各种馏分的操作也可以适当地在配有侧线汽提塔的真空精馏塔中进行,从而分离来自所述塔的馏分。
图1给出了本发明方法的一种优选实施方案。向加氢裂化反应器(2)中进料费-托产品(1)。分离气相产品后,流出物(3)被分离为石脑油馏分(5)、煤油馏分(6)、粗柴油馏分(7)和基础油前体馏分(8)。该馏分(8)的一部分通过(10)和(21)循环回到反应器(2),并且另一部分通过(9)进料至脱蜡反应器(11),所述反应器(11)通常为填料床反应器。
通过从反应器(11)的流出物中分离气相馏分和部分粗柴油馏分以及那些在催化脱蜡过程中形成的沸点在所述范围内的化合物(12),可以得到中间产品(13)。将中间产品(13)进料至真空精馏塔(14),该塔(14)配有设备如侧线汽提塔,从而沿塔的高度排放沸点在塔顶和塔底精馏产品之间的不同馏分。在图1中,作为塔(17)的精馏产品得到塔顶产品(15)、粗柴油馏分(19)、轻基础油级分(16)、中间基础油级分(17)和重基础油级分(18)。为了满足级分(17)和(18)的挥发度要求,中间馏分(20)从塔中采出并通过(21)循环回到加氢裂化器(2)中。作为(12)和(19)得到的粗柴油馏分可以循环回到精馏塔(4)中(图中未画出)。另外也有可能的是塔(14)的塔底精馏产品不能用作基础油级分。在这种情况下塔底精馏产品适当地循环回到反应器(2)中(图中未画出)。
按照本发明的方法可以适当地用于同时制备如下基础油级分:(i)在100℃时运动粘度(vK@100)为约2-4cSt的适合用作电器用油的基础油,(ii)vK@100为约2-15cSt的适合用作冷冻机油的基础油,和/或(iii)vK@100为约2至高达30cSt的适合用作处理油或作为药用白油应用的基础油。特别地可以制备vK@100为12-30cSt的基础油,其VI高于125,并且在250℃下1小时后的蒸发损失为至多0.5wt%。这种新的基础油可以用作增塑剂或脱模工艺油。这种脱膜剂可以有利地用于食品包装应用中。
因为其低的倾点,按照本发明方法可以得到的基础油可以有利地用于电器用油和冷冻机油。特别是倾点低于-40℃的级分是非常适合的。相对于目前所应用的低倾点的环烷类基础油来说,由于按照本发明得到的基础油具有较高的抗氧化性,因而对这种用途更有利。
vK@100范围为4-25cSt,优选为6-9cSt的药用白油可以应用上述方法所得到的基础油进行混合。UV光谱已经表明这些基础油具有很好的潜能来满足US Food and Drug AdministrationFDA§178.3620 b和FDA§178.3620c的要求。
工艺用油以及更具体的切削油优选以这些基础油为基础,这是因为对配制工艺用油来说需要更少的添加剂。因为工艺用油经常与操作机器的人员的皮肤接触,因此在这些应用中应尽可能避免应用添加剂,其中所述机器如应用工艺用油的切削机。当工艺用油与操作员的皮肤接触时,所述添加剂可能对皮肤有刺激。
所述基础油也可以有利地用于透平或液压液体。通过与一些补充的抗氧化剂组合应用本发明方法可得到的基础油,可以达到这种用途所需要高度抑制的氧化稳定性。优选的抗氧化剂为胺类(aminic)或受阻酚类抗氧化剂。
由上述方法可得到的其它基础油包括适用于自动输送流体(ATF)的基础油。优选应用已通过催化脱蜡进行了步骤(c)而得到的倾点低于-40℃的低倾点基础油。vK@100为约4cSt的基础油可以任选与vK@100为约2cSt的级分进行混合,从而得到适用于ATF的基础油。运动粘度为约2-3cSt的低粘度基础油可以适当通过催化脱蜡适当的粗柴油馏分得到,其中所述粗柴油馏分如在步骤(b)中的大气压和/或真空精馏中得到的。自动输送流体将包括上述基础油,优选为vK@100为3-6cSt的基础油,以及一种或多种性能添加剂。这种性能添加剂的例子为耐磨剂、抗氧化剂、无灰分散剂、倾点抑制剂、消泡剂、摩擦调节剂、防腐剂和粘度调节剂。
由本方法得到的vK@100值为2-9cSt的基础油也适合用于汽车发动机油。特别是具有非常低的倾点适当地低于-40℃的基础油已经发现非常适合用于润滑油配制品,如按照SAE J-300粘度分类中的OW-xx规格的高性能汽油机机油,其中xx为20、30、40、50、60。已经发现这些高等级的润滑油配制品可以利用通过本发明方法得到的基础油来制备。其它汽车发动机油应用为5W-xx和10W-xx配制品,其中xx如上面所述。汽车发动机油配制品适当地包括一种或多种上述的基础油和一种或多种添加剂。可以形成部分组成的添加剂种类的例子有无灰分散剂、优选为过碱性类型的清洁剂、粘度调节聚合物、优选为二烷基二硫代磷酸锌类(ZDTP)的极压/耐磨添加剂、优选为受阻酚或胺(aminic)类的抗氧化剂、倾点抑制剂、乳化剂、脱乳剂、防腐剂、防锈剂、防污添加剂和/或摩擦调节剂。这些添加剂的具体例子例如在Kirk-Othmer Encyclopedia of Chemical Technology,第3版,第14卷,第477-526页中进行了描述。
食品可用白油也可以适当地以本方法所获得的基础油级分为基础。这些基础油非常适合于这种应用,这是因为在这些基础油中不含或含有非常低含量的不饱和环状分子。
润滑脂也可以以这些基础油为基础,因为与应用常规的高粘度指数的基础油时相比,为了达到相同的所希望的润滑脂粘度规格,其似乎可以包括更多的皂类增稠剂。包括更多的增稠剂是有利的,这是因为其可以造成润滑脂具有较高的高温机械稳定性。因此应用通过本方法得到的基础油,已经发现有可能配制具有低倾点及改进的高温机械稳定性的润滑脂。这些润滑脂进一步具有改进的抑制氧化稳定性。
下面将通过下列非限定性实施例描述本发明。
实施例1
向加氢裂化步骤(步骤(a))中连续进料应用WO-A-9934917中实施例III的催化剂在实施例VII中得到的费-托产品的C5-C750℃+馏分。所述进料中含有约60wt%的C30 +产品。C60 +/C30 +比为0.55。在加氢裂化步骤中使所述馏分与EP-A-532118的实施例1中的加氢裂化催化剂接触。在真空条件下连续精馏步骤(a)的流出物,从而得到轻组分、燃料和沸点为370℃及更高的残余物“R”。基于加氢裂化步骤的新鲜进料的粗柴油馏分的产率为43wt%。这样得到的粗柴油的特性在表3中给出。
残余物“R”的主要部分循环回到步骤(a),而剩余部分被送至催化脱蜡步骤(c)。在加氢裂化步骤(a)中的条件为:新鲜进料的重量小时空速(WHSV)为0.8kg/l.h,循环原料的WHSV为0.25kg/l.h,氢气流量=1000Nl/kg,总压力=40bar,并且反应器温度为335℃。
在脱蜡步骤中,上述沸点为370℃至高于750℃的馏分与WO-A-0029511的实施例9中所描述的含有0.7wt%Pt和30wt%ZSM-5的脱铝的粘结二氧化硅的ZSM-5催化剂接触。脱蜡条件为40bar氢,WHSV=1kg/l.h,以及温度为355℃。
脱蜡油被精馏为三个基础油馏分,其沸点范围分别为305-410℃(基于脱蜡步骤的进料的产率为13.4wt%)、410-460℃(基于脱蜡步骤的进料的产率为13.6wt%)和沸点超过510℃的馏分(基于脱蜡步骤的进料的产率为41.2wt%)。
更为详细地分析了沸点范围为410-460℃的基础油馏分和沸点范围为305-410℃的基础油馏分(参见表1)。从表1可以看出,得到的基础油符合API第III组规格。
表1
级分3 | 级分4 | |
在20℃时的密度 | 805.5 | 814.5 |
倾点(℃) | -54 | -48 |
在40℃时的运动粘度(cSt) | 9.05.4 | 17.99 |
在100℃时的运动粘度(cSt) | 3.0 | 4.011 |
VI | 103 | 122 |
硫含量(%w) | <0.001 | <0.001 |
饱和物(%w) | >95 |
实施例2
重复实施例1,只是脱蜡温度为365℃。脱蜡油被精馏为三个基础油馏分,其沸点范围分别为305-420℃(基于脱蜡步骤的进料的产率为16.1wt%)、420-510℃(基于脱蜡步骤的进料的产率为16.1wt%)和沸点超过510℃的馏分(基于脱蜡步骤的进料的产率为27.9wt%)。更为详细地分析了沸点范围为420-510℃的基础油馏分和更重的馏分(参见表2)。
表2
级分5 | 重级分 | |
在20℃时的密度 | 818.5 | 837.0 |
倾点(℃) | -59 | +9 |
在40℃时的运动粘度(cSt) | 24.5 | |
在100℃时的运动粘度(cSt) | 4.9 | 22.92 |
VI | 128 | 178 |
硫含量(%w) | <0.001 | <0.001 |
饱和物(%w) | >95 |
实施例3-4
重复实施例1,只是改变了步骤(a)中的温度(参见表3)。进一步分析了粗柴油馏分(参见表3)。分别按ASTM D2500、ASTM D97和IP309-96确定浊点、倾点和CFPP。通过气相色谱确定C5 +、C30 +和C60 +馏分。
比较实验A和B
由Fischer Tropsch材料开始重复实施例1(实验A),所述材料按照EP-A-426223所述用钴/氧化锆/二氧化硅催化剂来制备。C5 +馏分中含有约30wt%C30 +产品,C60 +/C30 +比为0.19。按实验A进行实验B,只是步骤(a)中的反应温度不同(参见表3)。在表3中总结了粗柴油馏分的特性。
表3
实施例 | 3 | 1 | 4 | A | B |
温度 | 330 | 335 | 340 | 330 | 335 |
浊点 | -13 | -20 | <-24 | +1 | -2 |
CFPP | -14 | -21 | -28 | 0 | -5 |
倾点 | -18 | <-24 | <-24 | 0 | -6 |
正化合物(wt%) | 27.6 | 21.3 | 19.9 | 50.4 | 41.2 |
异化合物(wt%) | 72.4 | 78.7 | 80.1 | 49.6 | 58.8 |
单-甲基 | 37.3 | 39.5 | 39.5 | 29.2 | 32.2 |
二-甲基 | 21.7 | 25.5 | 26.7 | 13.9 | 18.1 |
其它 | 13.4 | 13.8 | 14.1 | 6.4 | 8.5 |
密度(kg/l) | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 |
十六烷(D976m) | 78 | 77 | 76 | 80 | 78 |
十六烷(D4737m) | 87 | 85 | 86 | 90 | 85 |
T95 | 363 | 360 | 358 | - | - |
Claims (13)
1.一种制备两种或多种润滑基础油级分和粗柴油的方法,所述方法通过
(a)加氢裂化/加氢异构化费-托产品,其中在费-托产品中具有至少60个或更多碳原子的化合物与具有至少30个碳原子的化合物之间的重量比为至少0.2,并且其中在费-托产品中至少有30wt%的化合物具有至少30个碳原子,
(b)将步骤(a)的产品分离成一种或多种粗柴油馏分和一种基础油前体馏分,
(c)对步骤(b)中得到的基础油前体馏分进行倾点降低步骤,和
(d)分离步骤(c)的流出物为两个或多个基础油级分。
2.权利要求1的方法,其中在费-托产品中至少有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,其中在费-托产品中具有至少60个或更多碳原子的化合物与具有至少30个碳原子的化合物之间的重量比为至少0.4。
4.权利要求1-3任一项的方法,其中步骤(a)的转化率为25-70wt%。
5.权利要求1-4任一项的方法,其中基础油前体馏分的初始沸点为330-400℃。
6.权利要求1-5任一项的方法,其中通过溶剂脱蜡法进行步骤(c)。
7.权利要求1-5任一项的方法,其中通过催化脱蜡法进行步骤(c)。
8.权利要求7的方法,其中催化脱蜡催化剂包括孔径为0.35-0.8nm的沸石、第VIII族金属和粘结剂。
9.权利要求8的方法,其中所述粘结剂为基本不含氧化铝的低酸度耐熔氧化物粘结剂,并且其中所述催化剂通过使沸石的挤出物及粘结剂与氟硅酸盐的水溶液接触而得到。
10.权利要求9的方法,其中步骤(c)在温度为275-375℃、压力为40-70bar下进行,从而得到倾点低于-60℃至最高-10℃的基础油。
11.在100℃时运动粘度为12-30cSt的基础油,其粘度指数高于125,并且在250℃下1小时后其蒸发损失为至多0.5wt%。
12.权利要求11的基础油用作增塑剂的用途。
13.权利要求11的基础油用作脱模处理油的用途。
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