CN1703496A - 制备具有高ⅵ基础料的方法 - Google Patents

制备具有高ⅵ基础料的方法 Download PDF

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CN1703496A
CN1703496A CNA2003801010852A CN200380101085A CN1703496A CN 1703496 A CN1703496 A CN 1703496A CN A2003801010852 A CNA2003801010852 A CN A2003801010852A CN 200380101085 A CN200380101085 A CN 200380101085A CN 1703496 A CN1703496 A CN 1703496A
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I·A·科迪
W·J·墨菲
S·S·汉茨尔
D·W·拉金
J·E·小加拉赫
金珍玊
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ExxonMobil Technology and Engineering Co
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Abstract

一种制备高VI润滑油基础料的方法，包括加氢处理、加氢脱蜡和可选择地加氢精制。加氢处理步骤的条件使得转化成343℃以下的量基础料小于5wt％并且较进料VI的VI增加值小于4。加氢脱蜡使用低α催化剂并且加氢精制采用基于M41S类的催化剂实现。

Description

制备具有高VI基础料的方法
发明领域
本发明涉及一种从含蜡进料制备具有高粘度指数(VI)的润滑油基础料的方法。更特别地，对含蜡进料进行温和条件下的加氢处理、催化加氢脱蜡和加氢精制。
发明背景
曾经，用于例如汽车发动机油应用的润滑油制品采用添加剂以改进用于制备成品的基础料的特定性能。随着对环境关注的增加，对基础料本身的性能要求增加。美国石油协会(API)对II类基础料的要求包括：饱和物含量至少为90％、硫含量为0.03wt％或更少及粘度指数(VI)为80～120。除了VI至少为120之外，对III类基础料的要求与对II类基础料的要求相同。
用于制备基础料的常规技术例如加氢裂化或溶剂萃取要求严格的操作条件例如高压和高温或者高的溶剂∶油料比以及高萃取温度，以达到所述较高的基础料质量。任何一种替换方案涉及到昂贵的操作条件和低产率。
已经将加氢裂化与作为预备步骤的加氢处理结合。然而，由于向通常伴随加氢裂化过程的馏出物的转化，这种结合因而也会导致降低的润滑油产率。
希望有一种通过最大限度地减少向低沸点馏出物的转化而以高产率制备III类基础料并且同时制得具有优异低温性能、高VI和高稳定性的制品的经济方法。
发明概述
本发明涉及一种制备VI至少约135的润滑油基础料的方法，其包括：
(1)在有效的加氢处理条件下，采用加氢处理催化剂将蜡含量基于进料为至少约60wt％的润滑油进料加氢处理，以使得小于5wt％的进料转化成650°F(343℃)以下的制品，从而制得较进料VI的VI增加值小于4的加氢处理进料；
(2)将所述加氢处理进料气提以从液体制品中分离出气体；和
(3)在催化有效的加氢脱蜡条件下采用脱蜡催化剂将所述液体制品加氢脱蜡，所述脱蜡催化剂是ZSM-48、ZSM-57、ZSM-23、ZSM-22、ZSM-35、镁碱沸石、ECR-42、ITQ-13、MCM-71、MCM-68、β沸石、氟化氧化铝、氧化硅-氧化铝或氟化氧化硅-氧化铝中的至少一种，其中该脱蜡催化剂含有至少一种9族或10族贵金属。
另一个实施方案涉及一种制备VI至少约125的润滑油基础料的方法，其包括：
(1)在有效的加氢处理条件下，采用加氢处理催化剂将蜡含量基于进料为至少约50wt％的润滑油进料加氢处理，以使得小于5wt％的进料转化成650°F(343℃)以下的制品，从而制得较进料VI的VI增加值小于4的加氢处理进料；
(2)将所述加氢处理进料气提以从液体制品中分离出气体；
(3)在催化有效的加氢脱蜡条件下采用脱蜡催化剂将所述液体制品加氢脱蜡，所述脱蜡催化剂是ZSM-22、ZSM-23、ZSM-35、镁碱沸石、ZSM-48、ZSM-57、ECR-42、ITQ-13、MCM-68、MCM-71、β沸石、氟化氧化铝、氧化硅-氧化铝或氟化氧化硅-氧化铝中的至少一种，其中该脱蜡催化剂含有至少一种9族或10族贵金属；和
(4)在加氢精制条件下采用源自M41S类的中孔加氢精制催化剂将来自步骤(3)的制品加氢精制。
另一个实施方案涉及一种制备VI至少约135的润滑油基础料的方法，其包括：
(1)在有效的加氢处理条件下，采用加氢处理催化剂将蜡含量基于进料为至少约60wt％的润滑油进料加氢处理，以使得小于5wt％的进料转化成650°F(343℃)以下的制品，从而制得较进料VI的VI增加值小于4的加氢处理进料；
(2)将所述加氢处理进料气提以从液体制品中分离出气体；
(3)在催化有效的加氢脱蜡条件下采用ZSM-48脱蜡催化剂将所述液体制品加氢脱蜡，其中该脱蜡催化剂含有至少一种9族或10族贵金属；和
(4)在加氢精制条件下采用MCM-41将来自步骤(3)的制品加氢精制。
根据本发明的基础料满足III类基础料的要求并且可以以高产率制备并同时具有优异的性能例如高VI和低倾点。
附图简述
该图是本方法的示意性流程图。
发明详述
用于本发明方法的进料是在润滑油范围内沸腾的含蜡进料，由ASTMD 86或ASTM 2887测得其通常具有10％的蒸馏点大于650°F(343℃)，并且源自矿物来源或合成来源。该进料的蜡含量基于进料为至少约50wt％，并且可以高达100wt％的蜡。可以通过核磁共振光谱法(ASTMD5292)、相关ndM方法(ASTM D3238)或者溶剂方法(ASTM D3235)测定进料的蜡含量。该含蜡进料可以源自许多来源例如溶剂精制过程的油如萃余液、部分溶剂脱蜡油、脱沥青油、蒸馏物、真空瓦斯油、焦化瓦斯油、疏松石蜡、脚子油等以及费-托蜡。优选的进料是疏松石蜡和费-托蜡。疏松石蜡通常源自通过溶剂或丙烷脱蜡的烃进料。疏松石蜡含有一些残油并且通常是去油的。脚子油源自去油的疏松石蜡。费-托蜡通过费-托合成方法制备。
进料可以具有高含量的氮-和硫-污染物。在本方法中可以处理含有基于进料至多0.2wt％氮和至多3.0wt％硫的进料。蜡含量高的进料通常具有高达200或更高的高粘度指数。可以分别通过标准ASTM方法D5453和D4629测量硫和氮含量。
对于源自溶剂萃取的进料而言，将来自常压蒸馏的高沸点石油馏分供入真空蒸馏单元，并且将来自该单元的蒸馏馏分进行溶剂萃取。可以将来自真空蒸馏的残留物脱沥青。溶剂萃取工艺选择性地将所述芳类组分溶解在萃取相中并同时将更多的石蜡组分留在萃余相中。环烷烃被分布在萃取相和萃余相之间。用于溶剂萃取的典型溶剂包括苯酚、糠醛和N-甲基吡咯烷酮。通过控制溶剂与油料的比例、萃取温度以及将待萃取的馏出物与溶剂接触的方法，可以控制萃取相和萃余相之间的分离程度。
加氢处理
就加氢处理而言，催化剂是对加氢处理有效的那些，例如含有6族金属(基于具有1-18族的IUPAC元素周期表)、8-10族金属和其混合物的催化剂。优选的金属包括镍、钨、钼、钴和其混合物。这些金属或金属混合物通常作为氧化物或硫化物存在于耐热金属氧化物载体上。所述金属混合物也可以以本体金属催化剂存在，其中金属的量基于催化剂为30wt％或更大。合适的金属氧化物载体包括例如以下氧化物：氧化硅、氧化铝、氧化硅-氧化铝或二氧化钛，优选氧化铝。优选的氧化铝是多孔的氧化铝例如γ-或η-氧化铝。单个金属或者金属混合物的量基于催化剂为约0.5～35wt％。在优选的9-10族金属与6族金属的混合物情况下，9-10族金属存在的量基于催化剂为0.5～5wt％，6族金属存在的量为5～30wt％。可以通过原子吸收光谱法、电感耦合等离子体-原子发射光谱法或者由ASTM规定的针对各个金属的其他方法测定金属量。
可以通过加入促进剂和/或掺杂剂或者通过控制金属氧化物载体的性质(例如通过控制加入氧化硅-氧化铝载体中的氧化硅的量)而控制金属氧化物载体的酸性。促进剂和/或掺杂剂的实例包括卤素尤其是氟、磷、硼、氧化钇、稀土氧化物和氧化镁。促进剂例如卤素通常可提高金属氧化物载体的酸性，而适度碱性的掺杂剂例如氧化钇或氧化镁往往会降低所述载体的酸性。
加氢处理条件包括：150～400℃、优选200～350℃的温度；1480～20786kPa(200～3000psig)、优选2859～13891kPa(400～2000psig)的氢气分压；0.1～10液体时空速率(LHSV)、优选0.1～5LHSV的空速；和89～1780m3/m3(500～10000scf/B)、优选178～890m3/m3的氢气与进料的比例。
加氢处理可减少含氮和含硫污染物的量至不会在后续脱蜡步骤中不可接受地影响脱蜡催化剂的水平。同样，可能会存在某些多核芳类物种，其将会通过所述温和的加氢处理步骤。如果存在，可以在后续的加氢精制步骤中除去这些污染物。
在加氢处理期间，小于5wt％、优选小于3wt％、更优选小于2wt％的进料被转化成650°F(343℃)以下的制品，以制得较进料VI的VI增加值小于4、优选小于3、更优选小于2的加氢处理进料。所述进料的高蜡含量会导致在加氢处理步骤期间最小的VI增加值。
可以将所述加氢处理进料直接供至脱蜡步骤或者优选地气提以在脱蜡之前除去气体污染物例如硫化氢和氨气。可以通过常规装置例如闪蒸罐或分馏器进行气提。
脱蜡催化剂
脱蜡催化剂可以是结晶的或者无定形的。结晶材料是含有至少一个10或12元环孔道的分子筛，并且可以基于铝硅酸盐(沸石)或者基于硅铝磷酸盐(SAPO)。用于氧化处理的沸石可以含有至少一个10或12元孔道。这种沸石的实例包括ZSM-22、ZSM-23、ZSM-35、ZSM-48、ZSM-57、镁碱沸石、ITQ-13、MCM-68和MCM-71。含有至少一个10元环孔道的铝磷酸盐的实例包括ECR-42。含有12环孔道的分子筛的实例包括β-沸石和MCM-68。在美国专利号5,246,566、5,282,958、4,975,177、4,397,827、4,585,747、5,075,269和4,440,871中描述了分子筛。在美国专利No.6,310,265中描述了MCM-68。在PCT公开申请WO0242207和WO0078677中描述了MCM-71和ITQ-13。在US6,303,534中公开了ECR-42。优选的催化剂包括ZSM-48、ZSM-22和ZSM-23。尤其优选ZSM-48。所述分子筛优选为氢型。还原作用可以在脱蜡步骤本身期间原位发生或者可以在另外的容器中非原位(ex situ)发生。
无定形脱蜡催化剂包括氧化铝、氟化氧化铝、氧化硅-氧化铝、氟化氧化硅-氧化铝和掺杂3族金属的氧化硅-氧化铝。这些催化剂描述于例如美国专利No.4,900,707和6,383,366中。
脱蜡催化剂是双官能的，即它们加载有金属加氢组分，该组分为至少一种6族金属、至少一种8-10族金属或其混合物。优选的金属是9-10族金属。尤其优选的是9-10族贵金属例如Pt、Pd或其混合物(基于具有1-18族的IUPAC元素周期表)。这些金属的加载比例基于催化剂为0.1～30wt％。在例如美国专利No.6,294,077中描述了催化剂的制备方法和金属加载方法，并且包括例如使用可分解的金属盐的离子交换和浸渍。金属分散技术和催化剂颗粒尺寸控制技术在美国专利No.5,282,958中作了描述。优选具有小颗粒尺寸和优良分散金属的催化剂。
所述分子筛通常与耐高温的粘结剂材料复合，其可以在脱蜡条件下使用以形成成品脱蜡催化剂，或者可以是无粘结剂的(自粘结)。所述粘结剂材料通常是无机氧化物例如氧化硅、氧化铝、氧化硅-氧化铝、氧化硅与其他金属氧化物例如二氧化钛、氧化镁、氧化钍、氧化锆等的二元组合物以及这些氧化物的三元组合物例如氧化硅-氧化铝-氧化钍和氧化硅-氧化铝-氧化镁。成品脱蜡催化剂中分子筛的量基于催化剂为的10～100wt％，优选35～100wt％。这种催化剂可以通过例如喷雾干燥、挤出等方法形成。所述脱蜡催化剂可以以硫化或未硫化的形式使用，优选以硫化形式使用。
脱蜡条件包括：250～400℃、优选275～350℃的温度；791～20786kPa(100～3000psig)、优选1480～17339kPa(200～2500psig)的压力；0.1～10hr-1、优选0.1～5hr-1的液体时空速率和45～1780m3/m3(250～10000scf/B)、优选89～890m3/m3(500～5000scf/B)的氢气处理气体速率。
加氢精制
在不进行分离的情况下将至少部分来自脱蜡工艺的制品直接供至加氢精制步骤中。优选将由脱蜡工艺得到的制品加氢精制以将制品质量调节到所希望的标准。加氢精制是旨在饱和任何润滑油范围的烯烃和残留芳类并除去任何残留的杂原子和有色体的温和加氢处理形式。后脱蜡加氢精制通常与所述脱蜡步骤级联进行。通常，在约150℃～350℃、优选180℃～250℃的温度下进行所述加氢精制。总压力通常为2859～20786kPa(约400～3000psig)。液体时空速率通常为0.1～5LHSV(hr-1)、优选0.5～3hr-1，氢气处理气体速率为44.5～1780m3/m3(250～10,000scf/B)。
加氢精制催化剂是含有6族金属(基于具有1-18族的IUPAC元素周期表)、8-10族金属和其混合物的那些。优选的金属包括至少一种具有强加氢作用的贵金属，尤其是铂、钯和其混合物。所述金属混合物也可以以本体金属催化剂存在，其中金属的量基于催化剂为30wt％或更大。合适的金属氧化物载体包括弱酸性氧化物例如氧化硅、氧化铝、氧化硅-氧化铝或二氧化钛，优选氧化铝。用于饱和芳类的优选加氢精制催化剂包含至少一种具有相对强加氢作用的位于多孔载体上的金属。典型的载体材料包括无定形或结晶的氧化物材料例如氧化铝、氧化硅和氧化硅-氧化铝。对于非-贵金属而言，所述催化剂的金属含量通常高至约20wt％。贵金属存在的量通常不大于约1wt％。
加氢精制催化剂优选为属于M41S类或系列催化剂的中孔材料。M41S系列催化剂是具有高氧化硅含量的中孔材料，其制备方法进一步描述于J.Amer.Chem.Soc.，1992，114，10834中。实例包括MCM-41、MCM-48和MCM-50。中孔是指催化剂的孔径为15～100。这类的优选对象是MCM-41，制备方法描述于美国专利No.5,098,684。MCM-41是具有六角形排列的均匀尺寸孔的无机多孔非层状相。MCM-41的物理结构像一束麦杆，其中麦杆的开口(所述孔的孔径)为15～100埃。MCM-48是立方对称的并且描述于例如美国专利No.5,198,203中，而MCM-50具有层状结构。MCM-41可以制备具有在中孔范围内不同尺寸的孔开口。所述中孔材料可以具有金属加氢组分，其为8族、9族或10族金属的至少一种。优选贵金属，尤其是10族贵金属，最优选Pt、Pd或其混合物。
加氢精制通常在约150℃～350℃、优选180℃～250℃的温度下进行。总压力通常为2859～20786kPa(约400～3000psig)。液体时空速率通常为0.1～5LHSV(hr-1)、优选0.5～3hr-1，氢气处理气体流速为44.5～1780m3/m3(250～10,000scf/B)。
得自根据本发明方法的产品具有非常高的粘度指数并且可以由含蜡进料以高产率制得。因此，可以获得具有VI为145或更大以及优异低温性能的润滑油基料。
现在参考附图，含蜡原料例如疏松石蜡通过管线10送入加氢处理单元14。氢气通过管线12加入加氢处理单元14。加氢处理装置14装有加氢处理催化剂床16。加氢处理原料通过管线18供入汽提器20并且轻质气体通过管线22移出。液体产品然后通过管线24从汽提器20送入加氢脱蜡单元28。附加氢气通过管线26加入。加氢脱蜡单元28装有加氢脱蜡催化剂床30。加氢脱蜡产品然后通过管线32送入装有加氢精制催化剂床36的加氢精制单元34。加氢精制产品然后通过管线38送入真空汽提器40。轻质产品通过管线42移出并且残留液体产品通过管线44送入真空蒸馏单元(未示出)。
通过以下实施例进一步说明本发明并不意味着作为限制的。
实施例
实施例1
该实施例说明了用硫化的加氢脱蜡催化剂处理干净的进料可以以优异的产率制得高质量的脱蜡油。该进料是在240℃的低剧烈条件下加氢处理的150N疏松石蜡，其性能在表1中给出。使用采用了重复性为0.5％的Houillon自动粘度计的标准ASTM测试(D445-94和D2270-91)测量粘度。通过标准ASTM测试(D97)测量倾点。分别可以通过标准ASTM方法D5453和D4629测量硫和氮的含量。产率和倾点的误差限度分别为±1和±3。
              表1
  100℃下的粘度，cSt   3.6
  氮，Wppm   0.4
  硫，Wppm   120
  蜡中的油，wt％   7.0
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表1的进料加氢处理：240℃、LHSV为0.7v/v/h、1000psig(6996kPa)、处理速率为1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的94.4wt％。加氢处理产品的性能在表2中给出。
             表2
  100℃下的粘度cSt   3.6
  氮，Wppm   0.1
  硫，Wppm   2
在以下条件下用非原位(ex sitw)化的ZSM-48催化剂将加氢处理产品进行加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。以35wt％氧化铝粘结的ZSM-48催化剂加载有0.6wt％Pt作为金属，并且在氮气中400ppm H2S至H2S临界点下对其进行非原位硫化。加氢脱蜡的结果在表3中给出。
                           表3
  平均反应器温度℃   329
  370℃+产率，基于供入加氢脱蜡装置(HDW)的进料，wt％   53.8
  370℃+产品性能
  100℃下的粘度(cSt)   3.3
  VI   136
  倾点(℃)   -21
使用含有Pt/Pd的MCM-41作为加氢精制催化剂将加氢脱蜡产品进行加氢精制。在以下条件下将加氢脱蜡产品进行加氢精制：200℃、LHSV为2.5v/v/h、1000psig H2(6996kPa)、2500scf/B H2(445m3/m3)。使用MCM-41催化剂的加氢精制可以将总的芳类物质减少至基本为0，而不会影响脱蜡产品的其他性能。这是由于该催化剂在低温下的高饱和活性。以这种方式将该实施例和后续实施例中的脱蜡产品加氢精制。
实施例2
该实施例说明了采用硫化的加氢脱蜡催化剂处理干净的进料可以以优异的产率制得高质量的脱蜡油。进料为150N疏松石蜡，其性能在表4中给出。在345℃的更加剧烈条件下将所述进料加氢处理。
              表4
  100℃下的粘度，cSt   3.6
  氮，Wppm   0.4
  硫，Wppm   120
  蜡中的油，wt％   7.0
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表4的进料加氢处理：345℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的93.2wt％。加氢处理产品的性能在表5中给出。
              表5
  100℃下的粘度，cSt   3.4
  氮，Wppm   0.1
  硫，Wppm   0
在以下条件下采用非原位硫化的ZSM-48催化剂将加氢处理产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。将ZSM-48催化剂(实施例1)在氮气中400ppm H2S至H2S临界点下非原位硫化。得自加氢脱蜡的产品性能在表6中给出。
                     表6
  平均反应器温度℃   329
  370℃+产率，基于供入HDW的进料，wt％   52.6
  370℃+产品性能
  100℃下的粘度(cSt)   3.3
  VI   134
  倾点(℃)   -26
实施例3
该实施例说明了在还原的加氢脱蜡催化剂上处理干净的进料可以以优异的产率制得高质量的脱蜡油。进料为150N疏松石蜡，其性能在表7中给出。
               表7
  100℃下的粘度，cSt   3.6
  氮，Wppm   0.4
  硫，Wppm   120
  蜡中的油，wt％   7.0
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表7的进料加氢处理：345℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的93.9wt％。加氢处理产品的性能在表8中给出。
               表8
  100℃下的粘度，cSt   3.4
  氮，Wppm   0.1
  硫，Wppm   0
在以下条件下采用还原的ZSM-48催化剂将加氢处理产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。加氢脱蜡的结果在表9中给出。
                            表9
  平均反应器温度℃   330   332
  370℃+产率，基于供入HDW的进料，wt％   64.9   61.8
  370℃+产品性能
  100℃下的粘度(cSt)   3.3   3.2
  VI   140   136
  倾点(℃)   -18   -23
实施例4
该实施例说明了在硫化的加氢脱蜡催化剂上处理干净的轻质进料可以以优异的产率制得高质量的脱蜡油。进料为具有较高油含量的150N疏松石蜡，其性能在表10中给出。
              表10
  100℃下的粘度，cSt   3.7
  氮，Wppm   2
  硫，Wppm   252
  蜡中的油，wt％   13.5
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表10的进料加氢处理：270℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的95.3wt％。加氢处理产品的性能在表11中给出。
              表11
  100℃下的粘度，cSt   3.7
  氮，Wppm   2
  硫，Wppm   0.5
在以下条件下采用非原位硫化的ZSM-48催化剂将加氢处理的产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。将ZSM-48催化剂(实施例1)在氮气中400ppm H2S至H2S临界点下非原位硫化。加氢脱蜡的结果在表12中给出。
                            表12
  平均反应器温度℃   329   327
  370℃+产率，基于供入HDW的进料，wt％   52.4   56.4
  370℃+产品性能
  在100℃下的粘度(cSt)   3.4   3.4
  VI   133   136
  倾点(℃)   -27   -20
实施例5
该实施例说明了在硫化的催化剂上处理干净的进料可以以优异的产率制得高质量的脱蜡油。进料为600N疏松石蜡，其性能在表13中给出。
              表13
  100℃下的粘度，cSt   8.0
  氮，Wppm   14
  硫，Wppm   912
  蜡中的油，wt％   16.5
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表13的进料加氢处理：317℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的97.3wt％。加氢处理产品的性能在表14中给出。
             表14
  100℃下的粘度，cSt   7.5
  氮，Wppm   3
  硫，Wppm   1
在以下条件下采用非原位硫化的ZSM-48催化剂将加氢处理产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。将ZSM-48催化剂(实施例1)在氮气中400ppm H2S至H2S临界点下非原位硫化。加氢脱蜡的结果在表15中给出。
                     表15
  平均反应器温度℃   329
  370℃+产率，基于供入HDW的进料，wt％   61.9
  370℃+产品性能
  100℃下的粘度(cSt)   6.5
  VI   145
  倾点(℃)   -17
实施例6
该实施例说明了在较高的加氢处理温度下处理干净的进料可以以优异的产率制得高质量的脱蜡油。进料为600N疏松石蜡，其性能在表16中给出。
              表16
  100℃下的粘度，cSt   8.0
  氮，Wppm   14
  硫，Wppm   912
  蜡中的油，wt％   16.5
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表16的进料加氢处理：340℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的94.6wt％。加氢处理产品的性能在表17中给出。
             表17
  100℃下的粘度，cSt   7.2
  氮，Wppm   5
  硫，Wppm   1
在以下条件下采用非原位硫化的ZSM-48催化剂将加氢处理产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。将ZSM-48催化剂(实施例1)在氮气中400ppm H2S至H2S临界点下非原位硫化。加氢脱蜡的结果在表18中给出。
                     表18
  平均反应器温度℃   329
  370℃+产率，基于供入HDW的进料，wt％   60.3
  370℃+产品性能
  100℃下的粘度(cSt)   6.3
  VI   147
  倾点(℃)   -21
实施例7
该实施例说明了在还原的加氢脱蜡催化剂下处理干净的进料可以以优异的产率制得高质量的脱蜡油。进料为600N疏松石蜡，其性能在表19中给出。
              表19
  100℃下的粘度，cSt   7.95
  氮，Wppm   14
  硫，Wppm   912
  蜡中的油，wt％   16.5
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表22的进料加氢处理：340℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的93.9wt％。加氢处理产品的性能在表20中给出。
              表20
  100℃下的粘度，cSt   7.2
  氮，Wppm   5
  硫，Wppm   1
在以下条件下采用还原的ZSM-48催化剂(35wt％铝/0.6wt％Pt)将加氢处理产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。加氢脱蜡的结果在表21中给出。
                    表21
  平均反应器温度℃   338
  370℃+产率，基于供入HDW的进料，wt％   60.4
  370℃+产品性能
  100℃下的粘度(cSt)   6.1
  VI   146
  倾点(℃)   -25
表21的结果说明可以由含蜡进料以高产率获得VI非常高的产品。
实施例8
该实施例说明了处理干净的、具有较高蜡中油含量的进料可以以优异的产率制得高质量的脱蜡油。进料为600N疏松石蜡，其性能在表22中给出。
             表22
  100℃下的粘度，cSt   8.2
  氮，Wppm   20
  硫，Wppm   1289
  蜡中的油，wt％   25.3
在以下加氢处理条件下采用Akzo Nobel KF848催化剂将表22的进料加氢处理：340℃、0.7v/v/h、1000psig(6996kPa)、1500scf/B H2(267m3/m3)。加氢处理产品的370℃+产率为进料的95.8wt％。加氢处理产品的性能在表23中给出。
              表23
  100℃下的粘度，cSt   7.4
  氮，Wppm   4
  硫，Wppm   1
在以下条件下采用非原位硫化的ZSM-48催化剂将加氢处理产品加氢脱蜡：1v/v/h、1000psig(6996kPa)、2500scf/B H2(445m3/m3)。ZSM-48催化剂(实施例1)在氮气中400ppm H2S至H2S临界点下非原位硫化。加氢脱蜡的结果在表24中给出。
                表24
  平均反应器温度℃   329
  370℃+产率，基于进料，wt％   61
  370℃+产品性能
  在100℃下的粘度(cSt)   6.8
  VI   142
  倾点(℃)   -22

Claims (13)

1.一种制备VI至少约135的润滑油基础料的方法，其包括：
(1)在有效的加氢处理条件下，采用加氢处理催化剂将蜡含量基于进料为至少约60wt％的润滑油进料加氢处理，以使得小于5wt％的进料转化成650°F(343℃)以下的制品，从而制得较进料VI的VI增加值小于4的加氢处理进料；
(2)将所述加氢处理进料气提以从液体制品中分离出气体；和
(3)在催化有效的加氢脱蜡条件下采用脱蜡催化剂将所述液体制品加氢脱蜡，所述脱蜡催化剂是ZSM-48、ZSM-57、ZSM-23、ZSM-22、ZSM-35、镁碱沸石、ECR-42、ITQ-13、MCM-71、MCM-68、Beta、氟化氧化铝、氧化硅-氧化铝或氟化氧化硅-氧化铝中的至少一种，其中该脱蜡催化剂含有至少一种9族或10族贵金属。
2.根据权利要求1的方法，其中脱蜡催化剂是ZSM-22、ZSM-23、ZSM-48或ZSM-57中的至少一种。
3.根据前述任一项权利要求的方法，其中所述加氢处理催化剂含有至少一种6族、9族或10族金属。
4.根据前述任一项权利要求的方法，其中所述加氢处理条件包括：150～400℃的温度、1480～20786kPa的压力、0.1～10hr-1的液体时空速率和89～1780m3/m3的氢气处理速率。
5.根据前述任一项权利要求的方法，其中所述脱蜡催化剂是ZSM-22、ZSM-23、ZSM-48或ZSM-57中的至少一种。
6.根据前述任一项权利要求的方法，其中所述脱蜡催化剂是ZSM-48。
7.根据前述任一项权利要求的方法，其中所述脱蜡催化剂含有Pt、Pd或其混合物。
8.根据前述任一项权利要求的方法，其中加氢脱蜡条件包括：250～400℃的温度、791～20786kPa的压力、0.1～10hr-1的液体时空速率和45～1780m3/m3的氢气处理速率。
9.根据前述任一项权利要求的方法，其中所述脱蜡催化剂是硫化的、还原的、或者硫化并还原的。
10.根据前述任一项权利要求的方法，其中在有效的加氢精制条件下将来自步骤(3)的加氢脱蜡液体制品加氢精制。
11.根据前述任一项权利要求的方法，其中所述加氢精制包括含有至少一种6族、9族或10族金属的加氢精制催化剂。
12.根据前述任一项权利要求的方法，其中所述加氢精制包括其为源自M41S类的中孔催化剂的加氢精制催化剂。
13.根据前述任一项权利要求的方法，其中所述加氢精制催化剂含有至少一种贵金属。
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CN102066530B (zh) * 2008-06-17 2013-11-06 Sk润滑油株式会社 用于制造高品质环烷基油的方法
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US7282137B2 (en) 2007-10-16
US20040108249A1 (en) 2004-06-10
EP1551942B1 (en) 2018-07-18
CA2501044A1 (en) 2004-04-22
CN100564491C (zh) 2009-12-02
CN100378202C (zh) 2008-04-02
CN1703497A (zh) 2005-11-30
WO2004033597A3 (en) 2004-05-27
JP4459057B2 (ja) 2010-04-28
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