CN1097083C - 合成喷气燃料和其生产方法 - Google Patents

合成喷气燃料和其生产方法 Download PDF

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CN1097083C
CN1097083C CN98802353A CN98802353A CN1097083C CN 1097083 C CN1097083 C CN 1097083C CN 98802353 A CN98802353 A CN 98802353A CN 98802353 A CN98802353 A CN 98802353A CN 1097083 C CN1097083 C CN 1097083C
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R·J·维敦布林克
P·J·伯洛维茨
B·R·库克
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Abstract

通过分离蜡为较重的馏分和较轻的馏分，由费-托合成蜡生产用做喷气燃料或喷气燃料的混合料的清洁馏分燃料；进一步分离该较轻的馏分和加氢异构化该较重的馏分和高于约475°F的较轻馏分部分。把该异构化的产物与较轻馏分的未处理的部分混合，得到高质量的清洁喷气燃料。

Description

合成喷气燃料和其生产方法
发明领域
本发明涉及一种具有很好的适合作为具有很好的润滑性能的喷气燃料或作为其混合料的馏分燃料以及涉及该喷气燃料的制备方法。更具体地说，本发明涉及由费-托合成蜡制备喷气燃料的方法。
发明背景
对不含硫、氮或芳烃的清洁馏分物流极大的需要是或者将来很可能是作为喷气燃料或作为混合的喷气燃料。具有较好的润滑性和稳定性的清洁馏分油是特别有价值的。一般的由石油得到的馏分油是不清洁的，一般它们含有显著量的硫、氮或芳烃。另外，为了生产具有足够稳定性的燃料所需要的苛刻的加氢处理常常会得到润滑性能很差的燃料。通过苛刻的加氢处理生产的这些石油衍生的清洁馏分油比未加氢处理的燃料具有明显高的费用。为了很好的操作燃料输送系统所需要的燃料润滑性可以通过使用通过鉴定的添加剂整套配方来加以改善。在公开的文献中已经公开了由费-托合成蜡生产清洁的、高十六烷值的馏分燃料，但是，所公开的生产这样的馏分燃料的方法也使得该馏分燃料缺少一种或多种重要的性能，例如润滑性。因此，所公开的费-托合成馏分油需要与其它不太合乎要求的油料混合或使用贵重的添加剂。这些较早的方案公开了加氢处理该总的费-托合成产物，包括整个的700°F-馏分。该加氢处理使得从该喷气燃料中完全除去了含氧化合物。
借助于本发明，保留了少量的含氧化合物，得到具有很好的润滑性能的产物。该产物本身可以用做喷气燃料或作为由其它的低级物料制备喷气燃料的混合料。
发明概述
按照本发明，优选的由费-托合成蜡和优选的用钴或钌催化剂，通过分离该蜡产物成为较重的馏分和较轻的馏分，可以生产具有按照Ball on Cylinder(BOCLE)试验所测定的润滑性能大约等于或好于好的润滑性的对照燃料的润滑性能的用作喷气燃料或用作喷气燃料的混合料的清洁的馏分燃料；通常的分离温度是例如约700°F。于是，该较重的馏分主要含有700°F+的馏分，该较轻的馏分主要含有700°F-的馏分。
通过进一步分离该较轻的馏分为至少两种其它的馏分：(i)其中之一含有C7-12伯醇，和(ii)另一种不含有这样的醇。馏分(ii)是550°F+的馏分，优选500°F+的馏分，更优选475°F+的馏分，还更优选正C14+馏分。在一般的加氢异构化的条件下，在双功能催化剂的存在下，把该较重的馏分(ii)的至少一部分，优选全部，进行加氢转化(例如加氢异构化)。作为费-托合成蜡(即由费-托合成反应得到的较重的700°F+的馏分)的加氢异构化反应，该馏分的加氢异构化可以分开进行或在同一个反应区进行，优选在同一个反应区进行。在任何情况下，例如一部分475°F+的物料转化为较低沸点的馏分，例如475°F-的物料。然后，把至少一部分，优选全部的由该物料加氢异构化得到的与喷气燃料的结冰相适应的物料与至少一部分，优选全部的馏分(i)混合，馏分(i)优选的是250-475°F的馏分，其更优选的特征是不存在任何的加氢处理，例如加氢异构化。本发明的喷气燃料或喷气燃料混合组分的沸点在喷气燃料的范围内，其可以含有沸点高于喷气燃料的沸点范围的烃物料，其含量使得这些附加的物料与喷气燃料的冰点规格即-47℃或更低相适应。这些所谓的相适应的物料的量取决于在加氢异构化区域转化的程度，而更多的异构化导致生成更多的该相适应的物料，即更高支链的物料。于是，该喷气燃料的范围通常是250-550°F，优选250-500°F，更优选250-475°F，其可以包括该相适应的物料，并且其具有下面所述的性质。
由分馏塔回收的该喷气燃料物质具有下表所示的性质：烷烃         至少95重％，优选至少95重％，更优选至少97重％，
         还更优选至少98重％异构/正构比  约0.3-3.0，优选0.7-2.0硫           ≤50ppm(重)，优选0氮           ≤50ppm(重)，优选≤20ppm(重)，更优选0不饱和物     ≤2.0(重)％，优选≤1.0(重)％，最优选≤0.05(重)％(烯烃和芳烃)含氧化合物   约0.005-少于约0.5重％的氧，无水基
该异构烷烃通常是单甲基支链的，因为该方法使用费-托合成蜡，所以该产物不含有环烷烃，例如没有环己烷。
在较轻馏分例如250-475°F的馏分中，所含的含氧化合物的基本含量是例如是≥95％，并且主要是例如≥95％的C6-C12末断直链醇。
附图的描述
图1是本发明的方法的示意图。
优选实施方案的介绍
参考附图可以更详细的介绍本发明。把在管线1中所含有的合适比例的合成气、氢气和一氧化碳加到费-托合成反应器2中，优选是浆液反应器，在管线3和4中分别回收700°F+和700°F-的产物。该较轻的馏分通过一个热分离器6，在管线8中回收475-700°F的馏分，同时在管线7中回收475°F-的馏分。然后把该475-700°F的馏分与管线3中的700°F+的物质再混合，并加入到加氢异构化反应器中，在其中，一般约50％的物质转化为700°F-的物质。该700°F-的物质通过冷却分离器9，由此在管线10中回收C4-气体。在管线11中回收C5-475°F的馏分，并且在管线12中与异构化反应器的产物混合。
管线12送到蒸馏塔，在其中分馏得到管线16的C4-250°F的石脑油物流、管线15的250-475°F的喷气燃料、管线18的475-700°F的柴油和700°F+的物质。该700°F+的物质可以循环回到加氢异构反应器5或用做制备高质量润滑油基础油。如果该异构化反应器5基本上转化所有的正C14+烷烃为异构烷烃，优选的是，从475°F向上调整管线15和18之间的距离。该切割点优选的是500°F，最优选550°F，只要喷气燃料的冰点保持在-47℃。
加氢异构化方法是众所周知的，下面的表列出了该步骤的某些宽范围的和优选的条件。
条件             宽范围               优选范围温度，°F             300-800              500-750总压力，psig          300-2500             500-1500氢气处理速度，SCF/B   500-5000             1500-4000其中，psig表示磅/英寸2(表压)，SCF/B表示标准立方英尺/桶。
实际上，虽然用于加氢处理(例如加氢异构化或选择性加氢裂化)的任何由金属加氢组分和酸性组分组成的双功能催化剂对于该步骤可能都是满意的，但是某些催化剂比另一些催化剂要好并且是优选的。例如，含有担载的VIII族贵金属(例如铂或钯)的催化剂与含有0.5-20重％的一种或多种VIII族非贵金属(例如镍、钴)的催化剂一样有用，含有VIII族非贵金属的催化剂也可以包括或不包括1.0-20重％的VI族金属(例如钼)。担载这些金属的载体可以是任何的耐热的氧化物或沸石或它们的混合物。优选的载体包括氧化硅、氧化铝、氧化硅-氧化铝、氧化硅-氧化铝磷酸盐、氧化钛、氧化锆、氧化钒和其它VIII族、IV族、VA族或VI氧化物，以及Y型分子筛，例如超稳Y分子筛。优选的载体包括氧化铝和氧化硅-氧化铝。
优选的催化剂的表面积约为200-500m2/gm，优选0.35-0.80ml/gm，其是由水吸附法测定的，和堆积密度约为0.5-1.0g/ml。
该催化剂包括VIII族非贵金属例如铁、镍，与IB族金属例如铜，一起担载在酸性载体上。该载体优选的是无定型氧化硅-氧化铝，其中氧化铝的存在量少于约50重％，优选5-30重％，更优选10-20重％。另外，该载体可以含有少量的例如20-30重％的粘接剂，例如氧化铝、氧化硅、IVA族金属氧化物和各种类型的粘土、氧化镁等，优选氧化铝。
在Ryland，Lloyd B.，Tamele，M.W.，andWilson，J.N.，Cracking Catalysts，Catalysis：Volume VII，Ed.Paul H.Emmett，Reinhold Publishing Corporation，New york，1960，pp.5-9中已经公开了无定型氧化硅-氧化铝微球的制备方法。
该催化剂的制备是：把金属从溶液中共沉淀到载体上，在100-150℃干燥，在200-550℃空气中焙烧。
该VIII族金属的存在量约为15重％或更少，优选1-12重％，而IB族金属的存在量通常较少，例如与VIII族金属的比例约为1∶2-1∶20。一般的催化剂表示如下：
        Ni，重％             2.5-3.5
        Cu，重％             0.25-0.35
        Al2O3-SiO2        65-75
        Al2O3(粘接剂)      25-30
        表面积               290-325m2/gm
        孔体积(Hg)           0.35-0.45mL/gm
        堆积密度             0.58-0.68g/mL
700°F+的馏分转化为700°F-的馏分约20-80％，优选20-70％，更优选约30-60％。在加氢异构化过程中，基本上所有的烯烃和含氧的物质都被加氢。另外，大多数的直链烷烃异构化或裂化，使得大大的改善了低温性能例如喷气燃料的冰点。
700°F-物流分离成为C5-475°F物流和475-700°F物流，如所述，475-700°F物流的加氢异构化使得改善产物的冰点。但是，另外在C5-475°F物流中的含氧化合物具有改善生成的喷气燃料的润滑性能的作用，当其用做混合料时，可以改善通常所生产的喷气燃料的润滑性能。
优选的费-托合成方法是使用非变换(即没有水气变换能力)催化剂，例如钴或钌或它们的混合物，优选钴，优选促进的钴催化剂的方法，该促进剂是锆或铼，优选铼。这样的催化剂是众所周知的，优选的催化剂公开在U.S.P.4,568,663和EP 0 266 898中。
费-托合成方法的产物主要是烷烃。钌催化剂主要生产沸点范围即C10-C20馏分的烷烃，而钴催化剂一般生产较重的烃，例如C20+的烃，钴是优选的费-托合成催化金属。
好的喷气燃料一般的具有高烟点、低冰点、好的润滑性、好的氧化稳定性和适合于喷气燃料的规格的物理性能。
本发明的产物本身就可以用做喷气燃料，或者与其它的不合乎要求的含有约同样的沸点范围的石油或含烃原料混合。为了明显的改善最终混合的喷气燃料产物，当其用做混合料时，本发明的产物可以使用比较少的量，例如10％或多于10％。虽然本发明的产物将改善几乎所有的喷气燃料产物，但是特别合乎要求的是把该产物与炼厂的低质量的喷气燃料物流，特别是具有高芳烃含量的那些喷气燃料物流混合。
通过使用费-托合成方法，回收的馏分油基本上不含有硫和氮。这些杂原子化合物是费-托合成催化剂的毒物，要从费-托合成方法的便宜的原料的含有甲烷的天然气中除去。在任何情况下，含有硫和氮的化合物在天然气中的浓度要尽可能的低。另外，该方法不生产芳烃，或按通常的操作实际上没有芳烃产生。因为所提出的生产烷烃的途径之一是通过烯烃中间产物，所以产生一些烯烃。然而烯烃的浓度通常相当低。
在费-托合成过程中，产生了包括醇和某些酸的含氧化合物，但是在至少一种公知的方法中含氧化合物和不饱和物是通过加氢处理从产物中完全除去的。见例如，the Shell Middle Distilate Process，Eiler，J.，Posthuma，S.A.，Sie，S.T.，Catalysis Letters，1990，7，153-270。
但是，我们已经发现，该少量的含氧化合物，优选醇，对喷气燃料提供特殊的润滑性。例如，下面将说明的那样，具有少量的含氧化合物的高烷烃喷气燃料具有按该BOCLE试验(ball on cylinderlubricity evaluator)所显示的优异的润滑性能。但是，当例如通过萃取、分子筛吸附、加氢处理等使得不存在该含氧化合物，在该试验的馏分中氧的含量到低于10ppm(无水基)时，其润滑性能相当差。
通过本发明所公开的加工方案，一部分较轻的700°F-的馏分，即250-475°F的馏分不进行任何的加氢处理。在该馏分不进行加氢处理的情况下，在该馏分中保留少量的含氧化合物，主要是直链醇，而在较重的馏分中的含氧化合物在加氢异构化步骤被除去。为了改善润滑性能，该有价值的含氧化合物是在未处理的250-475°F的馏分中的C7+，优选C7-C12的，更优选C9-C12的伯醇。加氢异构化也增加馏分燃料中的异构烷烃，使得该燃料满足冰点要求。
被认为是提高润滑性能的该氧化合物可以描述为具有键能大于烃的键能(对于各种化合物，这些键能的测定可以在标准的参考文献中找到)的氢键；这种差别越大，润滑性能的效果越好。该含氧化合物也具有疏水端和亲水端，以使燃料润湿。
虽然酸是含氧化合物，但是酸是腐蚀性的，其是在非转换的条件下在费-托合成的过程中以非常少的量产生的。相对于由直链醇所说明的优选单-含氧化合物，酸是二-含氧化合物。于是，二-或多-含氧化合物通常是不能由红外测定法检测的，并且是按氧计例如少于约15wppm氧。
对于本领域的技术人员来说，非转换费-托合成反应是公知的，其可以用条件来表征，即所形成的副产物CO2减少到最少。通过各种方法，包括下面的一种或多种方法可以达到这些条件：在比较低的CO分压下操作，即在氢与CO的比例至少约1.7/1，优选约1.7/1-2.5/1，更优选至少约1.9/1，在1.9/1-约2.3/1的范围内，所有带α的至少约0.88，优选至少约0.91；温度是约175-225℃，优选180-220℃；使用含有钴或钌的催化剂作为主要的费-托合成催化剂。
为了达到所要求的润滑性能，按无水基的氧计，所存在的含氧化合物的量是比较少的，即至少约0.01重％的氧(无水基)，优选0.01-0.5重％的氧(无水基)，更优选0.02-0.3重％的氧(无水基)。
下面将用实施例说明本发明，但是不是限制本发明。
在浆液费-托合成反应器中，把氢气和二氧化碳合成气(H2∶CO2为2.11-2.16)转化为重烷烃。该费-托合成反应所用的催化剂是前面所述的在U.S.P.4,568,663中所介绍的氧化钛担载的钴/铼催化剂。其反应条件是422-428℃，287-289psig，线速度是12-17.5厘米/秒。该费-托合成反应步骤的α是0.92。然后，把该烷烃费-托合成产物分离成三种不同标称沸点的物流，使用粗闪蒸分离。该三种大约沸点的馏分是：1)C5-500°F沸点范围的馏分，下面指定为F-T冷分离器液体；2)500-700°F沸点范围的馏分，下面指定为F-T热分离器液体；和3)700°F+沸点范围的馏分，下面指定为F-T反应器蜡。实施例1
把70重％的加氢异构化的F-T反应器蜡、16.8重％的加氢处理的F-T冷分离器液体和13.2重％的加氢处理的F-T热分离器液体混合并剧烈的搅拌混合。喷气燃料A是该混合物的250-475°F沸点范围的馏分，是蒸馏分离的，其是按如下的方法制备的：按U.S.P.5,292,989和U.S.P.5,378,348中所介绍的，在一次通过的固定床装置，使用钴和钼促进的无定型氧化硅-氧化铝催化剂制备该加氢异构化的F-T反应器蜡。加氢异构化的条件是708°F，750psig H2，2500 SCF/B H2和液时空速(LHSV)0.7-0.8。使用一次通过的固定床反应器，使用市场上买到的大体积的镍催化剂制备加氢处理的F-T冷和热分离器液体。加氢处理的条件是450°F，430psig H2，1000 SCF/B H2和0.3LHSV。燃料A是一般的完全加氢处理的钴得到的费-托合成喷气燃料的代表，其是本领域公知的。实施例2
把78重％的加氢异构化的F-T反应器蜡、12重％的未加氢处理的F-T冷分离器液体和10重％的加氢处理的F-T热分离器液体混合并混合均匀。喷气燃料B是该混合物的250-475°F沸点范围的馏分，是蒸馏分离的，其是按如下的方法制备的：按U.S.P.5,292,989和U.S.P.5,378,348中所介绍的，在一次通过的固定床装置，使用钴和钼促进的无定型氧化硅-氧化铝催化剂制备该加氢异构化的F-T反应器蜡。加氢异构化的条件是690°F，725 psig H2，2500 SCF/B H2和液时空速(LHSV)0.6-0.7。燃料B是本发明的代表例。实施例3
为了测定本发明的喷气燃料与目前市场上所用的工业喷气燃料的润滑性能，和其在与工业喷气燃料的混合物中的作用，用下面的燃料进行试验。燃料C是满足工业喷气燃料规格的市场上买到的U.S.喷气燃料，其是已经通过使其通过adapulgous粘土除去杂质而处理的。燃料D是40％燃料A(加氢处理的F-T喷气燃料)和60％燃料C(US工业喷气燃料)的混合物。燃料E是40％燃料B(本发明的喷气燃料)和60％燃料C(US工业喷气燃料)的混合物。实施例4
实施例1的燃料A与在本发明的燃料B中的样品化合物醇按如下混合：燃料F是在燃料A中加0.5重％的1-庚醇，燃料G是在燃料A中加0.5重％的1-十二烷醇，燃料H是在燃料A中加0.05重％的1-十六烷醇，燃料I是在燃料A中加0.2重％的1-十六烷醇，燃料J是在燃料A中加0.5重％的1-十六烷醇。实施例5
使用标准的Scuffing Load Ball on Cylinder LubricityEvaluation(BOCLE或SLBOCLE)，进一步按Lacey，P.I.“The U.S.Army Scutting Load Wear Test”，January 1，1994所介绍的来进行喷气燃料A-E的所有试验。该试验是以ASTM D 5001为基础。结果列于表2，按Lacey所述，是以对照燃料2的百分比，和以磨损负载的绝对克。
                      表1
喷气燃料A-E的Scuffing BOCLE结果。所列的结果是按上面所述，按绝对磨损负载和对照燃料2的百分比。喷气燃料            磨损负载                 ％对照燃料2A                      1300                       19％B                      2100                       34％C                      1600                       23％D                      1400                       21％E                      2100                       33％
完全加氢的喷气燃料A显示非常低的一般是所有烷烃喷气燃料的润滑性能。喷气燃料B，其含有以直链C5-C14伯醇的高含量的烷氧基化物，其显示明显优异的润滑性能。喷气燃料C，其是工业上得到的U.S.喷气燃料，其比燃料A显示稍微好的润滑性能，但是不等于本发明的燃料B。燃料D和E表示本发明的混合燃料B的结果。对于燃料D，低润滑性能的燃料A与燃料混合，按预期产生一种润滑性能在这两种组分之间的润滑性能，其比本发明的F-T燃料明显的差。通过把燃料B加到燃料C中，像是燃料E，把差的工业燃料的润滑性能改善到与燃料E相同的水平，即使燃料B仅是最终混合物的40％。这就说明通过把本发明的燃料与常规的喷气燃料和喷气燃料组分混合可以得到明显的改善。实施例7
附带的说明，通过把特殊的醇加到低润滑性能的燃料A中，显示醇对润滑性能的影响。所加的醇是一般的在本发明中所述的费-托合成方法的产物，其可以在燃料B中找到。
                        表2
燃料A和F-J的Scuffing BOCLE结果。所列的结果是按上面所述，按绝对磨损负载和对照燃料2的百分比。喷气燃料                磨损负载             ％对照燃料2A                          1300                   19％F                          2000                   33％G                          2000                   33％H                          2000                   32％I                          2300                   37％J                          2700                   44％实施例8
对于航空燃料，按ASTM D5001 BOCLE试验方法，试验实施例卜5的燃料。该试验测定对于实施例6和7所示的刮伤负载，在球上的磨损划痕(以毫米计)。该试验给出了燃料A、B、C、E、H和J的试验结果，其说明刮伤负载试验的结果类似于ASTM D5001 BOCLE试验的结果。
                      表3
燃料A、B、C、E、H和J的ASTM D5001 BOCLE试验的结果。所列的结果是按ASTM D5001所述的磨损划痕直径。
       喷气燃料                磨损划痕直径
         A                        0.57mm
         B                        0.54mm
         C                        0.66mm
         E                        0.53mm
           H                 0.57mm
           J                 0.54mm上述的结果表明，本发明的燃料B比工业喷气燃料C或加氢处理的费-托合成燃料A显示优异的性能。刮痕负载BOCLE试验发现，把润滑性能差的工业燃料C与燃料B混合，得到的燃料性能等于燃料B。加很少量的醇到燃料A中，在该试验中不能改善润滑性能，就象在刮痕负载试验(燃料H)的结果，但是在较高浓度的情况下性能得到改善(燃料J)。

Claims (11)

1.一种用做喷气燃料或喷气燃料的混合组分的物料，其包括由非转换费-托合成方法得到的121.1-287.8℃的馏分，该馏分含有：
至少95重％的异构/正构比为0.3-3.0的烷烃，
硫和氮都≤50ppm(重)，
小于1.0(重)％的不饱和物，和
0.01-少于0.5重％的氧，该氧主要是以直链C7-C12伯醇存在。
2.根据权利要求1的物料，其中该喷气燃料由121.1-287.8℃的馏分组成。
3.根据权利要求1的物料，其中该喷气燃料含有121.1-246.1℃的馏分。
4.根据权利要求1-3之一的物料，其中该醇是由费-托合成方法得到的。
5.一种生产喷气燃料的方法，其包括：(a)分离费-托合成方法得到的产物为较重的馏分和较轻的馏分；(b)进一步分离该较轻的馏分为至少两种馏分，(i)至少一种含有C7-C12伯醇和具有基本上不包括所有的正C14烷烃的终馏点的馏分和(ii)一种或多种其它馏分；(c)在加氢异构化条件下把至少一部分步骤(a)的较重的馏分加氢异构化并回收371.1℃-的馏分；(d)把至少一部分馏分(b)(i)与至少一部分在步骤(c)回收的371.1℃-的馏分混合。
6.根据权利要求5的方法，其中还加氢异构化至少一部分(b)(ii)馏分。
7.根据权利要求6的方法，其中还从步骤(d)的混合产物中回收沸点范围121.1-287.8℃的产物。
8.根据权利要求6的方法，其中还从步骤(d)的混合产物中回收沸点范围121.1-246.1℃的产物。
9.根据权利要求8的方法，其中回收的步骤(d)的产物含有0.01-0.5重％的氧，无水基。
10.根据权利要求6的方法，其中馏分(b)(i)基本上含有所有的C7-C12伯醇。
11.根据权利要求5的方法，其特征在于馏分(b)(ii)是475°F-的馏分。
CN98802353A 1997-02-07 1998-01-27 合成喷气燃料和其生产方法 Expired - Lifetime CN1097083C (zh)

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