CN100384965C - 制备费-托产品的方法 - Google Patents
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Abstract
通过进行以下步骤制备蜡状提余液产品的方法:(a)使费-托衍生产品经历加氢转化步骤,在该费-托衍生产品中,沸点高于540℃的化合物与沸点在370℃~540℃之间的化合物的重量比大于2;和(b)分馏步骤(a)的流出液,以获得沸点在燃料范围内的产品和沸点在350~600℃之间的蜡状提余液产品。
Description
本发明涉及从费-托合成产品制备高产率的基础油或中间蜡状提余液产品的方法。
此类方法可由WO-A-9941332,US-A-6080301,EP-A-0668342,US-A-6179994或WO-A-02070629中获知。这些方法全都包括费-托合成产品的某种加氢异构化,以及之后使所述加氢异构化得到的较高沸点馏分脱蜡的步骤。
例如,WO-A-02070629描述了一种方法,其中,费-托合成产品的C5+馏分先在无定形二氧化硅-氧化铝担载的铂催化剂存在下,经历加氢裂化/加氢异构化步骤。这一转化步骤的流出液被分离成为中间馏分油产品、基础油前体馏分(也称为蜡状提余液产品)和较高沸点馏分。基础油前体馏分在铂-ZSM-5类催化剂存在下催化脱蜡,重质馏分再循环回到加氢裂化/加氢异构化步骤。
虽然这样的方法能产生品质优异的基础油,但仍有改进空间。尤其是中间蜡状提余液产品的质量和产率可得以改善。本发明的目的在于(a)使费-托衍生产品经历加氢转化步骤,该费-托衍生产品中沸点高于540℃的化合物与沸点在370℃~540℃之间的化合物的重量比大于2;和(b)分馏步骤(a)的流出液,以获得沸点在燃料范围内的产品,和沸点在350~600℃之间的蜡状提余液产品。
本申请人发现,通过处理这样的相对重质费-托衍生产品,能获得由步骤(a)原料生产蜡状提余液产品的更高产率,而且其中改善了蜡状提余液的质量。已经发现,诸如冷流性能如倾点和浊点所表示的,蜡状提余液的蜡含量减少,使其成为更好的基础油前体原料。使这样的蜡状提余液脱蜡成基础油也更简单有效。
费-托衍生产品包括费-托合成产品。“费-托合成产品”是指从费-托合成反应直接获得的产品,该产品可能已非必要地经过蒸馏和/或仅经过氢化。费-托合成产品可由公知方法获取,如所谓的商业Sasol法,Shell中间馏分油法,或非商业的Exxon法。这些方法及其它方法例如更详细地描述在EP-A-776959、EP-A-668342、US-A-4943672、US-A-5059299、WO-A-9934917和WO-A-9920720中。典型地,这些费-托合成产品包括具有1~100个,甚至多于100个碳原子的烃。这种烃产品包括正链烷烃,异链烷烃,含氧产品和不饱和产品。为了除去任何含氧化合物或不饱和产品,可以氢化步骤(a)的原料,或步骤(a)得到的任何馏分。
在步骤(a)的原料中,沸点高于540℃的化合物与沸点介于370~540℃之间的化合物的重量比大于2,优选大于2.5,甚至更优选大于3。费-托衍生产品的T10wt%回收点优选低于400℃。这种原料的制备可通过从费-托合成产品中分离出部分或全部的沸点为370℃~540℃的链烷烃馏分,和/或把含沸点高于540℃化合物的费-托衍生馏分加到费-托合成产品中。“沸点主要在某数值之间,或高于某数值”是指至少80重量%的所述馏分,优选至少90重量%的所述馏分在所述数值之间沸腾,或高于所述数值沸腾。
分离出来的沸点为370~540℃的链烷烃馏分可有利地作为石蜡销售,或作为原料,用于根据例如EP-A-1204723所述脱蜡方法制备基础油。脱蜡之前,该馏分适于经历如EP-A-776959所述的加氢异构化步骤。
沸点主要高于540℃的馏分可以是从费-托合成产品分离出来的石蜡产品,其具有高于90℃,优选高于95℃的冻点。
本发明还涉及一种方法,该方法通过以下步骤同时制备两个或多个等级的冻点为30~120℃的石蜡以及蜡状提余液产品:
(i)使部分费-托合成产品经历氢化步骤,以从费-托产品中除去含氧化合物和烯烃;
(ii)从氢化后的费-托产品中分离两个或更多蜡等级,其中,至少一个等级具有30~80℃的冻点,至少一个重质等级具有高于90℃、优选高于95℃的冻点;
(iii)混合部分或全部重质蜡与另一部分费-托合成产品,以获得用于步骤(a)的费-托衍生产品。
对本发明方法特别有利的是,步骤(i)中用的费-托合成产品的相当部分,优选超过10重量%,更优选超过30重量%,甚至更优选超过50重量%,在高于550℃时沸腾。制备这种重质费-托合成产品的一个合适方法的实例描述在WO-A-9934917和AU-A-698392中。当将这种产品用于上述方法时,必须从所述费-托合成产品中分离出少量沸点370~540℃的馏分,和/或必须再加少量沸点高于540℃的材料,以获得同样所需重量的馏分。或者可选地,可以获得甚至更高重量的馏分,从而从本发明的优点中获益更多。
在步骤(a)中,费-托衍生原料经氢化步骤产生蜡状提余液产品。步骤(a)在氢和催化剂的存在下进行,催化剂选自本领域技术人员已知适于此反应的催化剂。用于步骤(a)的催化剂典型地是无定形催化剂,包括酸官能度和氢化/脱氢官能度。优选的酸性官能度是耐火金属氧化物载体。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,二氧化钛和其混合物。优选包括在本发明方法的催化剂中的载体材料是二氧化硅,氧化铝,和二氧化硅-氧化铝。特别优选的催化剂包括担载在二氧化硅-氧化铝载体上的铂。如果需要,可以向载体上施加卤素部分,特别是氟或氯,以增强催化剂载体的酸度,但是由于环境原因,这通常不优选。合适的加氢裂化/加氢异构化方法及合适催化剂的实例描述在WO-A-200014179,EP-A-532118,以及较早引用的EP-A-776959中。
优选的氢化/脱氢官能度是VIII族非贵金属,例如WO-A-0014179、US-A-5370788或US-A-5378348中描述的镍;更优选是VIII族贵金属,例如钯和最优选为铂。催化剂可包括氢化/脱氢活性组分,该组分的量,以每100重量份载体材料计,为0.005~5重量份,优选0.02~2重量份。特别优选用于加氢转化阶段的催化剂包括铂,以每100重量份载体材料计,铂的量为0.05~2重量份,优选0.1~1重量份。催化剂还可含有粘结剂,以增强催化剂强度。粘结剂可以是非酸性的。实例为粘土和本领域技术人员已知的其它粘结剂。优选地,催化剂基本上是无定形的,这意味着催化剂中不存在晶体相。因此排除了含分子筛如β沸石的催化剂,因为它们通常引起过量的重质尾馏分裂化,而不是增加所需的异构化反应。
在步骤(a)中,费-托衍生原料与氢气在高温高压和催化剂存在下接触。温度典型地为175~380℃,优选高于250℃,更优选300~370℃。压力典型地为10~250巴,优选20~80巴。氢气以100~10000Nl/l/hr,优选500~5000Nl/l/hr的气时空速供应。烃原料以0.1~5kg/l/hr,优选高于0.5kg/l/hr,更优选低于2kg/l/hr的重时空速供应。氢气与烃原料的比值为100~5000Nl/kg,优选为250~2500Nl/kg。
步骤(a)的转化率定义为沸点高于370℃的原料单程反应成为沸点低于370℃的馏分的重量百分比,其优选至少20重量%,更优选至少25重量%,优选不超过80重量%,更优选不超过65重量%,甚至更优选不超过50重量%。
接下来,蜡状提余液产品可通过例如EP-A-1366135或EP-A-1366134描述的通常已知的溶剂或催化脱蜡法,脱蜡成为基础油。蜡状提余液产品也可用在传统的精制环境中,以改善由矿物油原料的基础油生产。由于蜡状提余液具有低于40℃,优选低于35℃,甚至更优选低于30℃的相对低倾点,它易于通过例如船舶输送到距终端消费者更近的海外精炼厂。适当地,可将蜡状提余液加入催化脱蜡单元的矿物油基原料中,以改善最终基础油的粘度指数。
通过下面的实施例说明本发明。
实施例1
使表1的原料2经历加氢裂化步骤,其中原料接触无定形二氧化硅-氧化铝载体担载的0.8重量%铂。裂化步骤的条件是:原料重时空速(WHSV)为1.0kg/l·h,无循环,氢气流量为1000Nl/kg,总压力为32巴。反应器温度如表2所列。分析裂化器的流出液,将蜡状提余液产品的产率和性能示于表2中。
表1
对比例A
用表1的原料1重复实施例1。结果示于表2中。
表2
实施例 | 1 | 2 |
反应器温度,℃ | 333 | 336 |
沸点低于370℃的馏分 | 57.3 | 57.2 |
沸点为370~540℃的馏分 | 20.4 | 21.8 |
沸点为370~540℃的馏分的倾点为 | +30℃ | +27℃ |
沸点为370~540℃的馏分的浊点 | +43℃ | +38℃ |
比较实施例1中由原料2所得结果和对比例中由原料1所得结果可见,根据本发明由原料2获得的基于费-托衍生产品(原料)的蜡状提余液产率(21.8%),显著高于使用现有技术原料1获得的产率(20.4%)。由原料2获得的蜡状提余液,其蜡状提余液馏分的倾点和浊点(倾点为+27℃,浊点为+38℃)都明显好于由现有技术原料1获得的蜡状提余液(倾点为+30℃,浊点为+43℃)。
Claims (9)
1.通过进行以下步骤制备蜡状提余液产品的方法:
(a)使费-托衍生产品经历加氢转化步骤,在该费-托衍生产品中,沸点高于540℃的化合物与沸点在370℃~540℃之间的化合物的重量比大于2;和
(b)分馏步骤(a)的流出液,以获得沸点在燃料范围内的产品和沸点在350~600℃之间的蜡状提余液产品。
2.根据权利要求1的方法,其中沸点高于540℃的化合物与沸点在370~540℃之间的化合物的重量比大于2.5。
3.根据权利要求1~2任一项的方法,其中费-托衍生产品的T10wt%回收点低于400℃。
4.根据权利要求1~2任一项的方法,其中步骤(a)的费-托衍生产品是通过从费-托合成产品中分离出部分或全部的沸点为370℃~540℃的链烷烃馏分而制备的。
5.根据权利要求1~2任一项的方法,其中步骤(a)的费-托衍生产品是通过将含沸点高于540℃化合物的费-托衍生馏分加到费-托合成产品中而制备的。
6.通过以下步骤同时制备两个或多个等级的冻点为30~120℃的石蜡以及蜡状提余液产品的方法:
(i)使部分费-托合成产品经历氢化步骤,以从费-托产品中除去含氧化合物和烯烃;
(ii)从氢化后的费-托产品中分离出两个或更多个蜡等级,其中至少一个等级具有30~80℃的冻点,至少一个重质等级具有高于90℃的冻点;
(iii)混合部分或全部重质蜡与另一部分费-托合成产品,以获得费-托衍生产品,在该费-托衍生产品中,沸点高于540℃的化合物与沸点在370~540℃之间的化合物的重量比大于2,而且将该费-托衍生产品用于权利要求1的方法中。
7.根据权利要求6的方法,其中在步骤(ii)中,至少一个重质等级的冻点高于95℃。
8.根据权利要求1~6任一项的方法得到的蜡状提余液产品作为原料制备基础油的用途。
9.通过实施权利要求1~6任一项的方法以及实施用所述蜡状提余液作为原料的附加脱蜡步骤,制备基础油的方法。
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EP (2) | EP1641898B1 (zh) |
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CN (2) | CN100439475C (zh) |
AT (2) | ATE498670T1 (zh) |
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US7727376B2 (en) | 2010-06-01 |
DE602004009073T2 (de) | 2008-06-19 |
WO2005003067A3 (en) | 2005-05-19 |
WO2005005575A1 (en) | 2005-01-20 |
EP1641898A2 (en) | 2006-04-05 |
US20060157384A1 (en) | 2006-07-20 |
DE602004031423D1 (de) | 2011-03-31 |
DE602004009073D1 (de) | 2007-10-31 |
CN1761733A (zh) | 2006-04-19 |
ATE498670T1 (de) | 2011-03-15 |
JP2009513496A (ja) | 2009-04-02 |
CN100439475C (zh) | 2008-12-03 |
WO2005003067A2 (en) | 2005-01-13 |
EP1641897B1 (en) | 2011-02-16 |
EP1641897A1 (en) | 2006-04-05 |
ATE373698T1 (de) | 2007-10-15 |
JP4740128B2 (ja) | 2011-08-03 |
CN1761734A (zh) | 2006-04-19 |
EP1641898B1 (en) | 2007-09-19 |
JP5000296B2 (ja) | 2012-08-15 |
JP2009513729A (ja) | 2009-04-02 |
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