CN101528648A - 用于gtl装置的轻烃回收方法 - Google Patents

用于gtl装置的轻烃回收方法 Download PDF

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CN101528648A
CN101528648A CNA2007800390693A CN200780039069A CN101528648A CN 101528648 A CN101528648 A CN 101528648A CN A2007800390693 A CNA2007800390693 A CN A2007800390693A CN 200780039069 A CN200780039069 A CN 200780039069A CN 101528648 A CN101528648 A CN 101528648A
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gas
isolating
synthetic
make
synthetic gas
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莫塞斯·K·明特
爱德华·L·金布尔
拉塞尔·H·奥尔弗克
埃里克·D·纳尔逊
罗斯·莫夫雷
阿尔布雷希特·格特姆
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ExxonMobil Technology and Engineering Co
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Abstract

本发明涉及GTL方法，其包括：在多种条件下使可燃性碳质材料在合成气反应器、优选自热转化器中反应，以制造合成气；使该合成气与F－T催化剂接触以形成液体产物和尾气；使该尾气与该液体产物分离；使该尾气中的CO2与轻产物分离；回收该轻产物作为附加产物用于销售或其它用途，并且利用分离的CO2的至少一部分作为送至合成气反应器的进料流。

Description

用于GTL装置的轻烃回收方法
技术领域
本发明主要涉及包含烃的气体进料向液体产物的转化，这种转化通常被称为气液(GTL)方法。更具体地，本发明涉及一种用于改进来自GTL方法的尾气产物的利用的系统和方法。
背景技术
由天然气或其它合成气体(合成气)源合成制造液体燃料、润滑剂、醇、醇衍生物和其它含氧化合物是众所周知的，并且一般称为气液(GTL)方法。基本上，首先把碳质材料转化成包含一氧化碳和氢气的气体，即，合成气。然后，通过众所周知的Fischer-Tropsch方法将合成气催化转化成液体产物。
使碳质材料气化成合成气的方法在工业中是已知的。之前采用了三种基本方法。这些方法是：(1)一种或多种轻烃如甲烷在催化剂上的蒸汽转化；(2)一种或多种轻烃的亚化学计量部分氧化；及(3)被称为自热转化的部分氧化和蒸汽转化的组合。
自热转化具有这样的优点，即把通过部分氧化方法产生的热用来提供吸热的蒸汽转化反应必需的热。此外，与单独蒸汽转化相比，自热方法导致合成气中更低的氢气对一氧化碳比例。已知F-T方法的H2/CO化学计量比为约2∶1，但是除了化学计量比，还有许多使用的理由。可以向三种合成气方法中任一种的进料中添加蒸汽(H2O)和CO2，以改变产物H2/CO比例。额外的蒸汽提高了H2/CO的比例，而额外的CO2降低了该比例。
在F-T方法中获得的反应产物取决于所采用的反应条件和催化剂。例如，高反应温度有利于醇、醇衍生物如醚及其它含氧化合物的形成。低反应温度有利于液体链烷烃和蜡的形成。在任一情况下，产物流典型地还包含未反应的合成气、水及其它气体如CO2和N2。使烃和水分离，残留尾气典型地包含未反应的合成气、CO2、N2、Ar、想得到的气体产物和水蒸气。N2和Ar典型地存在于进料到自热转化器中的进料气体或氧气中。尾气可以用作GTL装置的燃料，或者部分尾气可以用作自热转化器的CO2源。对于任一用途来说，由于稀释了反应物浓度而导致更大设备的N2和Ar物种的存在，尾气的组成基本上小于最佳组成，并且在N2的情况下可能会在转化过程中形成不合需要的HCN和NH3副产物。
发明内容
本发明涉及从来自气液(GTL)装置的F-T反应器的尾气中回收气体烃(轻烃(light ends))以及提供用于GTL装置的工艺气流。
在本发明的一个方面，GTL方法包括：在多种条件下，使可燃性碳质材料在合成气反应器、优选自热转化器中反应，以制造合成气；使该合成气与F-T催化剂接触，以形成液体产物和尾气；使该尾气与该液体产物分离；使该尾气中的CO2与轻产物分离；回收该轻产物作为附加产物用于销售或其它用途，并且利用至少一部分分离的CO2作为送至合成气反应器的进料流。
在本发明的另一个方面中，所述方法用于从尾气中提取CO2用于隔离(sequestration)。这减少了来自GTL装置的净温室气体排放。
阅读了后面的具体实施方式，本发明的其它方面将变得显而易见。
附图说明
图1是阐明本发明的多个方面的方框图。图2A、2B、3A、3B、4和5是阐明本发明优选实施方案的示意图。
具体实施方式
为了方便起见，将具体参照用于制造液体产物如液体燃料和润滑剂的综合的自热转化和F-T烃合成方法描述本发明。然而，本发明同样适用于F-T方法的其它变化方式，如用于制造醇、特别是甲醇和其它含氧化合物的F-T方法。
在综合的自热转化和F-T合成方法中，自热转化步骤的进料典型地包含气体轻烃如甲烷。取决于进料的组成和物理性质，如果必要的话，可以对其进行预处理以除去进料中的任何杂质。然而，N2通常是无需被除去的杂质，如果以低得可以接受的含量存在的话。在任何预处理之后，把烃进料送到自热转化器中以使其在这里与蒸汽和包含氧气的气体如空气反应。取决于应用，优选地，所使用的氧气将是在空气分离单元中产生的基本上纯的氧气流，但是可以包含一些大气中的氩气和氮气，这取决于所利用的空气分离方法。
自热转化方法典型地在约1750°F(955℃)至约2000°F(1090℃)范围内的温度下于高达约800psig(5520kPa)的压力下进行。在自热转化方法中形成的热的气体产物，合成气，包含作为F-T烃合成步骤中的关键反应物的一氧化碳和氢气。
典型地，使来自于自热转化器的热合成气经受冷却和净化以除去过量的水、氨和其它杂质。然后把合成气送到F-T反应器中，在该反应器中使合成气与烃合成催化剂接触。
合成气中的氢气对一氧化碳的摩尔比可以从约0.5∶1至4∶1变化，但是更典型地在约0.7∶1至2.75∶1范围内且优选为0.7∶1至2.5∶1。
众所周知，在F-T合成方法中，催化剂可以为固定床、流化床或催化剂颗粒在烃浆料液体中的浆料形式。尽管适合的F-T催化剂包括一种或多种第VIII族金属如Fe、Ni、Co、Ru和Re，但是在本发明中优选所述催化剂包括钴催化成分。有用的催化剂和它们的制备是已知的，并且示例性实施例可以在美国专利4568663、4663305、4542122、4621072和5545674中找到。
采用负载的含钴催化剂的浆料方法中典型的F-T工艺条件包括，分别在约320°F至850°F(160℃至454℃)、80psia至600psia(550kPa至4136kPa)和100至40000V/小时/V范围内的温度、压力和气时空速，气时空速表示为每小时每单位体积催化剂的气体CO和H2混合物的标准体积(0℃，1atm)。
F-T烃合成方法的产物组成将取决于许多因素，如所采用的催化剂和工艺条件。典型地，产物将包括C1至C200及更高级的链烷烃和烯烃，不同量的二氧化碳，水及含氧化合物如醇、醛、酮和酯。
通常使F-T产物流分离成单独的尾气流、液体烃流和废水流。F-T方法想得到的产物是液体烃。这些液体烃典型地具有C5至C200及更高级的烃链。
F-T尾气流是当冷却反应产物时不冷凝的气态物流。典型地，尾气流包含CO、H2、CO2、H2O、N2、Ar和C1至C5烃。
本发明的一个方面是从尾气流中回收轻烃。这通过首先使尾气流脱水以提供干气流，此后把干气流分馏成至少被回收的轻烃(C3和更重)以及包含甲烷、乙烷、乙烯、H2、CO和CO2、N2及Ar的气流而实现。本发明的另一方面是从尾气中回收富含CO2的气流，富含CO2的气流的至少一部分用作自热转化器中的进料。希望使N2和Ar与送到自热转化器中的CO2分离并返回富含CO2的流，因为这些气体在该方法中是惰性的并降低了生产效率，同时增加所需设备尺寸，并且氮气会反应形成不合需要的副产物。
把CO2进料到自热转化器中以帮助控制合成气H2/CO比例。其对进料气体中的H2O(蒸汽)起着平衡作用。增加CO2和/或降低H2O将趋向于降低合成气H2/CO的比例。相反地，降低CO2和/或增加H2O将趋向于提高H2/CO的比例。以这样的方式利用CO2和H2O是控制合成气化学的高效方法。对合成气化学的精确控制是F-T反应最有效率的工作必需的。
在本发明的方法中，通过压缩气体并且冷却压缩的气体至足以导致尾气中水和任何烃液体分离的温度和压力，使尾气脱水。典型的温度和压力在约50°F(10℃)至约100°F(38℃)和约225psig(1650kPa)至约1100psig(7686kPa)范围内。然后使冷凝的液体与气体分离，从而提供脱水的尾气流。在该步骤中，气体不应当冷却至低于形成水合物的温度。
作为选择或者另外，可以通过使气体经过吸附剂如分子筛，通过使用隔膜分离器，或者利用干燥剂如三乙二醇或氯化钙，使尾气进一步脱水。任选地，可以使脱水的尾气流经受其它净化步骤(polishing step)以保证水从尾气流中基本上完全除去。可以采用任何通常使用的天然气脱水技术来使尾气脱水，这些技术对于本领域的技术人员来说是已知的。
为了从脱水的尾气流中回收轻烃，在约225psig(2760kPa)至约1100psig(7580kPa)的压力下把干气体冷却至约-50°F(-46℃)至约32°F(0℃)的温度范围内，选取条件来液化足够的CO2以达到所需的生产速率。然后把冷却的混合物传送到第一分馏塔中，以使干尾气中的任何惰性气体如N2和Ar与液体CO2和轻烃分离。然后把液体CO2和轻烃传送到第二分馏塔中，以使CO2与轻烃分离。然后回收轻烃用于销售或其它用途。例如，在本发明的一个实施方案中，把轻烃的一部分再循环到第一分馏塔中，以提高第一分馏塔的工作效率。
在本发明的另一个实施方案中，把分离的富含CO2的气流的至少一部分用作自热转化器中的进料气体。
在本发明的又一个实施方案中，把来自第一分馏塔的包含惰性气体、H2和CO的气体用作GTL装置的燃料。
在本发明的优选实施方案中，在自冷却过程中，分馏塔中惰性气体的分离所需的低温冷却由产生功的气体骤冷器(expander)提供。惰性气体是沸点低于CO2和轻烃的气体，因此在第一分馏塔中更容易蒸发和分离。由产生功的骤冷器提供的过冷用来为进料分馏塔的工艺物流提供补充冷却。此外，由骤冷器产生的功用来提供在工艺的前端压缩工艺物流所需的功，从而增强工艺的脱水步骤。过程中热能和机械能两者的完全整合增强了整体性能，使外部能量需求最小。
现在将通过参照附图描述本发明的方法和系统。首先转向图1流程图，使碳质燃料10、蒸汽11和包含氧气的气流12在合成气产生反应器14中反应，以产生被传送到烃合成反应器16(F-T反应器，例如)中的合成气流15。然后把烃合成反应器16的产物17传送到烃回收单元18中，在这里使产物分离成水和含氧化合物19、液体烃20、蜡21和尾气22。接着把尾气22送到尾气加工体系23中以回收轻烃24、富含CO2的气流25和剩余流26，剩余流26可以包含惰性气体、H2和CO。富含CO2的气流25的至少一部分作为进料引入到合成气产生反应器14中以控制反应化学。合成气产生反应器14优选为自热反应器，但是可以为其中需要CO2流的用于制造合成气的几种转化技术中任何一种，如与部分氧化体系组合的蒸汽甲烷转化的部件。此外，烃合成反应器(HSR)(16)是合成反应器如F-T反应器或甲醇合成反应器的代表，这是本领域的技术人员已知的。剩余气流26可以用作GTL装置的低BTU燃料。
尾气加工体系23将描述为包括两个阶段：脱水阶段和产物分离阶段。首先转向脱水阶段，如图2A所示，尾气22在压缩机28中压缩和在冷却器29中冷却，并传送至分离单元30以分离成水27、烃液体31和尾气流32。尽管仅示出了单个的压缩机，但是应当理解压缩可以分多个阶段完成以及压缩机的功率可以由骤冷器提供。此外，冷却体系29可以由几个冷却源组成，该冷却源包括水或空气、外部冷却如丙烷-基单元和/或来自工艺的其它部件的冷流。干尾气32任选地可以在脱水器33中经受最后净化步骤，在脱水器33中从尾气32中除去任何剩余水34以提供尾气流35。脱水器33可以包括含有一个或多个适合的用于干燥尾气流的分子筛的容器。图2B为脱水阶段的实施方案，其中大部分水分离分两个阶段完成。可以看出，元件具有与图2A中相同的附图标记，所不同的是，压缩机、冷却器和分离单元的附图标记分别包括在第一阶段和第二阶段中的“a”和“b”。
现在参照产物分离阶段并具体参照图3A，脱水尾气32或35在换热单元36(可以包括或不包括外部制冷剂的多股流换热器)中冷却，然后经由管线37引入到充当惰性气体排除塔的第一分馏塔38中。塔38主要除去惰性气体、H2和CO至所需水平，剩余富含轻烃和CO2的液体流。换热单元36中所需的冷却可以由外部冷却源如丙烷冷却单元，由通过骤冷(expanding)来自惰性气体排除塔38顶部的气体提供的自冷却，或者由工艺的其它部分中可利用的其它冷流提供。把来自惰性气体排除塔38底部的主要由轻烃和CO2组成的液体流经由管线47传送到第二分馏塔39，产物回收塔中，第二分馏塔39把液体流分离成富含CO2的气流25和富含轻烃组分的液体产物流24。优选地，富含CO2的气流25的至少一部分用来在换热单元36中提供补充冷却，然后如图1所示作为进料传送到合成气反应器中。
如图3A所示，来自塔38顶部的气流40可以在产生功的设备如骤冷器41中骤冷并经由管线42传送到分离器43中。把得自骤冷设备的液体经由管线44和泵45作为回流返回到塔38中，而剩余气流26任选地用于在换热单元36中的补充冷却并最后用作GTL装置中的燃料。塔38和39可以分别装备有再沸器50和52，以把一部分液体流再循环到它们各自的分馏塔中。塔39还可以装备有冷凝器48，以把一部分物流再循环回到塔中。图3B为产物分离阶段的实施方案，其中产物回收塔38为惰性气体排除塔提供了补充回流液流54。
本领域的技术人员应当理解在该实施方案内有许多变化方式，包括但不限于下列内容：进入惰性气体排除塔的输入物可以利用产生功的设备骤冷以制造流37；来自惰性气体排除塔顶部的气流的骤冷可以分两个阶段进行，以阻止CO2固体形成的可能性；可以向脱水的尾气32(35)中注入添加剂流，以增强塔中的分离过程并且添加剂随后可以从流24回收。
图4显示了本发明的替换实施方案，其中第一分馏塔60是高压吸收器。在该实施方案中，可以把未示出的附带的精馏器添加至第二塔39。可以实践几种其它任选的变化方式，这取决于工作条件和尾气的组成。例如，所有轻烃24都可以回收和使用或销售。任选地，轻烃的一部分可以回收，而另一部分可以经由管线62再循环到塔60中。在又一个选择中，可以在处理步骤61中对轻烃24进一步处理，该处理步骤包括例如一个附带的汽提塔或多个附带的汽提塔，如在Ryan-Holmes型工艺设备中所提供的。在该选择中，可以回收所有浓缩的轻烃，或者仅回收一部分用于销售或其它用途，而一部分经由管线62再循环到第一个塔60中。
图5显示了本发明的特别优选的实施方案。在该实施方案中，脱水阶段由两个连接以实现大部分液体分离的分离器30a和30b组成，其后是分子筛脱水单元33。在该实施方案中，第一分馏塔60是高压吸收器。第二分馏塔39装备有附带的精馏器64，以把一些液体返回到塔39中而提高该塔的工作效率。低BTU燃料气体26和富含CO2的气流25在该实施方案中分别用来向在30a和30b中脱水的进料气体22提供补充冷却。此外，用于满足工艺中压缩需要的功率部分地由过程骤冷器41和65提供。
任选的特征包括用于压缩进料到合成气产生反应器中的富含CO2的气流25的压缩机68的使用，用于在脱水之前压缩进料气体22的压缩机28的使用，及为了实现过程控制灵活性在进料气体回路的压缩机66的使用。
下表1显示了在图5中标记的各个状态点的加工条件。这些加工条件利用由Aspentech，Cambridge，Mass出售的商品名为Aspen HYSYS的工业过程模拟软件测定。
表1
  状态点   压力(kPa)   温度(℃)   流量(kg摩尔/小时)
  22   1724   48.9   29990
  1   3668   127.6   29990
  9   3599   44.6   30630
  3   6832   23.7   30220
  35   6728   24.8   29470
  37   5964   -31.6   29470
  47   3068   -37.4   6327
  40   5929   -34.8   24310
  24   3068   135.4   895
  25   3634   65.6   4309
  26   660   45.7   15380
  27   3599   44.6   296
  31   3599   44.6   198

Claims (24)

1.一种GTL方法，其包括：
(a)在制造合成气的条件下使碳质材料在合成气产生反应器中反应；
(b)在可形成液体产物及包含轻烃和CO2的尾气的条件下使该合成气与Fischer-Tropsch催化剂接触；
(c)使液体烃与尾气分离；
(d)使尾气中的CO2与轻烃分离；
(e)回收分离的轻烃；及
(f)利用至少部分分离的CO2作为合成气产生反应器中的进料。
2.根据权利要求1的方法，该方法包括使在步骤(c)中分离的尾气脱水及分馏分离且脱水的尾气，以使CO2与轻烃分离。
3.根据权利要求2的方法，其中通过将该尾气压缩至约1650kPa至约7700kPa的压力并且冷却至约10至约38℃范围内的温度，使尾气脱水。
4.根据权利要求3的方法，其中该脱水尾气在第一分馏塔中分馏以除去惰性气体，从而提供惰性气体含量减小的液体，此后在第二分馏塔中分馏第一分馏塔的液体以使CO2与轻烃分离。
5.根据权利要求4的方法，其中该脱水尾气首先在约2760kPa至约7580kPa的压力下冷却至约-46℃至约0℃范围内的温度。
6.根据权利要求5的方法，其中该第一分馏塔是高压吸收器。
7.根据权利要求6的方法，其中把在第二分馏塔中分馏的液体的一部分以足以提高塔的工作效率的量返回到第二塔中。
8.根据权利要求7的方法，该方法包括把步骤(e)的轻烃的一部分再循环到高压吸收器中。
9.根据权利要求6或7的方法，该方法包括在将分离的CO2进料到合成气产生反应器中之前，利用它作为冷却流。
10.根据权利要求9的方法，其中该合成气产生反应器为自热转化器。
11.根据权利要求9的方法，其中使该至少部分分离的富含CO2的气流被隔离。
12.在F-T合成方法中，其中在足以制造液体产物及包含惰性气体、CO2和气态烃(轻烃)的尾气的条件下使合成气与催化剂接触，并且其中将该液体产物与尾气分离并回收，改进包括：
使分离的尾气脱水；
在第一分馏塔中分馏脱水的尾气，以除去惰性气体；
分馏余量的尾气，以使CO2与气态烃分离；及
回收液体烃(轻烃)。
13.根据权利要求12的改进，该改进包括把至少一部分分离的CO2进料到在足以制造合成气的条件下工作的合成气产生反应器中。
14.根据权利要求13的改进，其中该合成气产生反应器为自热转化器。
15.根据权利要求14的改进，其中该第一分馏塔为高压吸收器。
16.根据权利要求15的改进，其中把回收的轻烃的一部分再循环到高压吸收器中。
17.一种用于制造液体烃的GTL系统，该系统包括：
(a)合成气产生反应器，其用于使碳质进料与氧化气流反应以制造包含H2、CO和CO2的合成气流；
(b)烃合成反应器，其用于使该合成气与催化剂接触以促进液体烃产物的形成；
(c)用于把来自该合成气产生反应器的合成气引入到烃合成反应器中的装置；
(d)用于使来自该合成反应器的产物液体烃与未反应的合成气和其它气体烃(尾气)分离的装置；
(e)用于使该气体烃与未反应的合成气分离并将气体烃回收的装置；及
(f)用于使CO2与未反应的合成气分离并把分离的CO2的至少一部分作为进料引入到合成气产生反应器中的装置。
18.根据权利要求17的系统，该系统进一步包括用于使与合成反应器的液体产物烃分离的未反应的合成气和其它气态烃脱水的装置。
19.根据权利要求18的系统，该系统进一步包括用于从在脱水装置中脱水的气体中分离惰性气体的分馏装置和用于使CO2与气体烃分离的分馏装置。
20.根据权利要求19的系统，该系统包括用于在把分离的CO2作为进料引入到合成气产生反应器中之前利用分离的CO2的冷却能力的装置。
21.根据权利要求20的系统，其中该脱水装置包括压缩机及用于冷凝和除去水蒸气的冷却体系。
22.根据权利要求21的系统，其中该合成气产生反应器为自热转化器。
23.根据权利要求22的系统，其中用于分离惰性气体的该分馏装置是高压吸收器。
24.根据权利要求23的系统，其中用于使CO2与气体烃分离的该分馏装置包括用于进一步分离所分离的烃的一部分并且将其返回到分馏装置中的精馏装置。
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