CN101489930A - 制备二硫化碳的方法和含二硫化碳的液态物流用于强化油采收的用途 - Google Patents

制备二硫化碳的方法和含二硫化碳的液态物流用于强化油采收的用途 Download PDF

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CN101489930A
CN101489930A CNA2007800249366A CN200780024936A CN101489930A CN 101489930 A CN101489930 A CN 101489930A CN A2007800249366 A CNA2007800249366 A CN A2007800249366A CN 200780024936 A CN200780024936 A CN 200780024936A CN 101489930 A CN101489930 A CN 101489930A
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dithiocarbonic anhydride
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C·M·A·M·梅斯特斯
R·J·斯洪比克
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Shell Internationale Research Maatschappij BV
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Abstract

本发明提供一种通过使一氧化碳和元素硫反应以形成硫化羰和使所形成的硫化羰歧化成二硫化碳和二氧化碳制备二硫化碳的方法，该方法包括在250－700℃的温度下使含一氧化碳的气态物流与含固体催化剂的液态元素硫相接触，以获得含硫化羰、二硫化碳和二氧化碳的气相。本发明另外提供可通过该方法获得的含二硫化碳、硫化羰和二氧化碳的液态物流用于强化油采收的用途。

Description

制备二硫化碳的方法和含二硫化碳的液态物流用于强化油采收的用途
技术领域
本发明提供制备二硫化碳的方法和可从该方法获得的含二硫化碳、硫化羰和二氧化碳的液态物流用于强化油采收的用途。
背景技术
通常根据以下反应方程式通过轻质饱和烃与气相元素硫进行反应制备二硫化碳：
CnH2(n+1)+(3n+1)S→nCS2+(n+1)H2S
例如在GB 1,173,344中公开了在不超过10个大气压、不存在催化剂的条件下，在温度维持在550-850℃的反应区中使气相硫和丙烷反应的方法。
US 3，087,788公开了在与优选随后进行的催化反应阶段结合的非催化反应阶段中从烃气和气态硫生产二硫化碳的方法，其中两个阶段在2-20个大气压和400-750℃的温度下操作。
也已知通过使液态硫和烃催化反应制备二硫化碳。例如在US2,492,719中公开了制备二硫化碳的方法，其中催化剂于熔态硫中的悬浮体与烃气在约500-700℃的温度下、足使硫保持在液相中的压力下进行接触。
使用烃作为碳源以制备二硫化碳的缺点在于烃中的氢原子与元素硫反应形成硫化氢。使用不含氢原子的碳源制备二硫化碳将是有利的。
1960年以前，将固体碳质材料例如木炭用作二硫化碳制备的碳源。在非常高的温度下使固体碳质材料与气化的元素硫接触。然而出于对环境和安全的考虑，这些使用固体碳质材料的方法被上述使用轻质烃(例如甲烷和丙烷)作为碳源的方法所替代。
已知使用一氧化碳作为二硫化碳制备的碳源。例如在US2004/0146450中公开了从一氧化碳和二氧化硫制备二硫化碳的双反应器方法。两个催化反应一前一后进行操作。在第一反应器中，在存在催化剂的条件下使一氧化碳和二氧化硫进行反应以形成硫化羰和二氧化碳。在第二反应器中，将在第一反应器中形成的硫化羰催化转化成二硫化碳和二氧化碳。通过溶剂从第二反应器连续移除二硫化碳。
在US 4,122,156中也公开了从一氧化碳和二氧化硫制备二硫化碳的双反应器方法。
已知二硫化碳是用于通过混相驱油强化油采收的适合溶剂。在通过混相驱油的强化油采收中，将用于油的溶剂加入油储层中和驱使通过油储层以与常规方法所能达到的油采收相比强化从储层的油采收。例如在US 3,847,221中公开了使用二硫化碳以强化从焦油砂的油采收。
目前已发现可通过在有效将所形成的硫化羰歧化成二硫化碳和二氧化碳的固体催化剂存在下，使一氧化碳与液态元素硫进行反应，从而在单个的反应区中从作为碳源的一氧化碳制备二硫化碳。
发明内容
因此，本发明提供一种通过使一氧化碳与元素硫进行反应制备二硫化碳的方法，该方法包括在250-700℃的温度下使含一氧化碳的气态物流与含固体催化剂的液态元素硫相接触，以获得含硫化羰、二硫化碳和二氧化碳的气相。预期本发明反应包括一氧化碳和元素硫的反应以形成硫化羰，随后将所形成的硫化羰歧化成二硫化碳和二氧化碳。
与使用烃作为碳源的常规二硫化碳制备法相比，本发明方法的一个重要优点是没有形成必须再循环至克劳斯装置以被转化成硫的硫化氢。
与已知的使用一氧化碳作为碳源的的二硫化碳制备方法(即US2004/0146450和US 4,122,156中公开的方法)相比，本发明方法的一个优点是该方法可在单个反应区中进行操作。另一个优点是副产更少的二氧化碳。在本发明方法中，1摩尔二硫化碳副产1摩尔二氧化碳，而在US 2004/0146450和US 4,122,156的方法中1摩尔二硫化碳副产5摩尔二氧化碳。
当与烃原料转化成合成气(即主要含一氧化碳和氢的气态混合物)组合操作时，本发明方法具有特别的优势。制得的合成气通常用于后续的通过费-托工艺合成烃、其它化学合成工艺、在燃气涡轮中发电或用于生产氢。经常地，对于设想的用途而言合成气中一氧化碳与氢的比太大，和随后通常通过使合成气进行水煤气变换反应而将合成气中的部分一氧化碳转化成氢。将本发明方法与合成气制备结合的优点在于将部分一氧化碳用于二硫化碳制备，从而将剩余合成气中一氧化碳与氢的比降低至更理想的水平。另一个优点是在合成气制备位置处通常可获得元素硫，这是因为通常在气化前对烃原料进行脱硫。另外的优点是将烃类化合物的氢原子转化成有价值的氢。副产的一氧化碳用作无氢原料以制备二硫化碳，和因此避免了形成硫化氢。
可冷凝在本发明方法中获得的含硫化羰、二硫化碳和二氧化碳的气相以获得含二硫化碳的液态物流。可对气相进行冷凝以获得含硫化羰、二硫化碳和二氧化碳的液相。替代地，可通过连续的部分冷凝步骤获得单独的液态物流，即主要含硫化羰和二氧化碳的第一液态物流和主要含二硫化碳的第二液态物流。含或不含硫化羰和二氧化碳的含二硫化碳的液态物流可用于强化油采收。
在另外的方面，本发明另外提供可通过本发明方法获得的含二硫化碳、硫化羰和二氧化碳的液态物流用于强化油采收的用途。
在本发明方法中，在250-700℃的温度下使含一氧化碳的气态物流与液态元素硫相接触。液态元素硫相含有将硫化羰有效催化歧化成二硫化碳和二氧化碳的固体催化剂。
液态硫相含在反应区(通常是反应器容器或反应器管)中，和含有固体催化剂。固体催化剂可以任意适合的方式含在液态硫相中，例如作为催化剂颗粒的固定床、作为涂布有催化剂的规整填料或作为分散在液态硫相中的催化剂颗粒。
通过使含一氧化碳的气态蒸汽与液态硫相接触，一氧化碳与元素硫根据以下反应方程式进行反应以形成硫化羰：
2CO+2S→2COS    (1)
随后使硫化羰歧化成二硫化碳和二氧化碳：
2COS<＝>CS2+CO2    (2)
对于反应(1)，热力学有利于平衡强烈向右进行。对于多至约700℃的反应温度，平衡常数远大于1和因此实现完全或几乎完全的转化。歧化反应(2)是热力学不太有利的。它是可逆反应。因为反应热接近0，平衡常数随温度变化不大。在本发明方法的温度和压力条件下，多至约40％的硫化羰可发生歧化。
反应(1)和(2)都在同时含液态元素硫相和浸于该相中的固体催化剂的相同反应区中进行。固体催化剂催化歧化反应(2)。反应(1)也可被催化剂催化。固体催化剂可以是有效将硫化羰催化歧化成二硫化碳和二氧化碳的任意催化剂。本领域中已知这些催化剂，例如在US2004/0146450和US 4,122,156已知的催化剂。优选地，催化剂包含一种或多种金属氧化物。适合的催化剂的实例为氧化铝、二氧化钛、氧化铝-二氧化钛、二氧化硅-氧化铝、石英或粘土例如高岭土。催化剂的比表面积优选为至少50m2/g、更优选至少100m2/g、甚至更优选至少200m2/g。特别优选的催化剂为γ-氧化铝、二氧化钛、氧化铝-二氧化钛或二氧化硅-氧化铝。
在本发明方法中，当含一氧化碳的气态物流与液态元素硫相接触时，将液态元素硫相保持在250-700℃的温度下。在低于250℃的温度下，液态硫相的高粘度将阻碍处理适当进行。优选地，温度为300-500℃。
该方法在足以维持液态元素硫相的压力下进行。优选地，压力为3-200巴(绝压)，更优选5-100巴(绝压)，甚至更优选5-30巴(绝压)。
该方法可在适合于在固体催化剂存在下使气体与液体接触的任意反应器构造中进行，例如并流或逆流固定床滴流反应器、浆态鼓泡塔或沸腾床反应器。
含一氧化碳的气态物流优选以一氧化碳与液态硫的接触时间为0.1-200秒的速度下供应至液态硫。因为在过程期间消耗元素硫，所以如果在过程期间没有向反应器补充供应元素硫的话则接触时间会随时间推移而降低。在过程期间可以将补充硫连续供应至反应器。替代地，可在一定时间投入生产之后，将元素硫分批供应至反应器。
气态物流的气体重量速度优选使得供应至催化剂的一氧化碳的小时速率为10-1000升一氧化碳(在标准温度和压力条件下)每千克催化剂每小时。气态物流中一氧化碳的含量可在较大范围内变化。优选一氧化碳的含量为气态物流总体积的10-100vol％。适合的含一氧化碳的气态物流的实例为合成气或贫氢合成气。本文所用的贫氢合成气指已通过例如变压吸收或膜分离除去其中部分氢的合成气。
优选地，含一氧化碳的气态物流是贫氢合成气。通常，通过首先部分氧化烃原料以获得含一氧化碳和氢的合成气和随后从合成气中分离至少部分氢而获得贫氢合成气。优选地，从富碳烃原料(即氢原子与碳原子的比低于1的烃原料)获得合成气或贫氢合成气。该富碳烃原料的实例是煤、焦油砂衍生沥青、从原油的真空蒸馏或从焦油砂衍生沥青的真空蒸馏获得的渣油。
在本发明方法中，获得含硫化羰、二硫化碳和二氧化碳的气相。优选地，至少部分冷凝该气相以获得含二硫化碳的液态物流。可将二硫化碳与硫化羰和二氧化碳一起进行冷凝。替代地，在连续部分冷凝步骤中，在第一冷凝步骤中首先冷凝硫化羰和二氧化碳和随后在第二冷凝步骤中冷凝二硫化碳。因此获得相对纯净的液态二硫化碳的物流。也可使用冷凝之外的纯化步骤以获得具有所需组成的含二硫化碳的液态物流。
应理解含二硫化碳的液态物流的所需组成将决定所需的冷凝和/或纯化步骤。对于二硫化碳的常规用途，例如将其用作生产人造丝的原材料或作为溶剂时，需要高纯度的二硫化碳。如果将液态物流用于强化油采收，即将其注入油储层中以从增大该储层的油产量，则液态二硫化碳物流可包含大量的硫化羰和二氧化碳。
在本发明方法中形成的含二硫化碳的液态物流特别适用于强化油采收中，因为液态物流通常包含在该应用中无需除去的二硫化碳之外的组分。因此，本发明方法优选另外包括将含二硫化碳的液态物流注入油储层中以强化油采收。在被注入油储层中之前，含二硫化碳的液态物流可与其它液态组分或物流进行混合。
通常，可通过本发明方法获得的含二硫化碳的液态物流也将含有硫化羰和二氧化碳。因此本发明另外提供可通过本发明方法获得的含二硫化碳、硫化羰和二氧化碳的液态物流用于强化油采收的用途。优选地，以液态物流的总体积计，使用的液态物流中二硫化碳的浓度为10-90vol％，硫化羰的浓度为5-80vol％，和二氧化碳的浓度为5-20vol％。
实施例
本发明方法将通过下列非限定实施例进行进一步说明。
实施例1(本发明)
用15克液态硫和7.1克比表面积为300g/m2的γ氧化铝三叶草(直径1.3mm，长度/直径比为3)的催化剂床层填充反应器管(内径12mm)。在10巴(绝压)的压力下、在60秒内，将由85.5vol％氮气和14.5vol％一氧化碳组成的气态物流以3.9标准升/小时的流量鼓泡通过反应器管。在不同的实验中，反应器管保持在不同的温度下(270-420℃)。用气相色谱分析气态反应器流出物的组成。在表1中示出了一氧化碳的总转化率和一氧化碳至二硫化碳的转化率。在所有实验中，歧化反应即硫化羰转化成二硫化碳和二氧化碳达到热力学平衡。
表1 使用催化剂的实验(实施例1)
 
实验 T(℃) CO转化率(％) 转化成CS2的CO转化率(％)
1 270 74 14
2 320 98 17
3 370 100 18
4 420 100 18
实施例2(对比例)
用32克液态硫填充反应器管(内径12mm)。反应器管不含有催化剂。在10巴(绝压)的压力下、在50秒内，将由80vol％氮气和20vol％一氧化碳组成的气态物流以3.0标准升/小时的流量鼓泡通过反应器管。在不同的实验中，反应器管保持在不同的温度下(370-520℃)。用气相色谱分析气态反应器流出物的组成。在表2中示出了一氧化碳的总转化率和一氧化碳至二硫化碳的转化率。
表2 不使用催化剂的实验(实施例2)
 
实验 T(℃) CO转化率(％) 转化成CS2的CO转化率(％)
5 370 10 0.03
6 420 30 0.04
7 520 98 0.3
结果显示在不存在催化剂的条件下下也发生了反应(1)(即一氧化碳转化成二硫化碳和二氧化碳)，尽管需要更高的温度来实现完全转化。在不存在催化剂的条件下则很难发生歧化反应(2)。

Claims (10)

1.一种通过使一氧化碳和元素硫反应制备二硫化碳的方法，所述方法包括在250-700℃的温度下使含一氧化碳的气态物流与含固体催化剂的液态元素硫相接触，以获得含硫化羰、二硫化碳和二氧化碳的气相。
2.权利要求1的方法，其中所述固体催化剂包含金属氧化物，优选选自氧化铝、二氧化钛、氧化铝-二氧化钛或二氧化硅-氧化铝的金属氧化物。
3.权利要求1或2的方法，其中所述含一氧化碳的气态物流在300-500℃的温度下与所述液态元素硫相接触。
4.前述权利要求任一项的方法，其中压力为3-200巴(绝压)，优选5-100巴(绝压)，更优选5-30巴(绝压)。
5.前述权利要求任一项的方法，其中所述含一氧化碳的气态物流是贫氢合成气。
6.权利要求5的方法，其中通过部分氧化氢原子与碳原子的比低于1的烃原料以获得含一氧化碳和氢的合成气和随后从合成气中分离至少部分氢获得所述贫氢合成气，优选其中氢原子与碳原子的比低于1的烃原料是煤、焦油砂衍生沥青、从原油的真空蒸馏或从焦油砂衍生沥青的真空蒸馏获得的渣油。
7.前述权利要求任一项的方法，另外包括冷凝至少部分含硫化羰、二硫化碳和二氧化碳的气相以获得含二硫化碳的液态物流。
8.权利要求7的方法，另外包括将含二硫化碳的液态物流注入油储层中用于强化油采收。
9.可通过权利要求7的方法获得的含二硫化碳、硫化羰和二氧化碳的液态物流用于强化油采收的用途。
10.权利要求9的用途，其中液态物流中二硫化碳的浓度为10-90vol％，硫化羰的浓度为5-80vol％，和二氧化碳的浓度为5-20vol％。
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