CN101443269A - 制备二硫化碳的方法 - Google Patents
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Abstract
本发明提供一种用于制备二硫化碳的方法,该方法包括:将含烃类化合物的进料供应至含液态元素硫相的反应区域,和在350-750℃的温度下、3-200巴(绝压)的压力下、不存在催化剂以及不存在氧分子的条件下于液态硫相中使烃类化合物与元素硫反应。本发明另外提供可通过该方法获得的含二硫化碳和硫化氢的液态物流用于强化油采收的用途。
Description
技术领域
本发明提供制备二硫化碳的方法和可通过该方法获得的包含二硫化碳和硫化氢的液态物流用于强化油采收的用途。
背景技术
通常根据以下的反应方程式通过将低级烃与气相元素硫进行反应制得二硫化碳:
CnH2(n+1)+(3n+1)S→nCS2+(n+1)H2S (1)
例如,在GB 1,173,344中公开了一种用于在维持于550-850℃温度下的反应区域内、在不超过10大气压的压力下、不存在催化剂的条件下使气相硫和丙烷进行反应的方法。
在US 3,087,788中公开了一种在与优选随后的催化反应阶段组合的非催化反应阶段中由烃气和硫蒸气生产二硫化碳的方法,其中两个阶段都在2-20大气压的压力和400-750℃的温度下进行。
另外已知通过液态硫与烃的催化反应制备二硫化碳。例如,在US2,492,719中公开了一种制备二硫化碳的方法,其中在足以将硫维持在液相下的压力下、在大约500-700℃的温度下将催化剂于熔融态硫中的悬浮体与烃气接触。
已知二硫化碳是用于通过混相驱强化油采收的适合溶剂。在通过混相驱强化油采收中,将用于油的溶剂加入油储层中和驱使溶剂通过储层,从而与常规方法相比提高从储层的油采收。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。
发明内容
目前已发现可在不含催化剂的条件下,通过使液态硫与烃反应以吸引人的收率制备硫化碳。
因此,本发明提供一种用于制备二硫化碳的方法,该方法包括将含烃类化合物的进料供应至含液态元素硫相的反应区域,和在350-750℃的温度下、3-200巴(绝压)的压力下、不存在催化剂以及不存在氧分子的条件下于液态硫相中使烃类化合物与元素硫反应。
本发明方法的优点在于该方法可在不存在催化剂的条件下进行。
与用于二硫化碳生产的常规气相法相比,本发明方法的优点在于该方法无需使硫气化。
在本发明的方法中,获得包含二硫化碳和硫化氢的气相。所述气相也可包含未转化的烃类化合物和元素硫。通过使气相经过单独或顺序的冷凝步骤,根据本发明的方法获得的包含二硫化碳和硫化氢的液态物流可适用于强化油采收。
因此,本发明另外提供包含二硫化碳和硫化氢的液态物流用于强化油采收的用途,所述液态物流可通过上文定义的方法获得。
在本发明的方法中,通过在含液态元素硫相的反应区域中使烃类化合物与元素硫反应制得二硫化碳。烃类化合物和元素硫之间的反应在液态硫相中进行。反应物在350-750℃的温度下和足以维持液态元素硫相的压力下互相进行反应。
该反应适合于在标准化学反应器例如釜式反应器中进行。这样的反应器通常包括竖直的管式反应器。长径比可为20/1-1/3,适宜地为10/1-1/1,例如5/1-1.5/1。烃类进料在反应器下端加入,至少在低于膨胀的液态硫柱的中部的位置。优选烃类进料在膨胀的液态硫柱下方1/3段加入,更优选在膨胀的液态硫柱下方1/4段例如膨胀的液态硫柱的10%高度处或甚至更低位置处加入。烃类进料和硫之间的反应在膨胀液态硫相的反应器中的边界内发生。本发明的方法包括固定反应器,不使用旋转反应器。
将含烃类化合物的进料供应至含液态元素硫相的反应区域。本文中提到的烃类化合物是含碳原子和氢原子以及任选的少量杂原子例如氧、硫或氮的化合物。在所应用的反应条件下,烃类化合物可为气态、液态或固态。适合的烃类化合物的实例是烃、沥青、硫醇、噻吩和烷基多硫化物。优选地,烃类化合物在所应用的反应条件下为气态。
烃类化合物优选是烃,更优选是饱和或不饱和脂族烃,更优选是含有1-20个碳原子的脂族烃。在本发明的方法中,含有1-4个碳原子的饱和烃、特别是甲烷、乙烷和丙烷是特别适合的反应物。
在本发明的方法中,烃类化合物和元素硫互相反应。当烃类化合物是饱和脂族烃时,该反应适用总反应方程式:
CnH2(n+1)+(3n+1)S→nCS2+(n+1)H2S
进料可包含一种以上烃类化合物。进料也可包含其它化合物,例如硫化氢、碳氧化物和惰性气体例如氮气和氦气。适用于本发明方法的进料的实例是天然气、液化丙烷气(LPG)、常压或真空馏出物、重油物流例如原油常压和/或真空蒸馏后获得的残余物、来自硫醇吸收器的含硫醇的尾气。特别适用的含烃类化合物的进料是天然气。
在本发明的方法中,通常将进料连续供应至反应区域。当烃类化合物在所应用的反应条件下是固态时,优选通过将进料与反应区域中将要填充的液态硫相进行预混将进料供应至反应区域。当烃类化合物在所应用的反应条件下是液态时,也可按照这种方法进行处理。优选地,将液态进料连续供应至反应区域。
当进料是气体时,该方法可在任意适用于气-液接触的反应器结构中进行,通常通过使气态反应物鼓泡通过填充有液态硫的反应器进行。为了防止形成气栓,反应器可含有固体接触器,例如规整填料或滤网。对于气态烃类化合物,烃类化合物与液态硫的初始接触时间优选为0.1-200秒。应该意识到最佳接触时间随着烃类化合物的折射特性而增大。因此,在所应用的反应条件下是固态的烃类化合物通常比在所应用的反应条件下是液态的烃类化合物需要更长的接触时间,和液态化合物通常比气态化合物需要更长的接触时间。
可将液态补充硫连续供应至反应区域。替代地,将反应区域中的元素硫定期更新。通常液态硫的量占总反应器体积的10-90体积%,优选20-80体积%,更优选30-70体积%。
本发明的方法在350-750℃、优选400-700℃、更优选400-650℃、特别是500-550℃的温度下进行。
反应物在足以维持液态元素硫相的压力下互相反应。因此,压力主要取决于反应温度。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)。
在本发明的方法中,形成了主要包含二硫化碳、硫化氢和元素硫的气相。当使用气态烃类化合物时,气相通常还包含未转化的烃类化合物。
优选地,本发明的方法另外包括从反应区域采出含二硫化碳和硫化氢的气相,和将至少部分所述气相冷凝以获得含二硫化碳的液态物流。
如果反应区域的流出物是混合的液态和气态流出物,例如可能是当将液态进料供应至反应区域时的情况,则首先在气-液分离器中分离流出物的气相和液相。
可将采出的气相冷凝以获得含二硫化碳的液态物流。优选地,将气相进行顺序部分冷凝步骤以获得含有更高二硫化碳浓度的液态物流。为了获得具有所需组成的含二硫化碳的液态物流,也可使用除冷凝步骤以外的纯化步骤。
优选地,首先将从反应区域采出的气相在超大气压力下冷却至元素硫冷凝而二硫化碳和其它组分保留在贫硫气相中的温度。随后可将冷凝的硫再循环至反应区域。可将贫硫气相冷凝以获得含二硫化碳的液态物流。应该意识到含二硫化碳的液态物流的所需组成决定所需的冷凝和/或另外的纯化步骤。对于二硫化碳的常规用途例如二硫化碳用作生产人造丝的原料或用作溶剂,需要高纯度的二硫化碳。如果液态物流用于强化油采收,即将液态物流注入油储层以从该储层提升油的产量,则液体二硫化碳物流可包含大量的其它组分例如硫化氢和烃类化合物。
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,因为所述液态物流通常包含在该应用中无需移除的二硫化碳之外的组分。因此,本发明的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。在将含二硫化碳的液态物流注入油储层中之前,可将含二硫化碳的液态物流与其它液体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还包含溶解于二硫化碳中的硫化氢,该硫化氢的浓度以二硫化碳的重量计通常为0.1-66wt%。这种含二硫化碳和硫化氢的液态物流特别适用于强化油采收。因此,本发明另外提供可根据本发明方法获得的包含二硫化碳和硫化氢的液态物流用于强化油采收的用途。
具体实施方式
实施例
在石英反应器管(内径12mm,长度40mm)中装入一定量的粉末元素硫。用氮气流将反应器的压力升高到10巴(绝压),和将反应器加热至高于400℃的反应温度。在反应温度下,用高度为15cm的液态硫柱填充反应器管。将含烃(甲烷或乙烷)的气体混合物供应至反应器的底部。在反应器的顶部,采出气体流出物。通过气相色谱分析气体流出物的组成。进行了7次不同的实验。
在下表中,给出了实验1-7的反应条件和结果。
Claims (10)
1.一种制备二硫化碳的方法,所述方法包括:将含烃类化合物的进料供应至含液态元素硫相的反应区域,和在350-750℃的温度下、3-200巴(绝压)的压力下、不存在催化剂以及不存在氧分子的条件下于液态硫相中使烃类化合物与元素硫反应。
2.权利要求1的方法,其中所述含烃类化合物的进料在反应器下端加入液态硫中。
3.权利要求1或2的方法,其中所述烃类化合物是在反应条件下为气态的化合物。
4.权利要求1-3任一项的方法,其中所述烃类化合物是烃,优选饱和或不饱和脂族烃,更优选含有至多20个碳原子的脂族烃,更优选含有至多4个碳原子的饱和脂族烃。
5.前述权利要求任一项的方法,其中反应区域中的温度是400-700℃,优选400-650℃。
6.前述权利要求任一项的方法,其中反应区域中的压力为3-200巴(绝压),优选5-100巴(绝压),更优选5-30巴(绝压)。
7.前述权利要求任一项的方法,另外包括从反应区域采出含二硫化碳和硫化氢的气相,和将至少部分所述气相冷凝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以强化油采收。
9.可通过权利要求7的方法获得的含二硫化碳和硫化氢的液态物流用于强化油采收的用途。
10.使用通过权利要求1-7任一项的方法制得的任选与硫化氢组合的二硫化碳强化油采收的方法。
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Application Number | Priority Date | Filing Date | Title |
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EP06114011.7 | 2006-05-16 | ||
EP06114011 | 2006-05-16 | ||
PCT/EP2007/054610 WO2007131976A1 (en) | 2006-05-16 | 2007-05-14 | A process for the manufacture of carbon disulphide |
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CN101443269A true CN101443269A (zh) | 2009-05-27 |
CN101443269B CN101443269B (zh) | 2012-06-27 |
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CN2007800176223A Expired - Fee Related CN101443269B (zh) | 2006-05-16 | 2007-05-14 | 制备二硫化碳的方法 |
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US (1) | US20090155159A1 (zh) |
EP (1) | EP2018349A1 (zh) |
CN (1) | CN101443269B (zh) |
AU (1) | AU2007251608A1 (zh) |
BR (1) | BRPI0711058A2 (zh) |
CA (1) | CA2651953A1 (zh) |
EA (1) | EA014708B1 (zh) |
MX (1) | MX2008014282A (zh) |
NO (1) | NO20085244L (zh) |
WO (1) | WO2007131976A1 (zh) |
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US8136590B2 (en) | 2006-05-22 | 2012-03-20 | Shell Oil Company | Systems and methods for producing oil and/or gas |
CN101489930A (zh) | 2006-07-07 | 2009-07-22 | 国际壳牌研究有限公司 | 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 |
CN101501295B (zh) | 2006-08-10 | 2013-11-20 | 国际壳牌研究有限公司 | 用于生产油和/或气的方法 |
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WO2009012374A1 (en) | 2007-07-19 | 2009-01-22 | Shell Oil Company | Methods for producing oil and/or gas |
WO2009058846A1 (en) | 2007-10-31 | 2009-05-07 | Shell Oil Company | Systems and methods for producing oil and/or gas |
CN101861445B (zh) | 2007-11-19 | 2014-06-25 | 国际壳牌研究有限公司 | 生产油和/或气的系统与方法 |
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CN102046917B (zh) | 2008-04-16 | 2014-08-13 | 国际壳牌研究有限公司 | 生产油和/或气的系统与方法 |
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-
2007
- 2007-05-14 AU AU2007251608A patent/AU2007251608A1/en not_active Abandoned
- 2007-05-14 WO PCT/EP2007/054610 patent/WO2007131976A1/en active Application Filing
- 2007-05-14 CN CN2007800176223A patent/CN101443269B/zh not_active Expired - Fee Related
- 2007-05-14 EP EP07729062A patent/EP2018349A1/en not_active Withdrawn
- 2007-05-14 CA CA002651953A patent/CA2651953A1/en not_active Abandoned
- 2007-05-14 US US12/300,759 patent/US20090155159A1/en not_active Abandoned
- 2007-05-14 MX MX2008014282A patent/MX2008014282A/es unknown
- 2007-05-14 BR BRPI0711058-8A patent/BRPI0711058A2/pt not_active IP Right Cessation
- 2007-05-14 EA EA200802327A patent/EA014708B1/ru not_active IP Right Cessation
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2008
- 2008-12-15 NO NO20085244A patent/NO20085244L/no not_active Application Discontinuation
Also Published As
Publication number | Publication date |
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EP2018349A1 (en) | 2009-01-28 |
EA200802327A1 (ru) | 2009-04-28 |
MX2008014282A (es) | 2008-11-18 |
CN101443269B (zh) | 2012-06-27 |
BRPI0711058A2 (pt) | 2011-08-23 |
US20090155159A1 (en) | 2009-06-18 |
CA2651953A1 (en) | 2007-11-22 |
EA014708B1 (ru) | 2011-02-28 |
WO2007131976A1 (en) | 2007-11-22 |
AU2007251608A1 (en) | 2007-11-22 |
NO20085244L (no) | 2008-12-15 |
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