Name: measurement of the rheology of crude oil in equilibrium with co2 at reservoir conditions
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作者衷心感谢卡塔尔碳酸盐和碳储存研究中心（QCCSRC）的资助，由卡塔尔石油，壳牌和卡塔尔科技园共同提供。作者感谢Frans van den Berg（壳牌全球解决方案，荷兰阿姆斯特丹）提供原油样品。

注意:由于实验在高温和高压下运行，所以安全至关重要。该系统通过注射泵控制器上的软件限制和混合器以及齿轮泵和流变仪之间的破裂盘（ 见图1和图2 ）来防止过压。此外，在每个实验之前，建议进行定期的泄漏检查。还建议对压力传感器几何进行摩擦检查，以确保流变仪运行良好9,10 。 1.准备原油样品注意:使用Zuata原油样品。下表显示了祖塔原油的基本物理性质。 <table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always"><tbody><tr><td>查racteristics </td><td>值</td></tr><tr><td> API重力</td><td> 9.28 </td></tr><tr><td>桶因子（bbl / t） </td><td> 6.27 </td></tr><tr><td>总硫（％wt） </td><td> 3.35 </td></tr><tr><td>里氏蒸气压（kPa） </td><td> 1 </td></tr><tr><td>倾点（°C） </td><td> 24 </td></tr><tr><td>现有H 2 S含量（ppm） </td><td> - </td></tr><tr><td>潜在H 2 S含量（ppm） </td><td> 115 </td></tr><tr><td>潜在的HCl含量（ppm） </td><td> - </td></tr><tr><td>计算器。总卡尔价值（kJ / kg） </td><td> 41855 </td></tr></tbody></table> 表1:祖塔原油的物理性质。 <ol><li>向300g Zuata原油中加入128.57g甲苯以制备用70wt％Zuata原油和30wt％甲苯稀释。将混合物在室温下摇匀3小时。 </li></ol> 2.将原油样品装入搅拌机<ol><li>断开混音器与系统的连接，并将其打开。在搅拌机的底部放置搅拌器。将200 mL原油样品装入搅拌机。拧紧所有螺丝后，将搅拌机连接到系统。 </li></ol> 3.用原油样品启动整个系统<ol><li> 用同轴圆柱体几何形状的压力单元来引导系统。 注意:请参考图1找到阀门。 <ol><li>通过拧紧压头9关闭流变仪压力传感器。将旋转杯安装在流变仪主轴上。调整到测量位置9 。 </li><li>关闭阀门A，D，E，F，G和H.打开阀门C. </li><li>打开氮气瓶。通过打开H和E阀将压缩气体引入混合器。当气体到达混合器时，关闭阀H和气瓶。 </li><li>打开阀A.压缩气体将原油样品通过吸管推入循环回路。当原油样品从图1中的阀C滴落时，整个系统由原油样品引发。 </li><li>打开阀门F释放剩余气体。关闭阀门C和打开阀门D.打开齿轮泵使流体循环一段时间。根据原油样品的粘度，可能需要1〜5小时。 注意:引入混合器的压缩氮气的压力取决于原油样品的粘度。如果原油样品的粘度超过5Pa·s，则压缩气体的压力可能大于15巴。 </li></ol></li><li> 使用双间隙几何压力池来填充系统。 注意:请参考图2找到阀门。 <ol><li>删除t他的压头和压力单元的量筒。 </li><li>关闭阀门A，D，E，F，G，H和I.打开阀门C. </li><li>打开氮气瓶。通过打开H和E阀将压缩气体引入混合器。当气体到达混合器时，关闭阀H和气瓶。 </li><li>打开阀A.压缩气体将原油样品通过吸管推入循环回路。当原油样品刚刚浸入双间隙几何形状的内部时，打开阀门F以释放混合器中的压力。 </li><li>打开齿轮泵。仔细调整齿轮泵的转速。确保通过齿轮泵确定的压力单元的入口流量小于或等于由重力确定的压力单元的出口流量。当发现齿轮泵的合理旋转速度并且原油样品从阀C滴落时，整个系统由油引发。 Ť母鸡关掉齿轮泵。 </li><li>将量筒和压头安装在压力单元10上 。关闭阀门C和打开阀门D.打开齿轮泵使流体循环。 注意:如果原油样品的粘度与水相似，则压力为3至4巴的压缩气体就足够了。 </li></ol></li></ol> 4.撤出系统剩余量<ol><li>关闭图1或图2中的阀门A和D。将真空泵连接到阀F.将真空泵打开15分钟。 </li><li>关闭阀门F，然后关闭真空泵。 </li></ol> 5.将CO 2引入搅拌机<ol><li> 同轴圆柱体几何压力单元 <ol><li>打开阀门G和图 2中的二氧化碳气瓶。打开图1中的阀门D。 </<html> LI&gt; <li>在CO 2填充系统中的剩余空间之后，关闭阀G和CO 2气缸，以防止CO 2回流到气缸。 </li></ol></li><li> 具有双间隙几何压力单元 <ol><li>打开阀门G和图2中的二氧化碳气瓶。打开图2中的阀D和I。 </li><li>在CO 2填充系统中的剩余空间之后，关闭阀G和CO 2气缸，以防止CO 2回流到气缸。 </li></ol></li></ol> 6.设定温度和压力<ol><li>将混合器和流变仪输入所需的温度值。输入管道网络加热系统所需的温度值。向注射泵输入所需的压力值。 </li><li>等待温度和压力稳定。 </li></ol>jove_title"&gt; 7。打开搅拌器和齿轮泵<ol><li>打开齿轮泵下游和上游的阀门。 </li></ol> 8.监测混合器中的体积和混合物的粘度<ol><li>每6小时记录一次注射泵的体积读数。 </li><li>每6小时一次，关闭搅拌器和齿轮泵。通过流变仪测量混合物的粘度。粘度测定以5分钟沉降时间开始，然后在10s -1的恒定剪切速率下测量粘度。 </li><li>当两次测量结果之间的体积和粘度值显示出相当大的差异（&gt; 4％）时，再次打开齿轮泵和搅拌器以继续混合。当体积和粘度测量值都不显示值（≤4％）时，确认了CO 2和原油样品之间的平衡。 </li><li>关闭齿轮泵和搅拌器进行流变测量。 注意:混合期可以持续1至2天，这取决于原油样品的粘度。 </li></ol> 9.进行流变学测量<ol><li> 同轴圆柱体几何压力单元9 <ol><li>关闭图1中的阀A和D进行流变测量。以10s -1的剪切速率对混合物预剪切0.5分钟。将混合物放置1分钟。 </li><li>在500 s -1至10 s -1的剪切速率下测量混合物的粘度。在每个剪切速率下，剪切速率调节时间为0.2分钟。每个剪切速率步长的测量持续时间从0.5分钟对数增加到1分钟，不包括剪切速率调整时间。 </li></ol></li><li> 具有双间隙几何压力单元10 <ol><li>关闭图2中的阀A和D进行流变测量。预剪混合物的剪切速率为10s -1 ，持续0.5分钟。将混合物放置1分钟。 </li><li>测量剪切速率下的混合物粘度为250s -1至10s -1 。在每个剪切速率下，剪切速率调节时间为0.2分钟。每个剪切速率步长的测量持续时间从0.5分钟对数增加到1分钟，不包括剪切速率调整时间。 </li></ol></li></ol> 10.将压力提高到下一个所需值<ol><li> 同轴圆柱体几何压力单元 <ol><li>关闭图1中的阀门E。 </li><li>通过打开阀G和CO 2气缸，将更多的CO 2引入注射泵。关闭阀G和CO 2气缸。打开阀门E以将更多的CO 2加入搅拌机。 </li><li>如果压力小于所需值，重复引入更多的二氧化碳。 </li><li>输入新的压力波int进入注射泵。等待压力稳定。 </li></ol></li><li> 具有双间隙几何压力单元 <ol><li>关闭图2中的阀门E和I。 </li><li>通过打开阀G和CO 2气缸，将更多的CO 2引入注射泵。关闭阀G和CO 2气缸。打开阀门E和I，以便在混合器中加入更多的二氧化碳。 </li><li>如果压力小于所需值，重复步骤以引入更多的二氧化碳。 </li><li>将新的压力设定点输入注射器泵。等待压力稳定。 注意:在较高压力下重复步骤7至10进行流变测量。 </li></ol></li></ol>

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作者没有什么可以披露的。

两个步骤在操作中至关重要。第一个是由原油样品引发整个系统。通过用原油样品填充系统，齿轮泵可以通过油样进行良好润滑，并且可以容易地识别循环回路中的任何堵塞。因此，可以防止齿轮泵的损坏。第二个关键步骤是定期监测混合物的粘度，以确认CO 2和原油之间的平衡。鉴于CO 2和粘性重质原油16之间的平衡需要相当长的时间，进行流变学测量太早将低估CO 2加入对油粘度的影响。因此，只有当测得的粘度达到恒定值（小于4％的变化）时，才能将混合物视为与CO 2平衡。 目前的测量系统允许CO 2饱和混合物的流变学测量。为了测量不足饱和的混合物，可以将上游容器引入CO 2流中。首先将CO 2引入上游容器，然后从源分离，使得CO 2的量可以通过上游容器中的体积和压力来控制。在这种情况下，系统的总压力将由惰性气体如氦气控制。 Kariznovi 等人对用于测量CO 2和重质原油混合物17的物理性能的装置提供了良好的综述。修改可以参考他们论文中审查的系统。 应该提到的是，这里描述的系统可以测量任何气液混合物的流变性;因此其应用不限于原油。例如，它可以用于测量rh对二氧化碳的影响Pickering乳液18,19的气味和气体诱导的增塑6 。通过将电导率测量装置引入到流变仪压力池中，也可以研究气体溶解对乳液的剪切诱导相转化的影响20,21,22,23。

在关于CO 2和原油混合物的物理性质的大多数文献中，使用粘度计测量粘度，这意味着测量是在恒定剪切速率或剪切应力下进行的。在这些研究中，以简单的方式研究了CO 2和原油混合物的粘度:感兴趣的焦点是粘度与其他参数（如温度，压力和二氧化碳浓度）之间的关系。这些研究中提出的关键假设，但很少提到明确的是，二氧化碳和原油混合物表现为牛顿流体。然而，众所周知，一些原油，特别是重质原油，可以在某些条件1,2,3,4中显示非牛顿行为。因此，要充分了解二氧化碳的影响，二氧化碳的粘度</sub&gt;和原油混合物应作为剪切速率或应力的函数进行研究。 据我们所知，只有Behzadfar 等人的研究报告使用流变仪5以不同剪切速率加入CO 2的重质原油的粘度。在Behzadfar 等人的测量中，CO 2和原油之间的混合通过同轴圆柱体几何形状的内圆筒的旋转来实现，这是非常缓慢的过程。此外，在文献中已经报道了CO 2溶解对聚合物熔体流变性的影响，这可以揭示重质原油和CO 2混合物的研究。 Royer 等使用高压挤出狭缝模具流变仪6测量三种商业聚合物熔体在各种压力，温度和CO 2浓度下的粘度。然后他们通过自由体积分析数据<html> e理论其他类似的研究可以在Gerhardt 等人 7和Lee 等 8 。我们的方法是在外部混合器中进行混合，同轴圆筒几何形状的流变学测量可以更全面地测量二氧化碳和原油混合物的流变性。 我们开发的循环系统包括四个单元:注射泵，搅拌机，齿轮泵和流变仪， 如图1和图2所示 。将搅拌棒放置在混合器的底部并与旋转的磁铁组磁耦合。搅拌器用于增强混合器中CO 2和原油之间的混合，加快了相间平衡的进行。 CO 2饱和油相使用汲取管从混合器的底部附近排出并循环通过测量系统。 <html>粘度通过安装在流变仪上的高压电池测量，有两种类型的压力单元，一种是同轴圆柱体几何形状，用于测量粘性流体;另一种是带有用于低粘度应用的双间隙几何。 <img alt="图1" class="xfigimg" src="/files/ftp_upload/55749/55749fig1.jpg" /> 图1:具有同轴圆柱体几何压力单元的循环系统方案。蓝线表示CO 2流，黑线表示原油混合物。转载自胡等人的许可14 。版权所有2016美国化学学会。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig1large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> e 2"class ="xfigimg"src ="/ files / ftp_upload / 55749 / 55749fig2.jpg"/&gt; 图2:具有双间隙几何压力池的循环系统的方案。蓝线表示CO 2流，黑线表示原油混合物。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig2large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图3" class="xfigimg" src="/files/ftp_upload/55749/55749fig3.jpg" /> 图3:同轴圆柱体几何压力单元。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig3large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> 同轴圆柱体几何压力单元（ 图3 ）内外圆柱之间的间隙为0.5 mm，样品体积为18毫升。内圆筒与旋转杯磁耦合，旋转杯连接到流变仪主轴。在内筒的顶部和底部有两个蓝宝石轴承，它们直接与内筒的旋转轴接触。由于蓝宝石轴承通过设计暴露于样品，所以轴承摩擦力可能会根据样品的润滑性能而变化。 <img alt="图4" class="xfigimg" src="/files/ftp_upload/55749/55749fig4.jpg" /> 图4:双间隙几何压力单元。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig4large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> 另一方面，双间隙压力单元包括双重间隙几何形状的圆柱形转子， 如图4所示 。安装量筒在压头上通过两个滚珠轴承并与旋转杯磁耦合，该旋转杯连接到流变仪主轴。滚珠轴承位于压头内部，不与样品接触，样品被注入到测量间隙中并溢出到定子中的凹部中，从而将其返回到混合容器中。 在典型的实验中，首先将原油样品装入混合器中。在用原油灌注整个系统之后，使用真空泵抽空系统中的剩余体积。然后通过注射泵将CO 2引入混合器中，并使系统达到所需的温度和压力。系统压力由注射泵通过CO 2相控制。当压力稳定时，打开搅拌器以将混合器内的CO 2和原油混合。然后齿轮泵打开，从中抽出油相混合器，填充流变仪并将流体再循环回混合器。因此，CO 2和原油之间的混合通过在混合器中同时搅拌并在循环中循环进行。通过对注射泵中的体积和混合物粘度的周期性测量来监测平衡状态。当体积和粘度均无变化（≤4％）时，确认平衡。在该阶段，齿轮泵和搅拌器被关闭，将流动悬浮在测量单元上并进行流变学测量。

<table><tbody><tr><td>Heavy Crude Oil</td><td>Shell</td><td>N/A</td><td>Produced from the Zuata oil flied. Used without further treatment</td></tr><tr><td>Toluene</td><td>Sigma-Aldrich</td><td>244511-2L</td><td>Anhydrous, 99.8%. Used without further treatment</td></tr><tr><td>CO&lt;sub&gt;2&lt;/sub&gt;</td><td>BOC</td><td>111304-F</td><td>CP Grade. Used without further treatment</td></tr><tr><td>&lt;strong&gt;Name&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>Syringe Pump</td><td>Teledyne ISCO</td><td>65D</td><td></td></tr><tr><td>Mixer</td><td>Parr Instruments</td><td>4651</td><td>Vessel volume 250 mL. Mounted on a series 4923EE bench-top heater</td></tr><tr><td>Gear Pump 1</td><td>Polymer Systems Inc.</td><td>CIP-12/1.5</td><td>Used with CC29/Pr pressure cell for high viscosity fluids.</td></tr><tr><td>Gear Pump 2</td><td>Micropump</td><td>GAH X21</td><td>Used with DG35.12/Pr pressure cell for low viscosity fluids.</td></tr><tr><td>Rheometer</td><td>Anton Paar</td><td>MCR301</td><td></td></tr><tr><td>Pressure cell 1</td><td>Anton Paar</td><td>CC29/Pr</td><td>With flow-through configuration. Used for high viscosity fluids. Coaxial cylinder geometry</td></tr><tr><td>Pressure cell 2</td><td>Anton Paar</td><td>DG35.12/Pr</td><td>With flow-through configuration. Used for low viscosity fluids. Double gap geometry</td></tr></tbody></table>

measurement of the rheology of crude oil in equilibrium with co2 at reservoir conditions

描述了在高温和高压下测量与二氧化碳（CO 2 ）平衡的原油流变性的流变仪系统。该系统包括连接到循环回路的高压流变仪。流变仪具有旋转流通测量单元，具有两个替代几何形状:同轴圆柱体和双间隙。循环回路包含混合器，使原油样品与CO 2平衡;以及齿轮泵，将混合物从混合器输送到流变仪，并将其再循环回混合器。通过搅拌和循环使CO 2和原油达到平衡，并通过流变仪测量饱和混合物的流变性。该系统用于测量Zuata原油（及其甲苯稀释度）在高达220巴的升高压力和50℃的温度下与CO 2平衡的流变性能。结果显示t帽子CO 2添加剂显着改变油流变性，最初在CO 2压力增加时降低粘度，然后将粘度增加到阈值压力以上。原油的非牛顿反应也随着加入二氧化碳而变化。

图5和图6显示了使用同轴圆柱体几何形状压力池在50℃下的Zuata原油及其CO 2饱和混合物的流变学测量。 图5显示了从环境到100巴的测量，而图6显示了从120巴到220巴的测量。此外， 图7示出了相对粘度，其是给定剪切速率下的粘度与最低剪切速率下的粘度的比率。 图7中的虚线是由几何轴承的摩擦引起的最大测量误差。 使用双间隙几何压力池，稀释的Zuata原油在50℃下的流变学测量是i如图8和图9所示 ，而图10示出了压力高达70巴的相对粘度。此外， 图10显示在环境压力下的稀释的原油表现为牛顿流体。然而，当CO 2压力为30巴至60巴时，观察到剪切变稀效应。在CO 2压力高于60巴时，剪切变稀消失，混合物再次作为牛顿流体。 从图5和图6可以看出，CO 2溶出显着降低了原油混合物的粘度直到100巴。当CO 2压力超过100巴时，油混合物粘度随着CO 2压力的增加而增加，但速度要低得多。 <pclass ="jove_content"fo:keep-together.within-page ="1"&gt; 图7显示，Zuata原油显示出没有加入CO 2的剪切变稀效应。当CO 2溶解在原油中时，由于较高CO 2压力下的曲线较平坦，剪切变稀效应减弱。在高于40巴的CO 2压力下，剪切速率的粘度变化在测量误差范围内，因此混合物可以认为是牛顿式。 CO 2溶解减弱，最终消除了Zuata原油的剪切稀化效应。这表明溶解在原油中的CO 2分子最终会破坏由原油中的大分子产生的缔合网络，如沥青质。 关于稀释的原油， 如图8所示 ，CO 2 ad大大降低了油混合物的粘度至70巴。当CO 2压力增加超过70巴（ 图9 ）时，较高的CO 2压力导致油粘度的增加。 根据Seifried 等人的研究11 ，在原始和稀释的祖塔原油中，沥青质沉淀的发生发生在80巴以上的CO 2压力下。然而，在压力高于80巴的流变学实验中，原油/二氧化碳混合物表现为牛顿流体。这意味着沥青质沉淀不会改变该混合物的流变性能。 稀释的原油的流变学结果也很有趣:在这种情况下，二氧化碳溶解引起非牛顿行为，只有应用程序耳朵处于一定范围的二氧化碳压力。这里给出了由CO 2添加引起的剪切稀化效应的两种推测。 第一个猜测是非牛顿行为是由二氧化碳溶解下沥青质分子形成的胶束引起的。溶解在原油中的CO 2可以通过其对沥青质聚集体的结构的作用来降低系统的临界胶束浓度（CMC），并且这可导致胶束12之间更大的相互作用。在30至60巴的压力下，沥青质胶束之间的距离可能在范德华力吸引力13的有效范围内。因此，在胶束之间形成缔合网络并引起剪切变稀效应。然而，当压力高于60巴时，CO 2对溶剂或非沥青质分子的影响是主要的导致CMC增加。因此，沥青质胶束不稳定，相应的联网消失。 第二个猜测是基于相位行为的观点。在CO 2压力30至60巴之间，可能产生富含CO 2的液相，这使混合物形成液 - 液 - 蒸气（LLV）系统。这两种液体的乳液可以通过搅拌和循环的混合形成，这是由于两个液相的密度相似。作为乳液的分散相，富CO 2的液相可以通过原油中的沥青质而稳定。该乳液显示出非牛顿行为，因为分散相产生联结网络。然而，当在高于60巴的压力下更多的CO 2溶解到油混合物中时，两个液相再次变得混溶。结果是一个<html>液体蒸汽（LV）系统由富含CO 2的蒸气平衡的富油液体和富油的液相组成，表现为牛顿流体。 <img alt="图5" class="xfigimg" src="/files/ftp_upload/55749/55749fig5.jpg" /> 图5. Zoata重质原油与CO 2在50℃和各种剪切速率下的粘度测量。 <img alt="方程" src="/files/ftp_upload/55749/55749_2RedDash.jpg" /> ，剪切速率下限; <img alt="方程" src="/files/ftp_upload/55749/55749_dRedDot.jpg" /> ， 周围; <img alt="方程" src="/files/ftp_upload/55749/55749_lRedDot.jpg" /> ，20巴; <img alt="方程" src="/files/ftp_upload/55749/55749_orangeDot.jpg" /> ，40巴; <img alt="方程" src="/files/ftp_upload/55749/55749_yellowDot.jpg" /> ，60巴<img alt="方程" src="/files/ftp_upload/55749/55749_greenDot.jpg" /> ，80巴;<html> ftp_upload / 55749 / 55749_dGreenDot.jpg"/&gt;，100 bar。经Hu 等人许可转载15。版权所有2016美国化学学会<a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig5large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图6" class="xfigimg" src="/files/ftp_upload/55749/55749fig6.jpg" /> 图6.在50℃和各种剪切速率下，二氧化碳的Zuata重质原油的粘度测量。 <img alt="方程" src="/files/ftp_upload/55749/55749_2RedDash.jpg" /> ，剪切速率下限; <img alt="方程" src="/files/ftp_upload/55749/55749_purpleDot.jpg" /> ，120巴; <img alt="方程" src="/files/ftp_upload/55749/55749_dRedDot.jpg" /> ，140巴; <img alt="方程" src="/files/ftp_upload/55749/55749_lRedDot.jpg" /> ，160巴;/ /，180吧; 5749 / 55749_orangeDot.jpg <img alt="方程" src="/files/ftp_upload/55749/55749_yellowDot.jpg" /> ，200巴; <img alt="方程" src="/files/ftp_upload/55749/55749_greenDot.jpg" /> ，220巴。转载自胡等人的许可15 。版权所有2016美国化学学会。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig6large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图7" class="xfigimg" src="/files/ftp_upload/55749/55749fig7.jpg" /> 图7. Zaata原油在50℃和各种剪切速率下的CO 2的相对粘度。 - - ，测量波动范围; <img alt="方程" src="/files/ftp_upload/55749/55749_dRedDot.jpg" /> ，环境压力<img alt="方程" src="/files/ftp_upload/55749/55749_lRedDot.jpg" /> ，20巴; <img alt="方程"<html> / src ="/ files / ftp_upload / 55749 / 55749_orangeDot.jpg"/&gt;，40 bar; <img alt="方程" src="/files/ftp_upload/55749/55749_yellowDot.jpg" /> ，60巴<img alt="方程" src="/files/ftp_upload/55749/55749_greenDot.jpg" /> ，80巴; <img alt="方程" src="/files/ftp_upload/55749/55749_dGreenDot.jpg" /> ，100巴<img alt="方程" src="/files/ftp_upload/55749/55749_dRedX.jpg" /> ，120巴; <img alt="方程" src="/files/ftp_upload/55749/55749_lRedX.jpg" /> ，140巴; <img alt="方程" src="/files/ftp_upload/55749/55749_orangeX.jpg" /> ，160巴; <img alt="方程" src="/files/ftp_upload/55749/55749_yellowX.jpg" /> ，180巴<img alt="方程" src="/files/ftp_upload/55749/55749_greenX.jpg" /> ，220巴。转载自胡等人的许可15 。版权所有2016美国化学学会。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig7large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <html> e_content"fo:keep-together.within-page ="1"&gt; <img alt="图8" class="xfigimg" src="/files/ftp_upload/55749/55749fig8.jpg" /> 图8.稀释的原油与CO 2在50℃和各种剪切速率下的粘度测量。 <img alt="方程" src="/files/ftp_upload/55749/55749_2RedDash.jpg" /> ，剪切速率下限; <img alt="方程" src="/files/ftp_upload/55749/55749_dRedDiamond.jpg" /> ，1巴; <img alt="方程" src="/files/ftp_upload/55749/55749_orangeDiamond.jpg" /> ，10巴<img alt="方程" src="/files/ftp_upload/55749/55749_lRedDiamond.jpg" /> ，20巴; <img alt="方程" src="/files/ftp_upload/55749/55749_lGreenDiamond.jpg" /> ，30巴<img alt="方程" src="/files/ftp_upload/55749/55749_dGreenDiamond.jpg" /> ，40巴; <img alt="方程" src="/files/ftp_upload/55749/55749_lBlueDiamond.jpg" /> ，50巴; <img alt="方程" src="/files/ftp_upload/55749/55749_dBlueDiamond.jpg" /> ，60巴d / 55749 / 55749_purpleDiamond.jpg"/&gt;，70 bar。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig8large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图9" class="xfigimg" src="/files/ftp_upload/55749/55749fig9.jpg" /> 图9.稀释的原油与CO 2在50℃和各种剪切速率下的粘度测量。 <img alt="方程" src="/files/ftp_upload/55749/55749_2RedDash.jpg" /> ，剪切速率下限; <img alt="方程" src="/files/ftp_upload/55749/55749_dRedX.jpg" /> ，80巴; <img alt="方程" src="/files/ftp_upload/55749/55749_orangeX.jpg" /> ，100巴<img alt="方程" src="/files/ftp_upload/55749/55749_lRedX.jpg" /> ，120巴; <img alt="方程" src="/files/ftp_upload/55749/55749_lGreenX.jpg" /> ，140巴; <img alt="方程" src="/files/ftp_upload/55749/55749_greenX.jpg" /> ，160巴; <img alt="方程"<html> / src ="/ files / ftp_upload / 55749 / 55749_lBlueX.jpg"/&gt;，180 bar; <img alt="方程" src="/files/ftp_upload/55749/55749_dBlueX.jpg" /> ，200巴; <img alt="方程" src="/files/ftp_upload/55749/55749_purpleX.jpg" /> ，220巴。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig9large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图10" class="xfigimg" src="/files/ftp_upload/55749/55749fig10.jpg" /> 图10.在50℃和各种剪切速率下CO 2的稀释原油的相对粘度。 - - ，测量波动范围; <img alt="方程" src="/files/ftp_upload/55749/55749_dRedDiamond.jpg" /> ，1巴; <img alt="方程" src="/files/ftp_upload/55749/55749_orangeDiamond.jpg" /> ，10巴<img alt="方程" src="/files/ftp_upload/55749/55749_lRedDiamond.jpg" /> ，20巴;tp_upload / 55749 / 55749_lGreenDiamond.jpg"/&gt;，30 bar; <img alt="方程" src="/files/ftp_upload/55749/55749_dGreenDiamond.jpg" /> ，40巴; <img alt="方程" src="/files/ftp_upload/55749/55749_lBlueDiamond.jpg" /> ，50巴; <img alt="方程" src="/files/ftp_upload/55749/55749_dBlueDiamond.jpg" /> ，60巴<img alt="方程" src="/files/ftp_upload/55749/55749_purpleDiamond.jpg" /> ，70吧。 <a href="http://ecsource.jove.com/files/ftp_upload/55749/55749fig10large.jpg" target="_blank">请点击此处查看此图的较大版本。</a>

Watch this Scientific Journal Video about Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions at JoVE.com

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

提出了一种在储层条件下测量与二氧化碳平衡的原油流变性的方法。

与CO平衡的原油流变学测量<sub&gt; 2</sub&gt;在水库条件

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The ...

measurement-rheology-crude-oil-equilibrium-with-co2-at-reservoir

Nanyang Technological University

Research

JoVE Journal

Environment

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

12.7K 次观看.  Imperial College London, Qatar Carbonate and Carbon Storage Research Centre. 提出了一种在储层条件下测量与二氧化碳平衡的原油流变性的方法。 

视频: Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

Measuring Carbon-based Contaminant Mineralization Using Combined CO2 Flux and Radiocarbon Analyses

A method is described which uses the absence of radiocarbon in industrial chemicals and fuels made from petroleum feedstocks which frequently contaminate the environment. This radiocarbon signal &#8212; or rather the absence of signal &#8212; is evenly distributed throughout a contaminant source pool (unlike an added tracer) and is not impacted by biological, chemical or physical processes (e.g., the 14C radioactive decay rate is immutable). If the fossil-derived contaminant is fully degraded to CO2, a harmless end-product, that CO2 will contain no radiocarbon. CO2 derived from natural organic matter (NOM) degradation will reflect the NOM radiocarbon content (usually &#60;30,000 years old). Given a known radiocarbon content for NOM (a site background), a two end-member mixing model can be used to determine the CO2 derived from a fossil source in a given soil gas or groundwater sample. Coupling the percent CO2 derived from the contaminant with the CO2 respiration rate provides an estimate for the total amount of contaminant degraded per unit time. Finally, determining a zone of influence (ZOI) representing the volume from which site CO2 is collected allows determining the contaminant degradation per unit time and volume. Along with estimates for total contaminant mass, this can ultimately be used to calculate time-to-remediate or otherwise used by site managers for decision-making.

Measuring Carbon-based Contaminant Mineralization Using Combined CO2 Flux and Radiocarbon Analyses

A protocol is described wherein CO2 mineralized from organic contaminant (derived from petroleum feedstocks) biodegradation is trapped, quantified, and analyzed for 14C content. A model is developed to determine CO2 capture zone's spatial extent. Spatial and temporal measurements allow integrating contaminant mineralization rates for predicting remediation extent and time.

测量碳为基础的污染物矿化结合使用CO<sub&gt; 2</sub&gt;助焊剂和放射性碳分析

A method is described which uses the absence of radiocarbon in industrial chemicals and fuels made from petroleum feedstocks which frequently contaminate ...

科研

环境科学

Reservoir Condition Pore-scale Imaging of Multiple Fluid Phases Using X-ray Microtomography

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space of a carbonate rock at pressures and temperatures representative of typical formations used for CO2 storage. Chemical equilibrium between the CO2, brine and rock phases was maintained using a high pressure high temperature reactor, replicating conditions far away from the injection site. Fluid flow was controlled using high pressure high temperature syringe pumps. To maintain representative in-situ conditions within the micro-CT scanner a carbon fiber high pressure micro-CT coreholder was used. Diffusive CO2 exchange across the confining sleeve from the pore-space of the rock to the confining fluid was prevented by surrounding the core with a triple wrap of aluminum foil. Reconstructed brine contrast was modeled using a polychromatic x-ray source, and brine composition was chosen to maximize the three phase contrast between the two fluids and the rock. Flexible flow lines were used to reduce forces on the sample during image acquisition, potentially causing unwanted sample motion, a major shortcoming in previous techniques. An internal thermocouple, placed directly adjacent to the rock core, coupled with an external flexible heating wrap and a PID controller was used to maintain a constant temperature within the flow cell. Substantial amounts of CO2 were trapped, with a residual saturation of 0.203 &#177; 0.013, and the sizes of larger volume ganglia obey power law distributions, consistent with percolation theory.

We present a methodology for the imaging of multiple fluid phases at reservoir conditions by the use of x-ray microtomography. We show some representative results of capillary trapping in a carbonate rock sample.

多重流体相储层孔隙条件级成像使用X射线微断层

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space ...

工程学

Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system requires the careful preparation of the sample in order to accurately replicate the natural formation of the water-accommodated fraction that occurs in nature. Low-energy water-accommodated fractions (LEWAF) are carefully prepared by mixing crude oil and water at a set ratio. Aspirator bottles are then irradiated, and at set time points, the water is sampled and extracted using standard techniques. A second challenge is the representative characterization of the sample, which must take into consideration the chemical changes that occur over time. A targeted analysis of the aromatic fraction of the LEWAF can be performed using an atmospheric-pressure laser ionization source coupled to a custom-built trapped ion mobility spectrometry&#8211;Fourier transform&#8211;ion cyclotron resonance mass spectrometer (TIMS-FT-ICR MS). The TIMS-FT-ICR MS analysis provides high-resolution ion mobility and ultrahigh-resolution MS analysis, which further allow the identification of isomeric components by their collision cross-sections (CCS) and chemical formula. Results show that as the oil-water mixture is exposed to light, there is significant photo-solubilization of the surface oil into the water. Over time, the chemical transformation of the solubilized molecules takes place, with a decrease in the number of identifications of nitrogen- and sulfur-bearing species in favor of those with a greater oxygen content than were typically observed in the base oil.

The low-energy water-accommodated fraction (LEWAF) of crude oil is a challenging system to analyze, because over time, this complex mixture undergoes chemical transformations. This protocol illustrates methods for the preparation of the LEWAF sample and for performing photo-irradiation and chemical analysis by trapped ion mobility spectrometry&#8211;FT-ICR MS.

原油水容纳组分的化学分析泄漏使用TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system ...

Microfluidic Devices for Characterizing Pore-scale Event Processes in Porous Media for Oil Recovery Applications

Microfluidic devices are versatile tools for studying transport processes at a microscopic scale. A demand exists for microfluidic devices that are resistant to low molecular-weight oil components, unlike traditional polydimethylsiloxane (PDMS) devices. Here, we demonstrate a facile method for making a device with this property, and we use the product of this protocol for examining the pore-scale mechanisms by which foam recovers crude oil. A pattern is first designed using computer-aided design (CAD) software and printed on a transparency with a high-resolution printer. This pattern is then transferred to a photoresist via a lithography procedure. PDMS is cast on the pattern, cured in an oven, and removed to obtain a mold. A thiol-ene crosslinking polymer, commonly used as an optical adhesive (OA), is then poured onto the mold and cured under UV light. The PDMS mold is peeled away from the optical adhesive cast. A glass substrate is then prepared, and the two halves of the device are bonded together. Optical adhesive-based devices are more robust than traditional PDMS microfluidic devices. The epoxy structure is resistant to swelling by many organic solvents, which opens new possibilities for experiments involving light organic liquids. Additionally, the surface wettability behavior of these devices is more stable than that of PDMS. The construction of optical adhesive microfluidic devices is simple, yet requires incrementally more effort than the making of PDMS-based devices. Also, though optical adhesive devices are stable in organic liquids, they may exhibit reduced bond-strength after a long time. Optical adhesive microfluidic devices can be made in geometries that act as 2-D micromodels for porous media. These devices are applied in the study of oil displacement to improve our understanding of the pore-scale mechanisms involved in enhanced oil recovery and aquifer remediation.

The goal of this procedure is to easily and rapidly produce a microfluidic device with customizable geometry and resistance to swelling by organic fluids for oil recovery studies. A polydimethylsiloxane mold is first generated, and then used to cast the epoxy-based device. A representative displacement study is reported.

微流体器件用于表征多孔介质中的孔隙尺度事件过程, 用于采油应用

Microfluidic devices are versatile tools for studying transport processes at a microscopic scale. A demand exists for microfluidic devices that are ...

Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve geologic seals and allow CO2 to escape. However, the dissolution processes at reservoir conditions are poorly understood. Thus, time-resolved experiments are needed to observe and predict the nature and rate of dissolution at the pore scale. Synchrotron fast tomography is a method of taking high-resolution time-resolved images of complex pore structures much more quickly than traditional &#181;-CT. The Diamond Lightsource Pink Beam was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 hours. The images were segmented and the porosity and permeability were measured using image analysis and network extraction. Porosity increased uniformly along the length of the sample; however, the rate of increase of both porosity and permeability slowed at later times.

Synchrotron fast tomography was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 h.

用同步快速反应层析成像动态孔隙规模油藏条件下成像碳酸盐

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve ...

Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil (HGO) for production of transportation fuels through a fluid catalytic cracking (FCC) route. Cracking experiments are performed with a fully automated reaction unit at a fixed weight hourly space velocity (WHSV) of 8 hr-1, 490-530 &#176;C, and catalyst/oil ratios of 4-12 g/g. When a feed is in contact with catalyst in the fluid-bed reactor, cracking takes place generating gaseous, liquid, and solid products. The vapor produced is condensed and collected in a liquid receiver at -15 &#176;C. The non-condensable effluent is first directed to a vessel and is sent, after homogenization, to an on-line gas chromatograph (GC) for refinery gas analysis. The coke deposited on the catalyst is determined in situ by burning the spent catalyst in air at high temperatures. Levels of CO2 are measured quantitatively via an infrared (IR) cell, and are converted to coke yield. Liquid samples in the receivers are analyzed by GC for simulated distillation to determine the amounts in different boiling ranges, i.e., IBP-221 &#176;C (gasoline), 221-343 &#176;C (light cycle oil), and 343 &#176;C+ (heavy cycle oil). Cracking of a feed containing canola oil generates water, which appears at the bottom of a liquid receiver and on its inner wall. Recovery of water on the wall is achieved through washing with methanol followed by Karl Fischer titration for water content. Basic results reported include conversion (the portion of the feed converted to gas and liquid product with a boiling point below 221 &#176;C, coke, and water, if present) and yields of dry gas (H2-C2's, CO, and CO2), liquefied petroleum gas (C3-C4), gasoline, light cycle oil, heavy cycle oil, coke, and water, if present.

This paper presents an experimental method to produce biofuels and biochemicals from canola oil mixed with a fossil-based feed in the presence of a catalyst at mild temperatures. Gaseous, liquid, and solid products from a reaction unit are quantified and characterized. Conversion and individual product yields are calculated and reported.

通过催化裂化转换从菜籽油生物燃料和生物化学实验室生产

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil ...

化学

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to visualize the behavior of petroleum samples under process conditions. The experimental setup relies on a custom-built micro-reactor fitted with a sapphire window at the bottom, which is placed over the objective of an inverted microscope equipped with a cross-polarizer module. Using reflection microscopy enables the visualization of opaque samples, such as petroleum vacuum residues, or asphaltenes. The combination of the sapphire window from the micro-reactor with the cross-polarizer module of the microscope on the light path allows high-contrast imaging of isotropic and anisotropic media. While observations are carried out, the micro-reactor can be heated to the temperature range of cracking reactions (up to 450 &#176;C), can be subjected to H2 pressure relevant to hydroconversion reactions (up to 16 MPa), and can stir the sample by magnetic coupling. 
Observations are typically carried out by taking snapshots of the sample under cross-polarized light at regular time intervals. Image analyses may not only provide information on the temperature, pressure, and reactive conditions yielding phase separation, but may also give an estimate of the evolution of the chemical (absorption/reflection spectra) and physical (refractive index) properties of the sample before the onset of phase separation.

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

This article describes a setup and method for the in situ visualization of oil samples under a variety of temperature and pressure conditions that aim to emulate refining and upgrading processes. It is primarily used for studying isotropic and anisotropic media involved in the fouling behavior of petroleum feeds.

在油样品的相行为在炼油工艺条件的原位可视化

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to ...

Combining Microfluidics and Microrheology to Determine Rheological Properties of Soft Matter during Repeated Phase Transitions

The microstructure of soft matter directly impacts macroscopic rheological properties and can be changed by factors including colloidal rearrangement during previous phase changes and applied shear. To determine the extent of these changes, we have developed a microfluidic device that enables repeated phase transitions induced by exchange of the surrounding fluid and microrheological characterization while limiting shear on the sample. This technique is &#181;2rheology, the combination of microfluidics and microrheology. The microfluidic device is a two-layer design with symmetric inlet streams entering a sample chamber that traps the gel sample in place during fluid exchange. Suction can be applied far away from the sample chamber to pull fluids into the sample chamber. Material rheological properties are characterized using multiple particle tracking microrheology (MPT). In MPT, fluorescent probe particles are embedded into the material and the Brownian motion of the probes is recorded using video microscopy. The movement of the particles is tracked and the mean-squared displacement (MSD) is calculated. The MSD is related to macroscopic rheological properties, using the Generalized Stokes-Einstein Relation. The phase of the material is identified by comparison to the critical relaxation exponent, determined using time-cure superposition. Measurements of a fibrous colloidal gel illustrate the utility of the technique. This gel has a delicate structure that can be irreversibly changed when shear is applied. &#181;2rheology data shows that the material repeatedly equilibrates to the same rheological properties after each phase transition, indicating that phase transitions do not play a role in microstructural changes. To determine the role of shear, samples can be sheared prior to injection into our microfluidic device. &#181;2rheology is a widely applicable technique for the characterization of soft matter enabling the determination of rheological properties of delicate microstructures in a single sample during phase transitions in response to repeated changes in the surrounding environmental conditions.

We demonstrate the fabrication and use of a microfluidic device that enables multiple particle tracking microrheology measurements to study the rheological effects of repeated phase transitions on soft matter.

微流体和 Microrheology 相结合测定软物质在重复相变过程中的流变特性

The microstructure of soft matter directly impacts macroscopic rheological properties and can be changed by factors including colloidal rearrangement ...

Pore-scale Imaging and Characterization of Hydrocarbon Reservoir Rock Wettability at Subsurface Conditions Using X-ray Microtomography

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to characterize the complex wetting conditions of hydrocarbon reservoir rock using pore-scale three-dimensional X-ray imaging at subsurface conditions. In this work, heterogeneous carbonate reservoir rocks, extracted from a very large producing oil field, have been used to demonstrate the protocol. The rocks are saturated with brine and oil and aged over three weeks at subsurface conditions to replicate the wettability conditions that typically exist in hydrocarbon reservoirs (known as mixed-wettability). After the brine injection, high-resolution three-dimensional images (2 &#181;m/voxel) are acquired and then processed and segmented. To calculate the distribution of the contact angle, which defines the wettability, the following steps are performed. First, fluid-fluid and fluid-rock surfaces are meshed. The surfaces are smoothed to remove voxel artefacts, and in situ contact angles are measured at the three-phase contact line throughout the whole image. The main advantage of this method is its ability to characterize in situ wettability accounting for pore-scale rock properties, such as rock surface roughness, rock chemical composition, and pore size. The in situ wettability is determined rapidly at hundreds of thousands of points. 
The method is limited by the segmentation accuracy and X-ray image resolution. This protocol could be used to characterize the wettability of other complex rocks saturated with different fluids and at different conditions for a variety of applications. For example, it could help in determining the optimal wettability that could yield an extra oil recovery (i.e., designing brine salinity accordingly to obtain higher oil recovery) and to find the most efficient wetting conditions to trap more CO2 in subsurface formations.

This protocol is presented to characterize the complex wetting conditions of an opaque porous medium (hydrocarbon reservoir rock) using three-dimensional images obtained by X-ray microtomography at subsurface conditions.

利用 X 射线层析在地下条件下油气储层岩石润湿性的孔隙度成像与表征

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to ...

Calibration Procedures for Orthogonal Superposition Rheology

Orthogonal superposition (OSP) rheology is an advanced rheological technique that involves superimposing a small-amplitude oscillatory shear deformation orthogonal to a primary shear flow. This technique allows the measurement of structural dynamics of complex fluids under non-linear flow conditions, which is important for the understanding and prediction of the performance of a wide range of complex fluids. The OSP rheological technique has a long history of development since the 1960s, mainly through the custom-built devices that highlighted the power of this technique. The OSP technique is now commercially available to the rheology community. Given the complicated design of the OSP geometry and the non-ideal flow field, users should understand the magnitude and sources of measurement error. This study presents calibration procedures using Newtonian fluids that includes recommendations for best practices to reduce measurement errors. Specifically, detailed information on the end-effect factor determination method, sample filling procedure, and identification of the appropriate measurement range (e.g., shear rate, frequency, etc.) are provided.

We present a detailed calibration protocol for a commercial orthogonal superposition rheology technique using Newtonian fluids including end-effect correction factor determination methods and recommendations for best practices to reduce experimental error.

正交叠加流变学校准程序

Orthogonal superposition (OSP) rheology is an advanced rheological technique that involves superimposing a small-amplitude oscillatory shear deformation ...

与CO平衡的原油流变学测量

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测量碳为基础的污染物矿化结合使用CO