WO2020224419A1 - 一种利用dnp-mri测量油水分布方法 - Google Patents

一种利用dnp-mri测量油水分布方法 Download PDF

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WO2020224419A1
WO2020224419A1 PCT/CN2020/085475 CN2020085475W WO2020224419A1 WO 2020224419 A1 WO2020224419 A1 WO 2020224419A1 CN 2020085475 W CN2020085475 W CN 2020085475W WO 2020224419 A1 WO2020224419 A1 WO 2020224419A1
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dnp
mri
water
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陈黎
陈俊飞
刘朝阳
张震
冯涛
冯继文
陈方
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中国科学院精密测量科学与技术创新研究院
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    • G—PHYSICS
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/12—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using double resonance
    • G—PHYSICS
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • G01N24/081—Making measurements of geologic samples, e.g. measurements of moisture, pH, porosity, permeability, tortuosity or viscosity
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    • G01—MEASURING; TESTING
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    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/44—Arrangements or instruments for measuring magnetic variables involving magnetic resonance using nuclear magnetic resonance [NMR]
    • G01R33/48—NMR imaging systems
    • G01R33/54—Signal processing systems, e.g. using pulse sequences ; Generation or control of pulse sequences; Operator console
    • G01R33/56—Image enhancement or correction, e.g. subtraction or averaging techniques, e.g. improvement of signal-to-noise ratio and resolution
    • G01R33/565—Correction of image distortions, e.g. due to magnetic field inhomogeneities
    • G01R33/56509—Correction of image distortions, e.g. due to magnetic field inhomogeneities due to motion, displacement or flow, e.g. gradient moment nulling
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/62—Arrangements or instruments for measuring magnetic variables involving magnetic resonance using double resonance
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/44—Arrangements or instruments for measuring magnetic variables involving magnetic resonance using nuclear magnetic resonance [NMR]
    • G01R33/448—Relaxometry, i.e. quantification of relaxation times or spin density
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A90/00—Technologies having an indirect contribution to adaptation to climate change
    • Y02A90/30—Assessment of water resources

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  • the invention belongs to the technical field of nuclear magnetic resonance applications, and specifically relates to a method for measuring oil-water distribution using DNP-MRI, which can be applied to analyze fluid distribution and flow laws in porous materials.
  • Porous materials such as reservoir rocks are rich in different fluid phases such as oil and water.
  • the distribution of oil and water in the rock formation is a key issue when exploring the seepage/displacement law.
  • the acquisition of two-phase distribution information helps to understand the two-phase saturation
  • the important parameters such as degree of permeability and relative permeability provide reference for reservoir evaluation and development.
  • NMR technology is widely used in the study of the structure and fluid properties of porous materials such as cores due to its non-destructive testing characteristics.
  • the present invention provides a method for measuring oil-water distribution using DNP-MRI, which is simple, convenient to operate, short in measurement time, and high in measurement efficiency.
  • a method for measuring oil-water distribution using DNP-MRI which is characterized by comprising the following steps:
  • step 3 Under the same MRI experimental conditions as in step 2, apply microwave excitation to perform DNP-MRI experiments, and collect DNP-enhanced MRI images of the sample to be tested;
  • the area where the MRI signal strength is enhanced is the fluid phase distribution area that is selected to be enhanced, and the area where the MRI signal strength does not change significantly is Non-selective enhanced fluid phase distribution area.
  • the free radicals are non-selective free radicals, which can enhance the NMR signal of the water phase and the oil phase at the same time. If only the NMR signal of the water phase needs to be enhanced, it is necessary to add an enhanced oil phase For relaxing relaxation reagents, if only the NMR signal of the oil phase needs to be enhanced, it is also necessary to add a relaxation reagent that can enhance the relaxation of the water phase.
  • the free radicals are selective free radicals.
  • the selective free radicals can enhance the NMR signal of the water phase or the oil phase by DNP. If DNP is required to enhance the NMR signal of the water phase, add a DNP capable of enhancing the NMR signal of the water phase. Selective free radicals. If DNP is needed to enhance the NMR signal of the oil phase, then a selective free radical capable of DNP can enhance the NMR signal of the oil phase is added.
  • the present invention has the following beneficial effects and advantages:
  • This method takes advantage of the immiscibility of the oil and water phases, and uses DNP to selectively enhance the NMR signal of the oil or water phase, which has strong applicability.
  • This method can improve NMR signal sensitivity and MRI image contrast. By comparing the MRI images before and after DNP enhancement, it can directly reflect the distribution of oil and water phases.
  • This method can improve the signal-to-noise ratio of NMR and ensure the reliability of the measurement results, and the measurement time is short and the measurement efficiency is high.
  • Figure 1 is a schematic diagram of a glass bead model.
  • Figure 2 is a schematic diagram of a spin echo pulse sequence containing microwave excitation.
  • Figure 3 is an MRI image of the glass bead model without DNP enhancement.
  • Figure 4 shows the enhanced MRI image of the glass bead model DNP.
  • Fig. 5 is the difference image between the MRI image of the glass bead model without DNP enhancement and the MRI image of the glass bead model with DNP enhancement.
  • the glass bead model (as shown in Figure 1) is made as follows: take a quartz tube 1 with a diameter of 10mm, open one end of the quartz tube 1, and seal the other end.
  • the glass beads 2 with a particle size of 3-5mm are randomly stacked in a quartz tube with a diameter of 10mm, and they are infiltrated by layers of water containing relaxation reagent MnCl 2 and mineral oil containing free radical TEMPO (Tetramethylpiperidine Nitrogen Oxide)
  • MnCl 2 Tetramethylpiperidine Nitrogen Oxide
  • the glass beads in the quartz tube, the upper layer is the oil phase
  • the lower layer is the water phase.
  • TEMPO can enhance the NMR signal of the oil phase under DNP conditions
  • MnCl 2 can enhance the relaxation of the water phase, and suppress the NMR signal of the water phase under DNP conditions ;
  • the glass bead model is placed in the sample area of a 0.06T DNP magnetic resonance imaging system, where the static magnetic field is provided by a permanent magnet, and the resonant cavity used to excite electronic resonance can provide a cylindrical sample with a diameter of 10mm and a height of 22mm. Space, the glass bead model is located in the center of the magnetic field;

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Abstract

一种利用DNP-MRI测量油水分布方法，该方法为：1、在含油水的待测样品中加入用于DNP增强水相或油相NMR信号的自由基；2、将待测样品进行MRI实验，采集待测样品无DNP增强的MRI图像；3、在与步骤2同等的MRI实验条件下，施加微波激励，进行DNP-MRI测试，采集待测样品DNP增强后的MRI图像；4、将DNP增强后的MRI图像与无DNP增强的MRI图像进行比较，DNP增强的MRI图像中，MRI信号强度增强的区域为选择增强的流体相分布区域，MRI信号强度未明显变化的区域为非选择增强的流体相分布区域。该方法简单，操作方便，测量时间短，测量效率高。

Description

一种利用DNP-MRI测量油水分布方法 技术领域
本发明属于核磁共振应用技术领域，具体涉及一种利用DNP-MRI测量油水分布方法，可应用于分析多孔材料中流体分布及流动规律。
背景技术
储层岩石等多孔材料富含油、水等不同流体相，岩层中的油水分布是开展渗流/驱替规律探究时所面临的关键问题，两相分布信息的获取，有助于了解两相饱和度、相对渗透率等重要参数，为储层评估、开发提供参考。
NMR技术以其无损检测的特点广泛应用于岩心等多孔材料结构及流体特性的研究。
高场NMR下，利用油水中 1H化学位移差异，采用化学位移成像可以获取两相流体分布。然而，受材料中固液两相磁化率差异引起的内部磁场梯度的影响，材料中两相化学位移谱的分辨率不高。高场并不适合岩心等材料的研究，尤其是岩心等非匀质材料，孔径越小，内部磁场梯度越大，会使小孔径内NMR信号快速衰减甚至不可测量，从而进一步降低测试结果的可靠性。
为了减少固液两相磁化率引起的磁场梯度，岩心等多孔材料的应用研究多在低场条件下开展。然而，低场条件下多依赖于样品的弛豫或扩散特性区分不同流体，但由于材料结构的非匀质性及流体的分布差异，不同流体可能具有相同的弛豫或扩散特性，从而不能有效区分。此外，较低的NMR灵敏度及分辨率极大地增加了样品的测试时间，也进一步限制了常规MRI方法在测量油水分布中的应用。为缩短样品测试时间，提高低场MRI方法的效率与可靠性，需要寻求新的方法来提高NMR的灵敏度。
发明内容
基于上述现有技术存在的问题，本发明提供了一种利用DNP-MRI测量油水分布方法，该方法简单，操作方便，测量时间短，测量效率高。
实现本发明上述目的所采用的技术方案为：
一种利用DNP-MRI测量油水分布方法，其特征在于包括如下步骤：
1、在含油水的待测样品中加入用于DNP增强水相或油相NMR信号的自由基；
2、将待测样品进行MRI实验，采集待测样品无DNP增强的MRI图像；
3、在与步骤2同等的MRI实验条件下，施加微波激励，进行DNP-MRI实验，采集待测样品DNP增强后的MRI图像；
4、将DNP增强后的MRI图像与无DNP增强的MRI图像进行比较，DNP增强的MRI 图像中，MRI信号强度增强的区域为选择增强的流体相分布区域，MRI信号强度未明显变化的区域为非选择增强的流体相分布区域。
进一步，所述的自由基为非选择性自由基，非选择性自由基能同时增强水相和油相的NMR信号，若只需要增强水相的NMR信号时，则还需加入能增强油相弛豫的弛豫试剂，若只需要增强油相的NMR信号时，则还需加入能增强水相弛豫的弛豫试剂。
进一步，所述的自由基为选择性自由基，选择性自由基能DNP增强水相或油相的NMR信号，若需要DNP增强水相的NMR信号时，则加入能DNP增强水相NMR信号的选择性自由基，若需要DNP增强油相的NMR信号时，则加入能DNP增强油相NMR信号的选择性自由基。
与现有技术相比，本发明的有益效果和优点在于：
1、该方法利用油水两相不相溶的特点，使用DNP选择性增强油相或水相NMR信号，适用性强。
2、该方法可提高NMR信号灵敏度及MRI图像对比度，通过对比DNP增强前后的MRI图像，可直观反映油水两相的分布情况。
3、该方法可提高NMR的信噪比，确保测量结果的可靠性，而且测量时间短，测量效率高。
附图说明
图1为玻璃珠模型示意图。
图2为含有微波激励的自旋回波脉冲序列的示意图。
图3为玻璃珠模型无DNP增强的MRI图像。
图4为玻璃珠模型DNP增强的MRI图像。
图5为玻璃珠模型无DNP增强的MRI图像与玻璃珠模型DNP增强的MRI图像的差值图像。
其中，1-石英管、2-玻璃珠。
具体实施方式
下面结合附图对本发明进行详细说明。
实施例1
1、制作玻璃珠模型以模拟含油水的多孔材料，玻璃珠模型(如图1所示)的制作方法为：取直径为10mm的石英管1，石英管1的一端开口，另一端密封，用粒径为3-5mm的玻璃珠2随机堆叠于直径为10mm石英管中，采用含弛豫试剂MnCl 2的水与含自由基TEMPO (四甲基哌啶氮氧化物)的矿物油分层浸润石英管中的玻璃珠，上层为油相，下层为水相，TEMPO能在DNP条件下增强油相的NMR信号，MnCl 2能增强水相的弛豫，在DNP条件下抑制水相的NMR信号；
2、将玻璃珠模型放置在0.06T DNP磁共振成像系统的样品区域，该系统中静磁场由永磁体提供，用于激发电子共振的谐振腔能够提供直径为10mm、高度为22mm的圆柱形样品空间，玻璃珠模型位于磁场中心；
3、进行常规、无DNP增强的MRI实验：
3.1、设置实验参数并开始测试，采用自旋回波脉冲序列(SE)，测试参数如下：FOV：30×30mm、AcquMatrix＝128×128、TE＝50ms、TR＝1.2s、累加次数NS＝4；成像方位为矢状位，并选定成像层面；
3.2、实验结束后，进行图像重建，重建结果记录为matrix1，将重建结果映射为灰度图像，即得到玻璃珠模型无DNP增强的MRI图像，如图3所示；
4、进行DNP-MRI实验：
4.1、设置实验参数并开始实验，采用含有微波激励的自旋回波脉冲序列(DNP-SE)，如图2所示，测试参数如下：FOV：30×30mm、AcquMatrix＝128×128、TE＝50ms、TR＝3s、累加次数NS＝1，微波照射时间1s，微波功率50W；成像方位为矢状位，并选定成像层面(与步骤3中的成像层面保持一致)；
4.2、测试结束后，进行图像重建，重建结果记录为matrix2，将重建结果映射为灰度图像，即得到玻璃珠模型DNP增强的MRI图像，如图4所示；
5、将步骤3.2和步骤4.2中得到的重建结果matrix1和matrix2作差，并将差值映射为灰度图像，即得到差值图像，如图5所示，以玻璃珠模型无DNP增强的图像作为参考图像，与图3相比较，图4中，石英管底部的MRI信号强度大幅减小甚至几乎消失，而石英管上部的MRI信号不仅没有减弱而且还进一步增强，由此表明，水分布在石英管的底部，油分布在石英管的上半部，图5中显示的灰度图像即为油的分布图像。

Claims (3)

  1. 一种利用DNP-MRI测量油水分布方法，其特征在于包括如下步骤：
    1.1、在含油水的待测样品中加入用于DNP增强水相或油相NMR信号的自由基；
    1.2、将待测样品进行MRI实验，采集待测样品无DNP增强的MRI图像；
    1.3、在与步骤2同等的MRI实验条件下，施加微波激励，进行DNP-MRI实验，采集待测样品DNP增强后的MRI图像；
    1.4、将DNP增强后的MRI图像与无DNP增强的MRI图像进行比较，DNP增强的MRI图像中，MRI信号强度增强的区域为选择增强的流体相分布区域，MRI信号强度未明显变化的区域为非选择增强的流体相分布区域。
  2. 根据权利要求1所述的利用DNP-MRI测量油水分布方法，其特征在于：所述的自由基为非选择性自由基，非选择性自由基能同时增强水相和油相的NMR信号，若只需要增强水相的NMR信号时，则还需加入能增强油相弛豫的弛豫试剂，若只需要增强油相的NMR信号时，则还需加入能增强水相弛豫的弛豫试剂。
  3. 根据权利要求1所述的利用DNP-MRI测量油水分布方法，其特征在于：所述的自由基为选择性自由基，选择性自由基能DNP增强水相或油相的NMR信号，若需要DNP增强水相的NMR信号时，则加入能DNP增强水相NMR信号的选择性自由基，若需要DNP增强油相的NMR信号时，则加入能DNP增强油相NMR信号的选择性自由基。
PCT/CN2020/085475 2019-05-08 2020-04-18 一种利用dnp-mri测量油水分布方法 WO2020224419A1 (zh)

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CN110082382A (zh) * 2019-05-08 2019-08-02 中国科学院武汉物理与数学研究所 一种利用动态核极化进行油水两相nmr信号分离的方法
CN112345573B (zh) * 2019-08-06 2022-05-03 中国科学院武汉物理与数学研究所 一种利用dnp-nmr区分油类粘度的方法
CN112666048B (zh) * 2019-10-16 2022-06-07 中国科学院武汉物理与数学研究所 一种利用动态核极化增强测试材料润湿性及孔径大小的方法

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