Preparation and Evaluation of Thermosensitive Plugging MaterialsBased on Shape Memory Polymers
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摘要:
传统堵漏材料对裂缝性漏失的封堵存在不足，针对该问题，将形状记忆聚合物材料引入封堵作业，利用其“温控形变”特性，制备出温敏型堵漏材料；采用热机械动力分析仪和形状恢复试验，评价了其玻璃态转变温度和形状记忆性能；通过裂缝封堵模拟试验，评价了温敏型堵漏材料的裂缝封堵效果，并探索了其裂缝封堵机理。研究结果表明：温敏型堵漏材料的形变温度（即玻璃态转变温度）可根据漏失层段位置需求在温度80～120 ℃范围内进行调控，形状记忆性能优异（形状恢复率大于95%），且耐温性能良好，初始热解温度230～258 ℃，可适用于温度80～120 ℃的地层，与传统堵漏材料复配后可封堵3～5 mm裂缝。研究结果可为研制和应用新型材料封堵裂缝提供参考。
Abstract:Considering the insufficient ability of traditional plugging materials to seal fractured leakage, shape memory polymers (SMPs) were introduced for plugging. A thermosensitive plugging material was prepared based on SMPs for their “temperature-controlled deformation” property. Then, its glass transition temperature and shape memory performance were evaluated by the thermo-mechanical dynamic analyzer and shape recovery test. Moreover, the simulation tests of fracture plugging were carried out to assess the plugging capability of the polymers on fractures and explore the plugging mechanism. The research results indicated that the deformation temperature(glass transition temperature) of the thermosensitive plugging material could be regulated in the range of 80–120 ℃ according to the locations of the leakage layers, featuring excellent shape memorizing performance (with a shape recovery ratio of more than 95%). In addition, the temperature resistance of this material was good, with the initial pyrolysis temperature between 230 and 258 ℃, which meant that the material could be applied in a formation temperature environment of 80–120 ℃. The compound of this material and the traditional plugging material could successfully seal the fractures with width ranging from 3–5 mm. The research results can provide a reference for the preparation and application of this new material to fracture plugging.
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图 1 形状记忆聚合物E-MP固化反应前后的红外光谱
Figure 1. Fourier transform infrared spectroscopy (FT-IR) of SMP E-MP before and after the curing process
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图 2 不同配比形状记忆聚合物的热性能测试结果
Figure 2. Thermal properties of SMPs with different compositions
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图 3 不同配比形状记忆聚合物的形状恢复率与时间的关系
Figure 3. Relationship between shape recovery ratio and time of SMPs with different compositions
表 1 形状记忆聚合物单体配比
Table 1 Composition of SMP monomer
样品 质量分数，% E-51 PMP TGE 2-EMI E-MP10 55.85 37.66 6.21 0.28 E-MP20 48.17 39.40 12.04 0.39 E-MP30 40.99 41.11 17.57 0.33 
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表 2 不同配比形状记忆聚合物的耐温性能
Table 2 Temperature resistance of SMPs with different compositions
样品 热解温度/℃ 玻璃态转变
温度/℃t5 t50 E-MP10 230.5 336.5 86.2 E-MP20 255.0 366.6 101.4 E-MP30 258.2 367.4 107.5 注：t5为样品质量损失5%时的外界温度，℃；t50为样品质量损失50%时的外界温度，℃。
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表 3 不同配比形状记忆聚合物的形状恢复性能
Table 3 Shape recovery performance of SMPs with differentcompositions
样品 形状固定率，
%形状恢复率，
%不同温度的形状恢复时间/s tg tg+10℃ tg+20℃ E-MP10 98 100 37 22 22 E-MP20 98 100 43 30 25 E-MP30 98 100 43 41 31
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表 4 形状记忆聚合物对钻井液流变性的影响
Table 4 Effect of SMPs on rheology of drilling fluids
试验浆 测试条件 表观黏度/
(mPa·s)塑性黏度/
( mPa·s)动切力/
Pa基浆 老化前 34.5 17.0 15.0 老化后 33.5 18.0 14.0 基浆+E-MP 老化前 35.0 16.0 16.0 老化后 34.0 17.5 14.5 注：基浆为4.0%膨润土+0.4%CMC-LV+水。
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表 5 裂缝封堵试验结果
Table 5 Results of fracture plugging experiment
堵漏
工作液裂缝开度/
mm温度/
℃封堵突破
压力/MPa漏失量/
mL封堵
效果1 3×2 25 0 全漏 无效 100 0 全漏 无效 2 3×2 25 0 全漏 无效 100 12.8 23 有效 4×3 100 11.5 36 有效 注：堵漏工作液1为常规堵漏工作液，配方为4.0%膨润土+0.4%CMC-LV+0.2%FIB+4.0%QJD（8/10目）+3.0%QJD（10/20目）+水；堵漏工作液2为含有形状记忆聚合物颗粒的温敏型堵漏工作液，配方为4.0%膨润土+0.4%CMC-LV+0.2%FIB+4.0%QJD（8/10目）+3.0%QJD（10/20目）+3.0%E-MP（8/10目）+3.0%E-MP（10/20目）+水。
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