Synthesis and Performance Evaluation of Drilling Fluid Core-Shell Self-Unplugging Temporary Plugging Agent JZD
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摘要: 传统暂堵剂往往因破胶不彻底、解封滞后或残留物难以清除，极易造成储层孔喉堵塞、渗透率下降等二次伤害，严重制约油气藏采收率提升。开发兼具高效封堵性能与自解堵功能的新型暂堵材料，成为当前油气田储层保护领域的核心研究方向与技术突破新思路。基于Stöber法，以改性聚对苯二甲酸-己二酸丁二酯为核、二氧化硅为壳，成功制备了适用于钻井液的核壳式自解堵暂堵剂，该暂堵剂采用核壳协同机制，内核保封堵强度，外壳带智能响应基团，实现“前期强堵、后期快解”，破解封堵与解堵的矛盾。采用傅里叶变换红外光谱（FT-IR）、场发射扫描电子显微镜（FE-SEM）和同步热重-差热分析（TG-DTA）系统，对该暂堵剂的化学结构、微观形貌及热稳定性进行了系统表征。结果表明，所研制的暂堵剂具有明显的核壳结构，在120 ℃、矿化度为150 000 mg/L条件下，15 d降解率为33.62%，36 d完成全部降解，可满足中长期安全作业需求。同时，该暂堵剂与钻井液体系配伍性良好，抗温能力可达130 ℃，并能耐受25%NaCl盐环境。封堵性能测试表明，随暂堵剂加量增加，砂床封堵深度从8.5 cm降至1.3 cm，封堵率达89.32%，渗透率恢复值为95.45%，兼具优异封堵能力与储层保护效果。Abstract: Conventional temporary plugging agents often cause secondary formation damage such as blocking of pore throats in reservoir formations and reduced permeability etc. due to incomplete gel-breaking, delayed unplugging or residues that are difficult to remove, severely restricting the recovery enhancement of oil and gas reservoirs. Developing novel temporary plugging materials with both efficient plugging capacity and self-unplugging capability has become a core research direction and a new idea for technical breakthroughs in the field of oil and gas reservoir protection. Based on the Stöber method, a core-shell self-unplugging temporary plugging agent for drilling fluids was successfully developed using modified poly(butylene adipate-co-terephthalate) as the core and silica as the shell. With core-shell synergistical mechanism, the core of this temporary plugging agent ensures plugging strength, while the shell, with its smart responsive groups, achieves the goal of “strong plugging in the early stage and fast unplugging in the later stage”, thus resolving the contradiction of plugging and unplugging. The chemical structure, micromorphology and thermal stability of this temporary plugging agent was systematically characterized using Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FE-SEM) and simultaneous thermogravimetric-differential thermal analysis (TG-DTA). The results of the characterization show that the temporary plugging agent developed has an obvious core-shell structure. At 120 ℃ and a salinity of 150,000 mg/L, the rate of degradation of the temporary plugging agent reaches 33.62% in 15 days, and it is completely degraded in 36 days, which can meet the requirements of medium- and long-term safe operation. Meanwhile, the temporary plugging agent is well compatible with drilling fluids, it functions normally at temperatures up to 130 ℃, and is resistant to 25% NaCl environment. Plugging capacity test results show that the plugging depth of sand-bed reduced from 8.5 cm to 1.3 cm as the amount of the temporary plugging agent increases, the plugging efficiency reaches 89.32%, and the percent recovery of permeability is 95.45%, demonstrating both excellent plugging capacity and reservoir protection performance.
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表 1 不同分子量和目数材料降解性
分子量 2万 10万 20万 30万 目数 300 100 150 200 300 降解率/% 15 d 100 57.4 54.2 39.2 46.0 45.0 45.8 30 d 100 76.6 76.0 66.8 68.3 69.3 70.4 注：降解率计算方法为质量损失法，具体计算方式为：降解率=1−残余质量/初始质量。 
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表 2 不同JZD加量下实验浆的流变性和滤失性测试结果
暂堵
剂/%实验
条件AV/
mPa·sPV/
mPa·sYP/
PaYP/PV/
Pa/mPa·sFLAPI/
mLFLHTHP/
mL0 老化前 28.0 16.0 12.0 0.8 20.0 142.0 老化后 20.0 14.0 6.0 0.4 30.0 0.5 老化前 38.0 20.0 18.0 0.9 13.8 84.0 老化后 35.0 21.0 14.0 0.7 15.6 1.0 老化前 43.0 23.0 20.0 0.9 9.4 62.0 老化后 40.5 22.0 18.5 0.8 11.2 1.5 老化前 40.5 23.0 17.5 0.8 7.2 43.0 老化后 27.0 17.0 10.0 0.6 9.8 2.0 老化前 39.5 23.0 16.5 0.7 6.1 36.0 老化后 33.0 19.0 14.0 0.7 8.0 注：老化条件为120 ℃、16 h。
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表 3 JZD在实验浆中的抗温性评价
T老化/
℃AV/
mPa·sPV/
mPa·sYP/
PaYP/PV/
Pa/mPa·sFLAPI/
mL110 46 25 21 0.8 12 120 43 24 19 0.8 14 130 40 23 17 0.7 16 140 32 20 12 0.6 25 150 26 18 8 0.4 38 注：老化条件为不同温度下热滚16 h。
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表 4 暂堵剂JZD的抗盐性能评价
NaCl/
%实验
条件AV/
mPa·sPV/
mPa·sYP/
PaYP/PV/
Pa/mPa·sFLAPI/
mL0 老化前 43.0 23.0 20.0 0.9 9.4 120 ℃、16 h 40.5 22.0 18.5 0.8 11.2 5 老化前 40.0 23.0 17.0 0.7 13.0 120 ℃、16 h 32 18.0 14.0 0.8 16.0 10 老化前 42.5 24.0 18.5 0.8 9.0 120 ℃、16 h 33.5 19.5 14.0 0.7 18.0 15 老化前 40.8 20.0 20.8 1.0 13.0 120 ℃、16 h 38.5 23.0 15.5 0.7 17.0 20 老化前 79.5 35.0 44.5 1.3 11.0 120 ℃、16 h 61.0 31.0 30.0 1.0 9.0 25 老化前 77.8 38.0 39.8 0.9 8.0 120 ℃、16 h 85.0 44.0 41.0 0.8 3.0
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