ISSN 1008-5548

CN 37-1316/TU

最新出版

用于油井水泥环微裂缝自修复的微胶囊的制备与性能评价

Preparation and performance evaluation of microcapsules for self-healing of micro-cracks in oil well cement sheaths


张翼飞1, 程小伟1, 张春梅1, 梅开元1, 韦庭丛2

1.西南石油大学 新能源与材料学院, 油气藏地质及开发工程全国重点实验室, 四川 成都 610500;

2.广西大学 土木建筑工程学院, 广西 南宁 530004


引用格式:

张翼飞, 程小伟, 张春梅, 等. 用于油井水泥环微裂缝自修复的微胶囊的制备与性能评价[J]. 中国粉体技术, 2026, 32(2): 1-14.

Citation:ZHANG Yifei, CHENG Xiaowei, ZHANG Chunmei, et al. Preparation and performance evaluation of microcapsules for self-healing of micro-cracks in oil well cement sheaths[J]. China Powder Science and Technology, 2026, 32(2): 1-14.

DOI:10.13732/j.issn.1008-5548.2026.02.002

收稿日期: 2025-09-10, 修回日期: 2025-12-29,上线日期: 2026-01-12。

基金项目: 国家自然科学基金项目, 编号: 42207206; 四川省科技厅自然科学基金项目, 编号:2 024NSFSC0154。

第一作者: 张翼飞(2001—),男,硕士生,研究方向为固井自修复材料。E-mail:1417339135@qq.com。

通信作者: 程小伟(1977—),男,教授,博士,博士生导师,四川省学术和技术带头人后备人选,研究方向为先进胶凝材料及其在固井中应用。E-mail:chengxw@swpu.edu.cn。


摘要 目的】为了解决吸油树脂与油井水泥的相容性差、水泥石强度下降的问题,实现对油井水泥环微裂缝的遇油自修复功能,保证油气井中固井水泥环的密封完整性。【方法】 采用化学沉淀法,以吸油树脂为芯材、活性二氧化硅为壳材,制备具有遇油膨胀微裂缝自修复功能的微胶囊;借助扫描电子显微镜、红外光谱仪、热重仪对吸油树脂、微胶囊进行测试与表征;对比分别掺入吸油树脂、微胶囊前、后的水泥石试样的抗压强度、抗压强度恢复率和渗透率,对水泥石微裂缝的自修复性能进行评价,探讨掺入吸油树脂和微胶囊的水泥石的微裂缝自修复机制。【结果 油树脂、微胶囊的中值粒径D50分别为5.601、 6.590 μm。在温度为0~213 ℃时,吸油树脂、微胶囊都几乎无质量损失,具有良好的热稳定性,满足固井施工要求; 在波数为941 cm-1处出现Si—OH的振动吸收峰;微胶囊具有较大的比表面积;吸油6 h后的吸油树脂、微胶囊的体积膨胀率分别为100%、10%;微胶囊的质量分数为1%时的水泥石试样的抗压强度在养护龄期为7 d时达到最大值,在自修复养护龄期为28 d时的抗压强度为(29.06±1.61) MPa,抗压强度恢复率为79.05%,在自修复养护龄期为28 d时的渗透率为0.563×10-3 μm2,降幅为39.36%。【结论】 微胶囊的二氧化硅外壳可提高水泥石破损后的抗压强度;当掺入微胶囊的水泥石受损产生裂缝时,二氧化硅外壳因裂缝尖端处的作用而破裂,内部吸油树脂遇油后膨胀,实现了水泥石裂缝的自修复。

关键词油井水泥环; 微裂缝自修复; 微胶囊; 吸油树脂; 二氧化硅; 渗透率


Abstract

Objective This study aims to address the poor compatibility between oil-absorbing resin and oil well cement, which leads to a reduction in the strength of cement stone, and to achieve oil-triggered self-healing of micro-cracks in the cement sheath, thereby ensuring the sealing integrity of the cement sheath in oil and gas wells. In this study, microcapsules with oil-swelling and micro-crack self-healing functions are prepared. The microcapsules are fabricated via a chemical precipitation method using oil-absorbing resin as the core material and reactive silica as the shell material.

Methods Scanning electron microscopy (SEM) imaging, thermogravimetric analysis (TG), Fourier-transform infrared (FTIR) spectroscopy, and energy-dispersive spectroscopy (EDS) mapping were employed to test and characterize the oil-absorbing resin and the microcapsule. The oil-swelling and micro-crack self-healing performance of cement samples incorporating the oil-absorbing resin or microcapsule was evaluated by investigating their compressive strength, recovery rate of compressive strength, and permeability. Furthermore, SEM imaging and EDS mapping were conducted on thin sections extracted from crack surfaces of the cement samples to investigate the micro-crack self-healing mechanism in cement systems containing oil-absorbing resin or microcapsule.

Results and Discussion The median particle sizes (D50) of the oil-absorbing resin and the microcapsule were 5.601 μm and 6.590 μm, respectively. Within the temperature range of 0-213 ℃, both the oil-absorbing resin and the microcapsule exhibited almost no mass loss, demonstrating good thermal stability that met the requirements for cementing operations. Within the temperature range of 214-304 ℃, the mass loss rates for the oil-absorbing resin and the microcapsule were 95.45% and 35.84%, respectively, indicating superior thermal stability of the microcapsule. A vibrational absorption peak for    Si—OH was observed at a wavenumber of 941 cm-1, indicating that the oil-absorbing resin was encapsulated within the silica shell. The microcapsule possessed a large specific surface area, which helped improve their dispersion stability and interfacial bonding performance within the cement matrix. After 6 hours of oil absorption, the volume expansion rates of the oil-absorbing resin and the microcapsule were 100% and 10%, respectively, demonstrating the integrity and effectiveness of the silica shell encapsulation. The compressive strength of cement sample A1, incorporating microcapsule, reached its maximum value at a curing age of 7 days, indicating an optimal microcapsule dosage of 1%. After a self-healing curing age of 28 days, sample A1 exhibited a compressive strength of (29.06±1.61) MPa and a compressive strength recovery rate of 79.05%. Although both the oil-absorbing resin and microcapsule improved the compressive strength recovery capability of the cement stone, the incorporation of oil-absorbing resin led to a decrease in the overall compressive strength. Therefore, microcapsule was more suitable for the self-healing of micro-cracks in cement stone. After a self-healing curing age of 28 days, sample A1 showed a permeability of 0.563×10-3 μm2, representing a reduction of 39.36%, indicating a significant decrease in the permeability of the cement stone.

Conclusion The silica shell of the microcapsule possesses high reactivity, enabling it to participate in the cement hydration process and provide nucleation sites, thereby enhancing the compressive strength of the cement stone after damage and addressing the issue of strength reduction caused by the incorporation of oil‑absorbing resin. When a crack forms in cement containing microcapsules, the silica shell is fractured by the stress at the crack tip, exposing the internal oil‑absorbing resin. Upon contact with oil, the oil‑absorbing resin swells and becomes adsorbed and aggregated among the hydration products and pores, making the microstructure of the cement stone more uniform and dense, thereby effectively promoting the self‑healing process of the cement stone.

Keywords: oil well cement sheath; micro-crack self-healing; microcapsule; oil-absorbing resin; silica; permeability


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