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交联聚乙烯醇制备工艺的优化及其在水泥浆中的热稳定性

Optimization of the Preparation Process of Crosslinked Polyvinyl Alcohol and Its Thermal Stability in Cementing Slurry.

作者信息

Li Junhao, Ai Haochen, Wang Qingchen, He Huifeng, Chang Xiaofeng, Chen Gang, Golian-Struhárová Alena, Slaný Michal, Qin Fangling

机构信息

Engineering Research Center of Oil and Gas Field Chemistry, Universities of Shaanxi Provence, Xi'an Shiyou University, Xi'an 710065, China.

Shaanxi Province Key Laboratory of Environmental Pollution Control and Reservoir Protection Technology of Oilfields, Xi'an Shiyou University, Xi'an 710065, China.

出版信息

Gels. 2025 Jan 30;11(2):98. doi: 10.3390/gels11020098.

Abstract

This study focuses on addressing the limitations of fluid loss additive in cement slurry under higher temperatures. The synthesis process of glutaraldehyde-crosslinked polyvinyl alcohol (PVA) was optimized to develop an efficient fluid loss additive for oil well cement slurries. Using one-factor experiments and the uniform design method, the optimal synthesis parameters were established: a reaction temperature of 50 °C; an acid concentration of 1 mol/L; a PVA mass concentration of 8%; a molar ratio of glutaraldehyde to PVA hydroxyl group of 1.47; and a crosslinking degree of 1.49%. The optimized crosslinked PVA demonstrated the ability to control API fluid loss within 50 mL when applied at 1% concentration in cement slurry under conditions of 30-110 °C and 6.9 MPa. Rheological analysis at medium and high temperatures revealed improved slurry properties, including smooth thickening curves and unaffected compressive strength. Further analyses, including thermogravimetric analysis (TGA), Zeta potential testing, and scanning electron microscopy (SEM), revealed that the crosslinked PVA hydrogel remained thermally stable up to 260 °C. Chemical crosslinking transformed the linear PVA into a network structure, enhancing its molecular weight, viscoelasticity, and thermal stability. This thermal resistance mechanism is attributed to the hydrogel's high-strength reticular structure which forms a uniform, dense, and highly stable adsorption layer, thereby improving both the additive's efficiency and the hydrogel's temperature resistance.

摘要

本研究着重解决高温下水泥浆体中降滤失添加剂的局限性。优化了戊二醛交联聚乙烯醇(PVA)的合成工艺,以开发一种高效的油井水泥浆降滤失添加剂。采用单因素实验和均匀设计方法,确定了最佳合成参数:反应温度50℃;酸浓度1mol/L;PVA质量浓度8%;戊二醛与PVA羟基的摩尔比1.47;交联度1.49%。优化后的交联PVA在30 - 110℃、6.9MPa条件下,以1%的浓度应用于水泥浆体时,能将API滤失量控制在50mL以内。中高温下的流变学分析表明,浆体性能得到改善,包括稠化曲线平滑且抗压强度不受影响。进一步的分析,包括热重分析(TGA)、Zeta电位测试和扫描电子显微镜(SEM),表明交联PVA水凝胶在高达260℃时仍保持热稳定性。化学交联将线性PVA转变为网络结构,提高了其分子量、粘弹性和热稳定性。这种耐热机理归因于水凝胶的高强度网状结构,该结构形成了均匀、致密且高度稳定的吸附层,从而提高了添加剂的效率和水凝胶的耐温性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/18c2/11854849/5b51872907fe/gels-11-00098-g001.jpg

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