有机锆交联魔芋葡甘聚糖凝胶的制备及性能  

Preparation and Properties of Organic Zirconium Crosslinked Konjac Glucomannan Gel

作　　者：姜启运 陈俊杰[1] 陈豪 吴志强 沈春晖[1] 高山俊[1] JIANG Qi-Yun;CHEN Jun-Jie;CHEN Hao;WU Zhi-Qiang;SHEN Chun-Hui;GAO Shan-Jun(School of Materials Science and Engineering,Wuhan University of Technology,Wuhan 430000,China)

机构地区：[1]武汉理工大学材料科学与工程学院,武汉430000

出　　处：《应用化学》2023年第10期1437-1447,共11页Chinese Journal of Applied Chemistry

摘　　要：以正丁醇锆为中心离子试剂,分别以3-氨基-1,2-丙二醇(APG)和N-甲基二乙醇胺(MDEA)为有机配体制备两种正丁醇锆交联剂,用魔芋葡甘聚糖(KGM)溶液与正丁醇锆交联剂制备了一系列水基压裂液。通过傅里叶变换红外光谱仪(FT-IR)、核磁共振波谱(NMR)、高分辨质谱(HRMS)、流变仪、扫描电子显微镜(SEM)和差示扫描量热仪(DSC)系统地表征了压裂液的结构、形貌以及性能。讨论了锆酸盐与植物胶发生交联的反应途径,并运用Winter-Chambon公式准确确定溶胶-凝胶转变点。研究了反应物浓度、配体种类对储能模量(G′)、损耗模量(G″)和溶胶-凝胶转变时间(tcr)的影响。结果表明,相较于APG配体,以MDEA为配体的有机锆/KGM凝胶体系的延迟交联性能、耐温耐剪切性能更好,其tcr随KGM质量浓度的增大呈先减小后增大的趋势,并且随配体浓度和交联剂质量分数的增加呈减小趋势,KGM质量浓度控制在4.0 g/L时,凝胶体系的常温延时交联时间在7~45 min内可调节,溶胶-凝胶转变温度(T_(sol-gel))为71.4℃,其耐温性能高达120℃,在170 s^(-1)剪切速率条件下能保持171 mPa·s的粘度。该有机锆交联KGM凝胶体系为石油开采领域的研究和应用提供有益借鉴。Two n-butanol zirconium crosslinkers were prepared using n-butanol zirconium as the central ionic reagent and 3-amino-1,2-propanediol(APG)and N-methyldiethanolamine(MDEA)as the organic ligands,respectively.A series of water-based fracturing fluids were prepared with konjac glucomannan(KGM)solution and n-butanol zirconium crosslinker The morphology,structure and properties of fracturing fluid are systematically characterized by Fourier transform infrared spectrometry(FT-IR),nuclear magnetic resonance spectroscopy(NMR),high resolution mass spectrometer(HRMS),rheometer,scanning electron microscopy(SEM),and differential scanning calorimeter(DSC).The reaction pathway of zirconate and KGM crosslinking is discussed.The sol-gel transition point is accurately determined by Winter-Chambon formula.The effects of reactant concentration and ligand species on storage modulus(G′),loss modulus(G″),and solgel transition time(tcr)are studied.It is found that compared with APG ligand,the organozirconium/KGM gel system with MDEA as ligand have better delayed cross-linking performance,better temperature and shear resistance.Its tcr shows a trend of first decreasing and then increasing with the increase of KGM concentration,and a decreasing trend with the increase of ligand concentration and crosslinking agent concentration.When the concentration of KGM solution is controlled at 4.0 g/L,the delay time of gel system can be adjusted within 7~45 min at room temperature,the sol-gel transition temperature(T_(sol-gel))is 71.4℃,and its temperature resistance can reach 120℃.The viscosity of 171 mPa·s is maintained at a shear rate of 170 s^(-1).The organic zirconium crosslinked KGM gel system provides a useful reference for the research and application in the field of petroleum exploitation.

关 键 词：魔芋葡甘聚糖 正丁醇锆 配位 延迟凝胶化 动态流变性能 

分 类 号：O636.1[理学—高分子化学]