第45卷第4期
石油与天然气化工
CHEMICALENGINEERING OF OIL & GAS
抗高温聚合物压裂液复合交联剂的研制
陈效领’李帅帅1苏盈豪”胡儒丽”唐菲利”
1.中国石油集团西部钻探工程有限公司井下作业公司2.北京希涛技术开发有限公司
摘要根据高温聚合物压裂液对交联剂的要求，采用四氯化钛、氯氧化铬、乙酰丙酮（AAT）、马来酸(MA)、异丙醇(IPA)为主要原料，制备出一种高温压裂液用复合交联剂JL-1。利用单因素实验法对各物质配比、反应温度等交联剂的合成方案和条件进行了研究，确定了最佳合成方案；运用红外光谱、核磁共振等现代分析手段，对交联剂的结构进行了表征；评价了交联剂的综合应用性能。交联剂的最佳合成方案为:n(ZrOCl):n(TiCl）:n(MA）:n(AAT):n(IPA)=0.120:0.080:0.220:0.180: 0.440,络合剂滴加反应温度为5℃,反应时间为1.5h,60℃回流反应时间为5h。在交联液与交联剂质量比为100：0.7时，0.80%～1.0%（w)增稠剂XSS296压裂液交联黏度为0.80～1.49Pa·s；180 ℃、170。-"剪切1.5h后黏度为50mPa·s以上，交联压裂液具有良好的悬砂性和耐温耐剪切能力。
关键词压裂液有机错有机钛复合交联剂抗高温
中图分类号：TE357.1+2文献标志码：A
D0I:10.3969/j.issn.1007-3426.2016.04.013
Developmentof heatresistantcompoundcrosslinkingagent
used for polymerfracturing fluid
Chen Xiaoling',Li Shuaishuai',SuYinghao,Hu Ruli’,Tang Feili
(l. Downhole Seruice Com pany of Xibu Drilling Engineering Company Limited , CN PC, Karamay 834000, Chind 2. Beijing Xitao Polymer Co ., Ltd., Beijing 101300, China)
Abstract: According to the requirements of heat-resisting fracturing fluids, a compound crosslinking agent (JL-l) was synthesized by the copolymerization of ZrOCl2 , TiClt , acetylacetone, maleic acid, and isopropyl alcohol. The optimum reaction conditions were determined through studying the synthetic scheme and conditions of crosslinking agent by using the single factor experiment ; and the structure of crosslinking agent was characterized by infrared spectroscopy and'HNMR analysis; the comprehensive application performance of crosslinking agent was evaluated. The optimum conditions were as follows : the molar ratio of ZrOCl:: TiCl : MA : AAT : IPA was 1.20 : 0.800 : 0.220 : 0.180 : 0.440; the initial reaction temperature was 5 ℃ for 1.5 h and reflux reaction time was 3 h at the constant temperature of 6o C . The viscosity of the fracturing fluid with 0.80 wt%~1.0wt% thickening agent XSS296was about 0.80~1.49 Pa ·s when the crosslinking mass ratio was l00 : O.7. The final viscosity of fracturing fluid was above 50 mPa . s after continuously shearing 1.5 h at the speed of 170 s- under 180C. The fracturing fluid system has good shear resistant and heat resistant stability and sand-carrying performance .
Key words : fracturing fluid, organic zirconium , organic titanium , compound crosslinking agent , high temperature resistance
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基金项目：中国石油集团公司重大科技专项“重大工程关键技术与装备研究”子课题“储层改造工作液与关键工具研发”专题三“高温人工合成聚合物压裂液”（2014E-38-07)。
作者简介：陈效领（1975一），高级工程师，毕业于中国石油大学（北京），现就职于中国石油集团西部钻探工程有限公司井下作业公司，研究所所长，主要从事酸化压裂作业和管理工作。E-mail:chxl007@cnpe.com-cn