抗温抗盐微球合成、优化及性能评价
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摘要
以丙烯酰胺(AM)、丙烯酸(AA)、2-丙烯酰胺-2-甲基丙磺酸(AMPS)和a-甲基苯乙烯(a-MSt)为聚合单体,采用二次反相乳液聚合法制备了抗温抗盐聚合物微球AMPST,并优化了微球的合成工艺。利用FTIR、GPC、光学显微镜、SEM、TG、流变分析仪以及岩心封堵实验对AMPST微球进行了结构表征与性能测试。结果表明,温度和AMPS含量与微球初始粒径大小密切相关,温度和引发剂含量决定了微球的膨胀倍数。在水化温度为65℃,地层模拟水矿化度为2.8937′10~3mg/L,合成温度为50℃,AMPS用量为15%(以水相中水的质量为基准,下同),合成的AMPST-8微球初始粒径中值为2.01mm,水化240 h后粒径中值为18.45mm,膨胀倍数为8.18。AMPST-8微球表面光滑,比表面大,呈聚集态;岩心封堵实验表明,AMPST-8微球在岩心内水化膨胀7 d后,残余阻力系数为8.4,封堵率88.00%,高于其他现场提供的微球。中试产品ZS-2微球岩心内水化膨胀7 d后,残余阻力系数7.8,封堵率87.24%。
Temperature-resistant and salt-tolerant polymer microspheres(AMPST) were prepared by inverse emulsion polymerization using acrylamide(AM), acrylic acid(AA), 2-acrylamide-2-methyl propane sulfonic acid(AMPS) and a-methyl styrene(α-MSt) as monomers. And the synthesis process of microspheres were optimized. The structure and performance of AMPST microspheres were characterized by FTIR, GPC, optical microscope, SEM, TG, rheological analyzer and core plugging experiments. The results showed that temperature and AMPS content were closely related to the initial particle size of microspheres, and temperature and initiator content determined the expansion ratio of microspheres. When the hydration temperature was 65 ℃ and the salinity of simulated formation water was 2.8937×10~3 mg/L,reaction temperature 50 ℃, dosage 15% of AMPS(based on the quality of water in aqueous phase, the same below), the average initial particle size of AMPST-8 microspheres was 2.01 μm, and 18.45 μm after240 hours of hydration, with an expansion ratio of 8.18. Furthermore, AMPST-8 microspheres had smooth surface, large specific surface exhibited an aggregate state. Core plugging experiments showed that the residual resistance coefficient of AMPST-8 microspheres was 8.4 and the plugging rate was 88.00% after 7 days of hydration expansion in the core, higher than other microspheres provided on site. After 7 days of hydration expansion, the residual resistance coefficient and plugging rate of pilot plant product, ZS-2 microspheres were 7.8 and 87.24%, respectively.
Temperature-resistant and salt-tolerant polymer microspheres(AMPST) were prepared by inverse emulsion polymerization using acrylamide(AM), acrylic acid(AA), 2-acrylamide-2-methyl propane sulfonic acid(AMPS) and a-methyl styrene(α-MSt) as monomers. And the synthesis process of microspheres were optimized. The structure and performance of AMPST microspheres were characterized by FTIR, GPC, optical microscope, SEM, TG, rheological analyzer and core plugging experiments. The results showed that temperature and AMPS content were closely related to the initial particle size of microspheres, and temperature and initiator content determined the expansion ratio of microspheres. When the hydration temperature was 65 ℃ and the salinity of simulated formation water was 2.8937×10~3 mg/L,reaction temperature 50 ℃, dosage 15% of AMPS(based on the quality of water in aqueous phase, the same below), the average initial particle size of AMPST-8 microspheres was 2.01 μm, and 18.45 μm after240 hours of hydration, with an expansion ratio of 8.18. Furthermore, AMPST-8 microspheres had smooth surface, large specific surface exhibited an aggregate state. Core plugging experiments showed that the residual resistance coefficient of AMPST-8 microspheres was 8.4 and the plugging rate was 88.00% after 7 days of hydration expansion in the core, higher than other microspheres provided on site. After 7 days of hydration expansion, the residual resistance coefficient and plugging rate of pilot plant product, ZS-2 microspheres were 7.8 and 87.24%, respectively.
引文
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[14]Min Jingli(闵敬丽).Synthesis and properties of polyacrylamide based thermo and salt tolerant polymers[D].Jinan:Shandong University(山东大学),2017.
[15]Pan Yuanjia(潘元佳).Preparation,characterization and application of novel functional polymer microspheres[D].Shanghai:Fudan University(复旦大学),2013.
[16]Zhao Yong(赵勇),He Binglin(何炳林),Ha Runhua(哈润华).Synthesis and properties of hydrophobically associating polyacrylamide in inverse microemulsion[J].Journal of Polymer Science(高分子学报),2000,(5):550-553.
[17]Lu Xiangguo(卢祥国).An experimental method for testing the swelling property of polymer microspheres in cores:CN107402286A[P].2017-11-28.
[18]Zhang Yuqi(张玉琦),Ma Rongyan(马荣延),Wei Qingbo(魏清渤),et al.Fabrication of core-shell polymer microspheres of P(St-AM)and the corresponding photonic crystals films[J].Journal of Polymer Science(高分子学报),2012,(6):648-652.
[19]Wang Dan(王丹).Study on water dispersible salt resistant polymer profile control agent[D].Xi'an:Shaanxi University of Science&Technology(陕西科技大学),2017.
[20]Cui Bo(崔波),Luo Wei(罗伟).Study on influencing factors of rheological properties of crosslinked polymer microspheres dispersion system[J].Application of Chemical Industry(应用化工),2009,38(5):635-659.
[21]Li Yahua(李雅华),Li Mingyuan(李明远),Lin Meiqin(林梅钦),et al.Rheological properties of crosslinked polymer microspheres dispersion system[J].Petroleum Geology and Recovery Efficiency(油气地质与采收率),2008,(3):93-95,117.
[2]Zhang Yanhui(张艳辉),Dai Caili(戴彩丽),Ji Wenjuan(纪文娟),et al.Profile control and flooding mechanism and application methods of polymer microsphere[J].Chemical Engineering of Oil&Gas(石油与天然气化工),2012,41(5):508-511,540.
[3]Wang Dailiu(王代流),Xiao Jianhong(肖建洪).Application of deep-profile control and displacement technology of cross-linked polymer micro ball system[J].Petroleum Geology and Recovery Efficiency(油气地质与采收率),2008,15(2):86-88.
[4]Han Xiuzhen(韩秀贞),Li Mingyuan(李明远),Guo Jixiang(郭继香),et al.Plugging property of linked polymer micro-spheres dispersed system[J].Journal of China University of Petroleum(Edition of Natural Science)(中国石油大学学报:自然科学版),2008,32(4):127-129.
[5]Wu Xingcai(吴行才),Han Dakuang(韩大匡),Lu Xiangguo(卢祥国),et al.Oil displacing mechanism of soft microgel particle dispersion in porous media[J].Earth Science(地球科学),2017,42(8):1348-1355.
[6]Wei Xin(魏欣),Jia Wenjun(加文君),Cao Jing(曹静),et al.Preparation of P(AM-AA-AMPS)polymer microspheres by inverse emulsion polymerization[J].Chemical Engineering of Oil&Gas(石油与天然气化工),2014,43(5):539-542.
[7]Wang Lei(王磊),Xue Rong(薛蓉),Zhao Yunpeng(赵云鹏),et al.Preparation and properties of core-shell polyacrylamide nanospheres[J].Fine Chemicals(精细化工),2018,35(3):517-524.
[8]Du Rongrong(杜荣荣),Liu Xiang(刘祥).Research on the microspheres of acrylamide copolymers made via inverse microemulsion polymerization[J].Chemical Industry and Engineering Progress(化工进展),2015,34(8):3065-3074.
[9]Ma Zhiguo(马智国),Wang Yonghe(王永鹤),Kang Hongyong(康宏元),et al.Synthesis and performance evaluation of a crosslinked polymer microsphere[J].Journal of Xi'an Shiyou University(Natural Science Edition)(西安石油大学学报:自然科学版),2014,29(4):84-88.
[10]Luo Qiang(罗强),Tang Ke(唐可),Luo Min(罗敏),et al.Migration properties of polymer microspheres in artificial conglomerate core[J].Petroleum Geology and Recovery Efficiency(油气地质与采收率),2014,21(1):63-65,115.
[11]Sun Huanquan(孙焕泉),Wang Tao(王涛),Xiao Jianhong(肖建洪),et al.Step wise deep profile control technology for new polymer microspheres[J].Petroleum Geology and Recovery Efficiency(油气地质与采收率),2006,(4):77-79,110.
[12]Lu Xiangguo(卢祥国),Song Helong(宋合龙),Wang Jingsheng(王景盛).Method for making heterogeneous cementation model of quartz sand epoxy resin:CN 200510063665.8[P].2005-09-07.
[13]Lu Xiangguo(卢祥国),Gao Zhenghuan(高振环),Yan Wenhua(闫文华).Experimental study on Influence Factors of artificial core permeability[J].Petroleum Geology and Development in Daqing(大庆石油地质与开发),1994,13(4):53-55.
[14]Min Jingli(闵敬丽).Synthesis and properties of polyacrylamide based thermo and salt tolerant polymers[D].Jinan:Shandong University(山东大学),2017.
[15]Pan Yuanjia(潘元佳).Preparation,characterization and application of novel functional polymer microspheres[D].Shanghai:Fudan University(复旦大学),2013.
[16]Zhao Yong(赵勇),He Binglin(何炳林),Ha Runhua(哈润华).Synthesis and properties of hydrophobically associating polyacrylamide in inverse microemulsion[J].Journal of Polymer Science(高分子学报),2000,(5):550-553.
[17]Lu Xiangguo(卢祥国).An experimental method for testing the swelling property of polymer microspheres in cores:CN107402286A[P].2017-11-28.
[18]Zhang Yuqi(张玉琦),Ma Rongyan(马荣延),Wei Qingbo(魏清渤),et al.Fabrication of core-shell polymer microspheres of P(St-AM)and the corresponding photonic crystals films[J].Journal of Polymer Science(高分子学报),2012,(6):648-652.
[19]Wang Dan(王丹).Study on water dispersible salt resistant polymer profile control agent[D].Xi'an:Shaanxi University of Science&Technology(陕西科技大学),2017.
[20]Cui Bo(崔波),Luo Wei(罗伟).Study on influencing factors of rheological properties of crosslinked polymer microspheres dispersion system[J].Application of Chemical Industry(应用化工),2009,38(5):635-659.
[21]Li Yahua(李雅华),Li Mingyuan(李明远),Lin Meiqin(林梅钦),et al.Rheological properties of crosslinked polymer microspheres dispersion system[J].Petroleum Geology and Recovery Efficiency(油气地质与采收率),2008,(3):93-95,117.
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