定量核磁共振氢谱法测定苄基喹啉季铵盐产品中二聚体的含量  

Content determination of the dimer derivative in benzyl quinolinium quaternary ammonium salt by quantitative 1H NMR method

作　　者：王婧 胡华友[2] 杨震 刘思源 吴佳佳[4] 王业飞[1] Wang Jing;Hu Huayou;Yang Zhen;Liu Siyuan;Wu Jiajia;Wang Yefei(School of Petroleum Engineering,China University of Petroleum(East China),Qingdao,Shandong,China;School of Chemistry and Chemical Engineering,Huaiyin Normal University,Huaian,Jiangsu,China;Sichuan Changning Natural Gas Development Co.,Ltd.,Yibin,Sichuan,China;Key Laboratory of Marine Environmental Corrosion and Bio-fouling,Institute of Oceanology,Chinese Academy of Sciences,Qingdao,Shandong,China)

机构地区：[1]中国石油大学(华东)石油工程学院 [2]淮阴师范学院化学化工学院 [3]四川长宁天然气开发有限责任公司 [4]中国科学院海洋研究所海洋环境腐蚀与生物污损重点实验室

出　　处：《石油与天然气化工》2023年第2期87-92,共6页Chemical engineering of oil & gas

基　　金：国家重点研发计划政府间国际科技创新合作重点专项“新型环保表面成膜型缓蚀剂的缓蚀机理及应用”(2021YFE0107000);国家自然科学基金面上项目“基于吲哚嗪衍生物的新型酸化缓蚀剂及其作用机制研究”(52074339);山东省自然科学基金面上项目“基于可控释放型自生泡沫的低渗油藏增能-调驱一体化提高采收率方法”(ZR201911080151)。

摘　　要：目的苄基喹啉季铵盐(BQC)是一种常用的酸化缓蚀剂,其合成中的副产物苄基喹啉季铵盐二聚体(BQD)被发现对金属腐蚀具有更高效的缓蚀作用。为了明确合成产物中BQD的有效含量,建立了测定BQD含量的定量核磁共振氢谱法。方法通过合成并提纯得到了BQD,使用元素分析、质谱、核磁、红外等手段对其结构进行表征;以氘代氯仿作溶剂,选择化学位移在δ12附近的BQD单峰和化学位移在δ5附近的内标物二溴甲烷的单峰作为定量峰,根据两峰的面积之比,计算得到产物中BQD的有效含量。结果合成产物中BQD质量分数为11.6%,与加入BQD纯品的比对实验结论基本一致。结论建立的核磁共振氢谱内标法是一种简便、快捷、结果可靠的BQD含量检测方法。Objective Benzyl quinolinium quaternary ammonium salt(BQC)is a common acidizing corrosion inhibitor,but a derivative,benzyl quinoline quaternary ammonium salt dimer(BQD)was found in the synthesis process of BQC,which has more efficient corrosion inhibition effect on metal corrosion.In order to determine the effective content of BQD in the synthesis,a quantitative nuclear magnetic resonance hydrogen spectrum method was established for the determination of BQD content.Methods BQD was synthesized and purified,and its structure was characterized by elemental analysis,HPLC-HRMS,NMR and FT-IR.The effective content of the synthesized BQD product was studied by using CDCl 3 as solvent,and the proton signals peaked at aroundδ12 for BQD and aroundδ5 for CH 2Br 2 were selected as the quantification peaks.By comparing the area of the two peaks,the effective content of BQD in the product was calculated.Results The sample test results showed that the content of BQD was 11.6%,which was basically consistent with the experimental results of adding pure BQD.Conclusion The 1H NMR internal standard method established in this paper is a simple,rapid,and reliable method for determining BQD content in BQC.

关 键 词：酸化缓蚀剂 苄基喹啉季铵盐二聚体 核磁共振氢谱 

分 类 号：TE983[石油与天然气工程—石油机械设备] O657.2[理学—分析化学]