Improvement of Method for Measuring Degree of Cationic Substitution of Drilling Fluid Polymers
-
摘要: 四苯硼钠法是现有作为检测季铵盐阳离子度最为有效、广泛的方法之一,但该方法容易受到无机钾离子、铵离子等外界干扰和分子结构自身的影响,导致阳离子度测定结果的准确度较低。针对此问题,笔者对四苯硼钠返滴定法测定钻井液用聚合物阳离子度的方法进行改进,通过对样品采用90%~95%乙醇醇洗提纯,消除钾离子、铵离子和小阳离子单体的干扰;加入H2O2,通过进行热氧降解降低分子量,减弱分子结构的影响;优化出以下测定条件:样品加量为0.2 g、沉淀pH值3.0~4.0、沉淀温度为15~25℃和滴定pH值为7.0~8.0等,从而提高四苯硼钠测定方法的准确性。结果表明,四苯硼钠返滴定法的检出限量为0.1 g,加标回收率达到了分析测试要求的加标回收率指标,说明该方法具有良好的准确度。Abstract: Testing the degree of cationic substitution of quaternary ammonium salts with sodium tetraphenylborate (STB) is one of the most effective methods that have been widely used. The drawbacks of this method are that the interference of inorganic potassium ions and ammonium ions, as well as the molecular structure of the samples make the test inaccurate to some extent. Studies have been conducted on the improvement of the accuracy of the STB method by eliminating ionic interferences to the STB method, optimizing the test conditions of the STB method and investigating the effects of the molecular structure of polymers on the measurement of cationic substitution. In laboratory tests, the polymer samples were purified with 90%-95% ethanol to eliminate interference from potassium ions, ammonium ions and low molecular weight (MW) cationic monomers from outside. The mass of sample was determined to be 0.2 g, pH value for the precipitation between 3.0 and 4.0, temperature for precipitation between 15℃ and 25℃, and pH value for titration between 7.0 and 8.0. H2O2 was used at a certain temperature to reduce the MW of polymers to minimize the effects of molecular structure on the test accuracy of test, thereby improving the accuracy of the STB method. The test results show that the modified STB method has good feasibility and accuracy; the identification limit of the test is 0.1 g, and recovery rate 92%-94%.
-
Key words:
- Drilling fluid /
- Polymer Degree of cationic substitution /
- Sodium tetraphenylborate /
- Testing /
-
[1] 关建宁,张金俊,万嵘,等. 四苯硼钠反滴法测季铵内盐的含量[J]. 南京工业大学学报(自然科学版), 2007,29(2):82-84. GUAN Jianning,ZHANG Jinjun,WAN Rong,et al. Reverse titration for the determ ination of amphoteric inner quatemary ammonium with four benzene boron sodium[J]. Journal of Nanjin University of Technology (Natural Science Edition),2007,29(2):82-84. [2] 李彦,谢娟,屈撑园,等. 四苯硼钠返滴定法测定季铵盐研究[J]. 西安石油大学学报(自然科学版), 2009,24(4):62-64. LI Yan,XIE Juan,QU Zhangyuan,et al.Reverse titration for the determination of amphoteric quatemary ammonium with four benzene boron sodium[J]. Journal of Xi an Shiyou University(Natural Science Edition), 2009,24(4):62-64. [3] 王孟,申迎华. 阳离子聚丙烯酰铵表征及其阳离子度测定方法[J]. 太原理工大学学报,2004,35(4):495-497.WANG Meng,SHEN Yinghua.Structural character and method of determining cationic degree of cationic polyacrylamide[J].Journal of Taiyuan University of Technology,2004,35(4):495-497. [4] 雷祖猛,司西强. 钻井液用阳离子烷基糖苷阳离子度的测定[J]. 能源化工,2016,37(2):32-34.LEI Zumeng,SI Xiqiang.Determination of cationic degree for cationic alkyl polyglycoside in drilling fluid[J]. Energy Chemical Industry,2016,37(2):32-34. [5] 郑怀礼,苗树祥,朱俊任,等. 阳离子聚丙烯酰铵P(AM-DAC)阳离子度的测定[J]. 重庆大学学报, 2014,37(1):110-116.ZHENG Huaili,MIAO Shuxiang,ZHU Junren, et al.Determination of cationic degree in cationic polyacrylamide P(AM-DAC)[J]. Journal of Chongqing University,2014,37(1):110-116. [6] 杜娜,龙毅,王磊,等. 阳离子型聚丙烯酰铵离子度测定方法的研究[J]. 中华纸业,2013,34(2):25-27.DU Na, LONG Yi,WANG Lei,et al. A study on determination for cationic degree of cationic polyacrylamide[J].China Pulp & Paper,2013,34(2):25-27. [7] 贾启高,杨建军,吴修刚,等. 阳离子褐煤中腐殖酸及阳离子含量测定方法[J]. 山东化工,2011,40(7):42-45.JIA Qigao,YANG Jianjun,WU Xiugang,et al.Testing method for the contents of humic acid and cation in cationic lignite[J].Shandong Chemical Industry,2011, 40(7):42-45. [8] 黄伟琴,周姝娜,沈丽萍,等. 钻井液用阳离子磺甲基酚醛树脂阳离子度的测定方法初探[J]. 中国石油和化工标准与质量,2007(12):34-37. HUANG Weiqin,ZHOU Shuna,SHEN liping,et al. Determination of cationic degree for cationic sulfonated phenolic resin in drilling fluid[J].China Petroleum and Chemical Standard and Quality,2007(12):34-37. [9] 周姝娜,湛玉玲,黄伟琴,等. 磷钨酸法测定钻井液材料中有机阳离子的探讨[J]. 油田化学,2013,30(2):280-282.ZHOU Shuna,ZHAN YuLing,HUANG Weiqin,et al. Tudiesonthe phos photungstic acid methodto determinethe organic cationsof rilling fluid materiais[J].Qilfield Chemistry,2013,30(2):280-282. [10] 王薇,杨新浩. 四苯硼酸钠季铵盐容量法测定钾的改进[J]. 山东海洋学院学报,1985,15(2):27-32.WANG Wei,YANG Xinhao.An improvement of volumetric method for determination of potassium with sodium tetraphenylboron and quaternary[J].Journal of Shandong College of Oceanology,1985,15(2):27-32. [11] 张祥兆. 钻井液用聚丙烯酰铵钾盐中钾含量测定的不确定度评定[J]. 石油工业技术监督, 2011,27(5):38-42.ZHANG Xiangzhao.The evaluation of the uncertainty about the measurement of potassium content in drilling fluid of polyarylamide potassium salt[J].The Chnology Supervision In Petroleum Industry,2011,27(5):38-42. [12] 李尧. 四苯硼钠-季铵盐容量法测钾含量误差分析[J]. 煤炭与化工,2014,37(7):111-112LI Yao.Four benzene boron sodium-quaternary ammonium salt capacity method of potassium content measurement[J].Error Analysis Coal and Chemical Industry,2014,37(7):111-112. [13] 霍春梅. 重量法与容量法测定钾含量的比较[J]. 盐与化工,2015,44(1):9-10.HUO Chunmei. Comparison of Gravimetric and Volumetric Method for Potassium Content Determination[J]. Journal of Salt and Chemical Industry, 2015,44(1):9-10. [14] 戴春亭,周姝娜. 双氧水降解法测定聚丙烯酰铵钾盐中钾的含量[J]. 油田化学,1999,16(4):308-309.DAI Chunting,ZHOU Shuna.Determinating potassium in potassium salt of partially hydrolyzed polyacrylamide by hydrogen peroxide degradation method[J].Qilfield Chemistry,1999,16(4):308-309. [15] 吴树宏,周春华. 加标回收率计算方法的探讨[J]. 甘肃环境研究与监测,2000,13(3):179-183.WU Shuhong,ZHOU Chunhua.Discussion on calculation of recovery[J].The administration and Technique of Environmental Monitoring,2000,13(3):179-183. [16] 王茂功,陈帅,李彦琴,等. 新型抗高温油基钻井液降滤失剂的研制与性能[J]. 钻井液与完井液,2016, 33(1):1-5.WANG Maogong,CHEN Shuai,LI Yanqin,et al. Development and envaluation of a new high temperature filter loss reducer used in oil base drilling fluid[J].Drilling Fiuid & Completion Fluid,2016,33(1):1-5. [17] 张国,徐江,詹美玲,等. 新型聚胺水基钻井液研究及应用[J]. 钻井液与完井液,2013,30(3):23-26.ZHANG Guo,XU Jiang,ZHAN Meiling,et al. Research and application of polyamine water-based drilling fluid system[J].Drilling Fluid & Completion Fluid,2013,30(3):23-26.
点击查看大图
计量
- 文章访问数: 576
- HTML全文浏览量: 158
- PDF下载量: 155
- 被引次数: 0