Study on Optimization of Method for Measuring the Content of Potassium Salt of Polyacrylamide in Drilling Fluids
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摘要: 聚丙烯酰胺钾盐是钻井液行业广泛应用的一种阴离子型聚合物。按照SY/T 5946—2002推荐方法进行检测过程中,存在无机盐对纯度的检测影响、特性黏数测定使用的易制爆化学品硝酸钠管理要求高、氯离子测定偏差较高等问题。在纯度检测的基础上采用乙醇加盐酸洗溶液,优化灼烧残渣的温度和时间,特性黏数测定使用氯化钠代替硝酸钠,氯离子含量测试优化样品处理和滴定pH值等方法和措施,提高聚丙烯酰胺钾盐技术指标检测的准确性。结果表明,纯洗溶液中加入1.5%盐酸,增加了含量无机盐的溶解,样品纯度甑别率提高40%;800℃灼烧3 h残渣含量能够较真实地体现样品的有效含量;采用氯化钠代替硝酸钠进行特性黏数测试,结果偏差范围为(0~0.40)/100 mL/g;氯离子测试过程中,高温灼烧处理样品,并增加了调整滴定溶液pH值,平行样间偏差由1.02%~1.73%降至0~0.18%之间。通过上述测试方法的优化,提高了聚丙烯酰胺钾盐技术指标检测结果的准确性和精确度,为该产品的质量控制提供了行之有效的检测依据。Abstract: The potassium salt of polyacrylamide (PAM) is a widely used anionic polymer. In examining the quality of this polymer in accordance with the standard SY/T 5946—2002, several factors affect the final results, for example, the purity of the polymer is affected by inorganic salts existed in the process of examination, sodium nitrate used to measure the intrinsic viscosity is a kind of easy-to-explode substance and requires high level of control, and there is a big error in the determined chloride ions concentration. The procedure of examining the quality of the potassium salt of PAM was modified in our laboratory experiment. In measuring the purity of the polymer in laboratory, ethanol and hydrochloric acid as the washing liquid. The temperature and time for residue ignition were optimized. Sodium chloride was used to replace the sodium nitrate in measuring the intrinsic viscosity. In measuring the chloride ions content, the treatment of the sample was optimized and the pH of the sample was measured with titration method. All these measures helped improve the accuracy of the examination. It was found in the experiment that by adding 1.5% hydrochloric acid in the pure washing liquid, the solubility of the inorganic salt in the sample was increased, and the parting rate of the purity of the sample was thus increased by 40%. The residue of the sample was ignited at 800 ℃ for 3 hours, in so doing the real effective content of the sample can be measured. When using NaCl to replace NaNO3 in the measurement of the intrinsic viscosity, the range of variation of the results was (00.40)/100 mL/g. In the measurement of chloride ions concentration, the sample was ignited at elevated temperatures and the pH value of the titration solution was adjusted, thus the variation of the results between parallel measurements was reduced from 1.02% - 1.73% to 0.0018%. These optimization measures help improve the accuracy and precision of the measurement, providing an effective base for examining the product quality of the potassium salt of PAM.
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[1] GB 12005.1-89《聚丙烯酰胺特性黏数测定方法》[S]. GB 12005.1-89 Determination for limiting viscosity number of polyacrylamide[S]. [2] GB/T 1632.1-2008《塑料使用毛细管黏度计测定聚合物稀溶液黏度第1部分:通则》[S]. GB/T 1632.1-2008Plastics-Determination of the viscosity of polymers in dilute solution using capillary viscometers viscometers-Par 1:General principles[S]. [3] SY/T 5946-2002《钻井液用聚丙烯酰胺钾盐》[S]. SY/T 5946-2002Potassium polyacrylamide for drilling fluid[S]. [4] Q/SH 0048-2007《钻井液用聚丙烯酰胺钾盐技术要求》[S]. Q/SH0048-2007Technical requirements for Polyacrylamide potash for drilling fluids[S]. [5] 王中华著. 钻井液处理剂实用手册[M]. 北京:中国石化出版社,2016:235-247. WANG Zhonghua. Practical manual for drilling fluid treatment agent[M].Beijing:China Petrochemical Press, 2016:235-247. [6] 张运峰.钻井液用聚丙烯酰胺钾盐检测标准对比分析与检测方法探讨[J]. 石油工业技术监督,2011(5):21-33. ZHANG Yunfeng.Comparative analysis of testing standard for Polyacrylamide potassium salt for drilling fluid and discussion of testing method[J].Technical Supervision of Petroleum Industry,2011(5):21-33. [7] 常兴伟. 采出液中氯离子含量检测影响因素研究及检验方法改进[J]. 化学工程与装备,2017(2):240-241. CHANG Xingwei.Research to the influential factors of chlorine ion in the produced fluid testing and inspection method improvement[J].Chemical Engineering and Equipmen,2017(2):240-241.
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