对氟苯甲酸乙酯油溶性示踪剂的制备与溶解性能研究
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Preparation and Solubility Property of Ethyl 4-Fluorobenzoate as Oil Soluble Tracer
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    摘要:

    针对油田用油溶性示踪剂种类少的情况, 根据含氟有机化合物性质稳定、 检测灵敏度高的特点, 通过氯化亚砜法和浓硫酸催化法两种方法合成对氟苯甲酸乙酯 (EB-F), 用核磁共振氢谱和质谱对产物结构进行了表征,根据高效液相色谱测得的色谱峰面积计算得到 EB-F在水和煤油中的溶解度, 通过 EB-F标准曲线的建立获得气质联用仪测定 EB-F浓度的检测下限。结果表明, 氯化亚砜法和浓硫酸催化法的产品收率约为 86%, 浓硫酸催化法操作简便、 成本低, 对环境污染小, 更适合工业化生产。EB-F 在油中易溶, 在水中微溶, 在煤油和水中的溶解度分别为 90 和 0.051 g/L, 油水分配比为 338。用气质联用仪可以对 EB-F 乙腈溶液进行痕量检 测, 标准曲线的线性范围为 0.1×10-3~ 50×10-3 mg/L, R2为 0.9984, 相对标准偏差 RSD为 4.1%, 最低检测限为 1.5×10-6mg/L。图3参 12

    Abstract:

    Aiming at the fact that there were few species of oil soluble tracer used in oilfield and according to the properties of organofluorine compound with stability and high sensitivity, ethyl 4-fluorobenzoate(EB-F)was synthesized by thionyl chloride method and concentrated sulfuric acid catalysis method. The structure of the product was characterized by 1H NMR and mass spectrometry. The solubility of EB-F in water and kerosene was researched through chromatographic peak area which detected by HPLC. And the detection limit of EB-F concentration by GC-MS instrument was determined by the establishment of standard curve. The results showed that the product yield of thionyl chloride method and concentrated sulfuric acid catalysis method was about 86%. Compared with thionyl chloride method, concentrated sulfuric acid catalysis method was easier to operate, had lower cost and less pollution to environment, and was more suitable for industrial production. EB-F was soluble in oil and slightly soluble in water. The solubility in kerosene and water was 90 and 0.051 g/L respectively, and the oil-water partition ratio was 338. Trace amount of EB-F acetonitrile solution could be detected by GC-MS with 0.1×10-3—50×10-3 mg/L linear range of standard curve, 0.9984 R2, 4.1% RSD, and 1.5×10-6mg/L minimum detection limit

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孟科全, 温守国, 王跃宽, 陈维余, 尹瑞娟, 江 涛.对氟苯甲酸乙酯油溶性示踪剂的制备与溶解性能研究[J].油田化学,2018,35(1):161-164.
MENG Kequan, WEN Shouguo, WANG Yuekuan, CHEN Weiyu, YIN Ruijuan, JIANG Tao. Preparation and Solubility Property of Ethyl 4-Fluorobenzoate as Oil Soluble Tracer[J]. OILFIELD CHEMISTRY,2018,35(1):161-164.

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  • 在线发布日期: 2018-04-26
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