油基压裂液用磷酸酯胶凝剂的室内合成

摘要

Using triethyl phosphate and phosphorus pentoxide as raw materials produced polyphosphate intermediates, and then generated dialkyl alkyl phosphate intermediates with the mixtures of n-butanol, n-octanol and n-octadecanol. By orthogonal designs ,changing the time, temperature, materials ratio and other reaction conditions to explore the optimal reaction conditions. The results show that the optimal reaction conditions of the phosphate monoester＇s production are that： the mole ratio of triethyl phosphate and phosphorus pentoxide is 1.25：1, reaction temperature is 85℃, reaction time is 6 h. The dialkyl phosphate＇s best reaction conditions are that： the mass fractions of n-butanol, n-octanol, n-octadecanol respectively is 7.78 %, 33.51%, 58.71%, the mole ratio of them and phosphorus pentoxide is 3.8：1, reaction temperature is 98 ℃, reaction time is 8 h. When the concentration of phosphate gellant is 2.0 %, the oil based fracturing fluid＇s viscosity is high to 359.5 mPa.s after being crosslinked,which is easy to break and flowback.%以磷酸三乙酯和五氧化二磷为原料反应生成聚磷酸酯中间体，进而与正丁醇、正辛醇和十八醇的混合醇反应生成二烷基磷酸酯。通过设计正交实验，改变反应时间、反应温度、物料配比，优化合成工艺条件。实验结果表明：磷酸单酯的最佳反应条件是磷酸三乙酯与五氧化二磷的摩尔比为1．25：1，反应温度85℃，反应时间6h；二炕基磷酸酯的最佳反应条件是正丁醇、正辛醇和十八醇的质量分数分别为7．78％、33．51％和58．71％，中高碳醇与五氧化二磷的摩尔比3．8：1，反应温度98℃，反应时间8h。磷酸酯增稠剂的的浓度为2．0％时，配制的油基压裂液的最大粘度为359．5mPa·s，且破胶容易，易返排。