10~#机油分散的P_2O_5与十二醇反应合成十二烷基磷酸酯

Synthesis of Dodecyl Phosphate from Lauryl Alcohol and Phosphorus Pentoxide Dispersed in 10~# Machine Oil

以10#机油为分散剂均匀分散P2O5,并与十二醇进行磷酸化反应和水解反应得到了高收率的十二烷基磷酸酯;比较了P2O5采用10#机油分散进料和直接粉状进料时的产物组成;通过正交实验对合成反应的条件进行了优化。实验结果表明,P2O5采用10#机油分散进料可提高产物中十二烷基磷酸酯的含量;磷酸化反应较佳的条件为:m(10#机油)∶m(P2O5)=1.5,n(十二醇)∶n(P2O5)=2.0,磷酸化温度80℃,磷酸化时间4h;水解反应较佳的条件为:水解温度70℃,水解时间2h,水用量2.0%(基于反应物的总质量)。在此条件下,产物中十二烷基磷酸单酯、双酯和游离磷酸的质量分数分别为66.12%,24.60%,9.28%。该方法解决了反应中P2O5易吸湿结块的问题。

Dodecyl phosphate was synthesized from P2O5 and lauryl alcohol through phosphorylation and hydrolysis. 10^# Machine oil was used as dispersant of P2O5 in the phosphorylation to avoid aggregation of hygroscopic P2O5, The corresponding reactions of lauryl alcohol with powder P2O5 and with P2O5 dispersed in 10^# machine oil were compared. Conditions reaction between lauryl alcohol and P2O5 dispersed in 10^# mineral oil were studied by orthogonal experiments. The optimum phosphorylation conditions are： mass ratio of 10^# machine oil to phosphorus pentoxide 1.5, mole ratio of lauryl alcohol to phosphorus pentoxide 2, 0, reaction temperature 80 ℃ and reaction time 4 h. The optimum hydrolysis conditions are： reaction temperature 70 ℃, reaction time 2 h and water mass fraction 2.0% （ based on total mass of reaction materials）, Under the optimum conditions, the mass fraction of monododecyl phosphate,didodecyl phosphate and phosphoric acid in products are 66.12% ,24.60% and 9.28%, respectively. Dispersing of P2O5 in 10^# machine oil avoids aggregation of hygroscopic P2O5 and can increase conversion of P2O5.