P2O5分散法合成十六烷基磷酸酯皮革加脂剂

以10#机油为分散剂均匀分散P2O5,并与十六醇进行磷酸化反应和水解反应,得到了低游离磷酸含量的十六烷基磷酸酯皮革加脂剂,解决了合成磷酸酯皮革加脂剂过程中P2O5易吸湿结块问题。通过正交实验对合成反应的条件进行了优化。结果表明,P2O5采用10#机油分散进料可提高产物中十六烷基磷酸酯的含量;当n(十六醇)∶n(P2O5)=2∶1,磷酸化反应较佳的条件为:m(10#机油)∶m(P2O5)=2∶1,磷酸化温度80℃,磷酸化时间3h;水解反应的较佳条件为:水解温度70℃,水解时间2 h,水用量2.0%(基于反应物的总质量)。在此优化反应条件下,产物中十六烷基磷酸单酯、双酯和游离磷酸的质量分数分别为65.2%、25.3%和9.5%。当10#机油与P2O5质量比大于2.5后,十六烷基磷酸酯加脂剂的乳液稳定性下降,加脂革柔软度降低。

Synthesis of Hexadecyl Phosphate Fatliquoring Agent from Hexadecanol and Phosphorus Pentoxide Dispersed in 10# Machine Oil

Hexadecyl phosphate fatliquoring agent was synthesized from P2O5 and hexadecanol through phosphorylation and hydrolysis.10# machine oil was used as dispersant for P2O5 in the phosphorylation to avoid aggregation of hygroscopic P2O5.When n(hexadecanol)∶n(P2O5)=2∶1,the optimum phosphorylation conditions are:mass ratio of 10# machine oil to phosphorus pentoxide 2∶1,reaction temperature 80 ℃ and reaction time 3 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 monohexadecyl phosphate,dihexadecyl phosphate and phosphoric acid in the product are 65.2%,25.3% and 9.5% respectively.When the mass ratio of 10# machine oil to P2O5 is greater than 2.5,stability of water emulsion of hexadecyl phosphate fatliquoring agent and softness of the oiled leather decline.