摘要
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。
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.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2008年第9期890-893,899,共5页
Fine Chemicals
基金
浙江省科技厅重大科技攻关项目(2004C11032~~