高碳醇磷酸酯加脂剂的合成与分析

以高碳醇为原料，采用P2O5溶剂法合成磷酸酯。探讨了P2O5溶剂的选择原则，确定10^#机油作为P2O5的分散溶剂，其10^#机油与P2O5质量比为2．5：1．0。实验表明，P2O5溶剂法解决了P2O5传统法加料时易吸潮、结块、炭化、反应不均匀和反应初期过于激烈等缺陷；其反应产物中磷酸单双酯的摩尔比、高碳醇转化率及总酸值均比传统法有了明显的提高，且产物色泽浅于P2O5传统法合成的磷酸酯；水解反应能进一步提高产物中磷酸单双酯的摩尔比和高碳醇转化率，水解后磷酸单双酯的摩尔比由3．96上升到4．16．高碳醇转化率由81．5％提高到88．7％。电位滴定法分析测定磷酸酯组分含量时发现，氯化钙溶液(10％)的最低加入量为11．0mL。

Synthesis and analysis of higher alcohol phosphate fat-liquor

Alkyl phosphate was prepared by higher alcohol and P_2O_5 in a solvent.The selection of the solvent was studied.10~# machine oil is selected as dispersing solvent,with a mass ratio of 10~# machine oil to P_2O_5 of 2.5 to 1.The experiment shows that solvent method resolves some problems in the traditional way including moisture absorption,caking and carbonization of the reactant,non-uniform reaction and too high reaction rate at initial stage.The molar ratio of mono-phosphate to di-phosphate,conversion rate of higher alcohol as well as total acid value and the color of the reaction product siginificantly improved than that obtained by traditional method.Hydrolysis reaction can further improve the molar ratio of mono-phosphate to di-phosphate and conversion rate of higher alcohol in its reaction product from 3.96 to 4.16 and from 81.5 % to 88.7 % respectively.In determining composition of phosphate by means of potentiometric method,the minimun dosage of calcium chloride solution (10 %)is 11.0 mL.