壬基酚聚氧乙烯醚磷酸酯的合成

SYNTHESLS OF PHOSPHATE POLYOXYETHYLENE NONYL PHENOL

阐述了以壬基酚聚氧乙烯醚（ＮＰ－７）为起始剂，五氧化二磷为磷化剂，经直接酯化、水解制备壬基酚聚氧乙烯醚磷酸酯的合成条件。考察了五氧化磷的投料方式，原料配比，酯化温度和酯化时间对产品色泽，酯化率，双、单酯比例的影响，确定了最佳酯化条件：在４０℃强烈搅拌下分批投入五氧化二磷；ＮＰ－７／Ｐ２Ｏ５为３．２／１（ｍｏｌ／ｍｏｌ）；酯化温度７０～８０℃；酯化时间４．５～５．０ｈ。同时考察了聚磷酸酯的水解，确定了最佳水解条件：加水量为４％（ｇ／ｇ）；水解温度８０～９０℃；水解时间１．５～２．０ｈ，在该条件下，合成产品酯化率大于８８％；无机磷含量小于１％；泡沫高度达１３６ｍｍ。在条件实验基础上，确定了壬基酚聚氧乙烯醚磷酸酯的最佳合成条件。

In this parer the synthesis conditions for preparing phosphate polyoxyethylene nonyl phenol have been pxpounded with polyoxyethylene nonyl pheno(NP.7) as starting agent and phosphorus pentoxide as phosphorizating agent by direct esterification and hydrolysis. The effect is investigated for the feeding way of phosphorus pentoxide, raw materials made up, the temperature and the time on the colur, the yield, the diester and single ester proportion of the product for esterifying. The optimum feeding way was: the feeding at batches and stirring stongly at 40C. The optimum esterifying conditions were: NP 7/P 2O 5 3.2/1 (mol/mol); 70～80℃, 4.5～5.0h, and the optimum hydrolytic conditions were adding water 4%, 80～90℃, time: 1.5～20h. At the optimum conditions, the esterifying yield of the product was more than 88%, the inorganic phophorus was less than 1.0%, the foam height was up to 136mm. The synthesis conditions are determined for preparing phosphate polyoxyethylene nonyl phenol on the basis of experimental result.