第 50 卷第 6 期 Vol. 50 No. 6 2020 年 12 月 Dec 2020

所属栏目：表面活性剂 高酯化率壬基酚聚氧乙烯（9）醚磷酸酯的合成工艺研究

赵炯烽，金一丰，秦 飞，郏超伟 （浙江皇马科技股份有限公司，浙江 上虞 312369）

摘　要：以壬基酚聚氧乙烯（9）醚（NPEO-9）和P2O5等为原料，合成了壬基酚聚氧乙烯（9）醚磷酸酯。以反应体系的酯化率、磷酸单酯含量、无机磷酸含量等为指标，对反应条件进行优化，优化的工艺条件：在亚磷酸存在的情况下，n（NPEO-9）∶n（P2O5）=2.4∶1.0，通过分步升温（60 ℃反应1 h，70 ℃反应1 h，90 ℃真空脱水反应2 h）的方式进行酯化反应。酯化反应结束后，加入1%的水进行水解，得到NPEO-9残留量低于2%，无机磷酸低于2%的浅色壬基酚聚氧乙烯（9）醚磷酸酯。

关键词：壬基酚聚氧乙烯醚；NPEO-9；五氧化二磷；壬基酚聚氧乙烯醚磷酸酯

中图分类号：TQ450.4　　文献标识码：A　　文章编号：1009-9212（2020）06-0056-05

Process for the Synthesis of Nonylphenol Polyoxyethylene (9) Ether Phosphate with High Esterification Ratio

ZHAO Jiong-feng, JIN Yi-feng, QIN Fei, JIA Chao-wei (Zhejiang Huangma Technology Co.,Ltd., Shangyu 312369, China)

Abstract：Nonylphenol polyoxyethylene (9) ether (NPEO-9) and P2O5 were used as raw materials to synthesize nonylphenol polyoxyethylene(9) ether phosphate. Taking the esterification ratio, the content of phosphate monoester and inorganic phosphoric acid as indicators, the reaction conditions were optimized as followings: in the presence of phosphorous acid and the molar ratio of NPEO-9 to P2O5 was 2.4∶1.0, the esterification reaction was heated up step-by-step (60 ℃ for 1 h, 70 ℃ for 1 h, 90 ℃ for 2 h under vacuum). After the esterification was completed, 1% of water was added for hydrolysis to obtain a light-colored nonylphenol polyoxyethylene(9) ether phosphate with the residual NPEO-9 less than 2% and the inorganic phosphoric acid less than 2%.

Key words：nonylphenol polyoxyethylene ether; NPEO-9; phosphorus pentoxide; nonylphenol polyoxyethylene ether phosphate

作者简介：赵炯烽（1988—），男，浙江绍兴人，博士，主要从事表面活性剂的合成研究及产业化生产（E-mail：974435691@qq.com）。

收稿日期： 2020-12-0