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

所屬欄目:表面活性劑

高酯化率壬基酚聚氧乙烯(9)醚磷酸酯的合成工藝研究
趙炯烽,金一豐,秦 飛,郟超偉 (浙江皇馬科技股份有限公司,浙江 上虞 312369)
摘 要:以壬基酚聚氧乙烯(9)醚(NPEO-9)和P2O5等為原料,合成了壬基酚聚氧乙烯(9)醚磷酸酯。以反應體系的酯化率、磷酸單酯含量、無(wú)機磷酸含量等為指標,對反應條件進(jìn)行優(yōu)化,優(yōu)化的工藝條件:在亞磷酸存在的情況下,n(NPEO-9)∶n(P2O5)=2.4∶1.0,通過(guò)分步升溫(60 ℃反應1 h,70 ℃反應1 h,90 ℃真空脫水反應2 h)的方式進(jìn)行酯化反應。酯化反應結束后,加入1%的水進(jìn)行水解,得到NPEO-9殘留量低于2%,無(wú)機磷酸低于2%的淺色壬基酚聚氧乙烯(9)醚磷酸酯。
關(guān)鍵詞: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
中圖分類(lèi)號:TQ450.4  文獻標識碼:A  文章編號: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
作者簡(jiǎn)介:趙炯烽(1988—),男,浙江紹興人,博士,主要從事表面活性劑的合成研究及產(chǎn)業(yè)化生產(chǎn)(E-mail:974435691@qq.com)。
收稿日期: 2020-12-0
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