响应曲面法优化曼尼希碱缓蚀剂的合成工艺

Optimization of the Synthesis Process of Mannich Base by Response Surface Method

采用响应曲面分析法对一种曼尼希碱的合成工艺进行优化。该曼尼希碱由曼尼希反应和季胺化反应合成得到。以Box-Behnken设计评价胺酮比、醛酮比、反应温度、pH和时间5个因素的显著性和交互作用分析,得出一种曼尼希碱的最佳合成条件为:胺酮比1.02,醛酮比1.066,反应温度67.2℃,pH为3.46和时间2.96 h,该条件下将这种曼尼希碱添加到腐蚀介质中后的腐蚀速率为0.02 g/(m^2·h)。本文采用响应曲面法建立的模型较准确,可以较准确的得出一种曼尼希碱在合成过程中5个因素的交互作用及其最高效的合成条件,为曼尼希碱合成效率的提高提供一定参考价值。

A Mannich base synthesis process was optimized by response surface analysis. The Mannich base was obtained via Mannich reaction and quaternary amination reaction. Taking amine-ketone ratio, aldehyde-ketone ratio, reaction temperature, pH and reaction time as experimental factors, based on the analysis of significance and interaction among different factors, the optimal condition of synthesis process was obtained as followed: the ratio of amine to ketone 1.02, the ratio of aldehyde to ketone 1.066, the reaction temperature 67.2 ℃, the pH 3.46 and the time 2.96 h. Mannich base was obtained under the optimal condition and its corrosion rate was 0.02 g·(m^2·h^-1) in corrosion medium. The model established by response surface methodology is accurate after model verification. The synthesis process of Mannich base and established model can provide reference value for synthesis of Mannich base.