基于正交试验设计的十三聚铝[Al13]7+含量多因素优化研究

采用碱中和滴定法合成羟基铝的过程中影响十三聚铝Al₁₃]₇₊含量的因素较多,本文选取了总铝浓度、碱化度、反应温度和碱化率等4个主要因素进行了综合优化研究,分析各因素的敏感性影响程度,最终确定合成Al₁₃]₇₊的最佳条件组合。对4个因素分别选取了代表性的3个水平,运用正交试验设计原理建立了9组实验方案,根据确立的方案合成羟基铝溶液并进行₂₇Al-NMR检测,然后以各铝形态的含量为指标进行极差分析。分析结果表明,4个因素中碱化度影响最显著,总铝浓度次之,反应温度和碱化率显著性较弱；合成Al₁₃]₇₊的最佳因素组合为总铝浓度为0.1 mol/L、反应温度为60 ℃、碱化度为2.5和碱化率为50 ml/min。

Experimental research on multi-factor optimization of the [Al13]7+ content based on orthogonal experimental design

The content of Al13]7+ is affected by many factors in the process of alkali neutralization titration method for synthesis of hydroxy aluminum solution. In this paper, four major factors, including total aluminum concentration, molar ratio of OH- to Al3+, reaction temperature and the rate of alkalization, are chosen for multi-factor optimization to study the influence degree of the four factors. Three levels are set for each factor and nine test schemes are made based on the principle of orthogonal experimental design. The hydroxy aluminum solution is then synthetized and examined by 27Al-NMR analysis. After that, experimental index of the content of aluminum species is selected for extreme difference analysis. The research results show: among four factors, the molar ratio of OH- to Al3+ has the most significant influence, the total aluminum concentration is in the second place and reaction temperature and the rate of alkalization is the third. The optimal Al13]7+ content form: the total aluminum concentration is 0.1mol/L, the reaction temperature is 60 deg.c, the molar ratio of OH- to Al3+ is 2.5 and the rate of alkalization was 50ml/min.