全氟烃基季铵盐的微波合成

Microwave Synthesis of a Perfluoroalkyl-Containing Quaternary Ammonium Salt

以全氟己基乙基碘和N-甲基二乙醇胺(MDEA)为原料,通过微波合成技术制备了全氟己基乙基甲基二羟乙基碘化铵。通过傅里叶变换红外光谱、质谱和核磁共振氟谱对产物的结构进行表征。通过单因素实验探讨了溶剂用量、微波功率、反应物摩尔比和反应时间对MDEA转化率的影响。采用三因素三水平的响应面分析法,通过建立N-甲基二乙醇胺的转化率与各因素之间的Central-Composite数学模型,对其合成工艺进行优化。全氟烃基季铵盐表面活性剂的最佳合成工艺条件为:0.015 mol全氟己基乙基碘、0.01 mol MDEA、溶剂用量为50%(10mL)、反应时间2.5 h、微波功率582.49 W,在该条件下MDEA转化率达到89.15%,所需时间仅为传统加热法的10.42%。

A novel perfluoroalkyl-containing quaternary ammonium salt was synthesized from N-methyl diethanolamine and perfluorinated hexyl ethyl iodide by microwave technique. The structure of the product was characterized by means of Fourier transform infrared spectroscopy, mass spectrometry and nuclear magnetic resonance spectrum. The effect of solvent dosage, microwave power, reactant mole ratio and reaction time on the conversion rate of the product was studied. The central-composite mathematical relational model between the conversion rate of N-methyl diethanolamine and the effect factors was established to optimize the synthesis technique of the product. The optimum synthesis conditions were as follows： perfluorinated hexyl ethyl iodide 0. 015 tool, N-methyt diethanolamine 0. 01 mol, solvent dosage 50% （ 10 mL） ,microwave power 582. 49 W,reaction time 2.5 h. Under the optimal conditions, where the reaction time was only 10.42% of the conventional heating time, the conversion rate of MDEA was 89. 15%.