山嵛酸双酯基有机硅季铵盐的微波合成工艺及性能

以山嵛酸、N-甲基二乙醇胺以及γ-氯丙基三甲氧基硅烷为主要原料，分别经过酯化和季铵化反应两步合成了一种超长碳链的双酯基有机硅季铵盐，并通过单因素、正交试验得到了微波法合成目标产物的最优工艺条件为：设置微波功率为800W，物料摩尔比为n（硅烷）∶n（酯胺）=1.2∶1，反应温度为170℃，溶剂用量为m（溶剂）∶m（原料）=0.8∶1，反应时间为12h，产品产率达96.60%。此方法克服了长链叔胺季铵化过程中普遍耗时过长的困难，提高了反应速率，而且实验重复性良好。实验中采用红外光谱、核磁共振氢谱对中间体及目标产物的结构进行了表征，与预期结果一致；建立了高效液相色谱-蒸发光散射检测器（HPLC-ELSD）测定季铵盐纯度的方法，基线稳定，峰型良好，产品纯度达98.77%，具有一定的参考价值。性能测试结果表明：对比DC-5700，目标产物具有良好的热稳定性，优异的乳化及增溶性能；其水溶液的临界胶束浓度为1.81mmol/L，表面张力（γ_CMC）为49.4mN/m。

Microwave synthesis process and properties of behenic acid diester-based silicone quaternary ammonium salt

Diester-based silicon quaternary ammonium salts with long carbon chains were synthesized via esterification and quaternization reaction in two steps using behenic acid, N-methyldiethanolamine, and γ-chloropropyltrimethoxysilane. Single-factor and orthogonal array design experiments to synthesis desired products by microwave method were carried out to investigate the optimal reaction conditions, which were the microwave power 800W, material mole ratio n(silane):n(ester amine)=1.2:1, reaction temperature 170℃, the amount of solvent m(solvent):m(raw material)=0.8:1, and reaction time 12h, and a yield of 96.60%. The method overcame the long time-consuming difficulties in the quaterization process of long chain tertiary amine, improved the reaction rate, and obtained a good reaction repeatability. The chemical structures of the intermediates and target compounds were characterized by FTIR and ¹H NMR spectra, which were consistent with the expected results. A simple, rapid and accurate method for the purity determination of quaternary ammonium salts by HPLC-ELSD was established with some reference valuea. The purity of the product was confirmed to reach 98.77% with a stable baseline and sharp peak.The results of performance tests showed that, compared with DC-5700, the target products had good thermal stability, excellent emulsifying and solubilizing properties; the CMC of the aqueous solution was 1.81mmol/L, and the corresponding surface tension was 49.4mN/m.