安定剂双-(2,6-二甲氧基苯酚基)三甘醚合成及表征研究

Synthesis and characterization of bis-(2,6-dimethoxyphenol)triethyleneglycolether

以2,6-二甲氧基苯酚(BG)与1,2-双(氯乙氧基)乙烷(BCE)为原料,通过取代反应合成了二(2,6-二甲氧基苯)三甘醚(Stab-5),并利用元素分析、核磁共振、质谱及红外光谱等鉴定其结构,收率可达85.5%;优化了反应条件,最优工艺条件为:n(催化剂):n(BG)=2.5∶1,n(BG)∶n(BCE)=2.4∶1,反应温度为80℃;改进了精制方法,采用无水乙醚与石油醚混合溶剂进行纯化研究,其最佳比例为V(乙醚)∶V(石油醚)=2∶1,获得的产品纯度可达98.7%以上。Stab-5毒性小,不具有致癌性,在双基固体推进剂中作为安定剂使用具有应用前景。

Using syringol(BG)and 1,2-bis(chloroethoxy)ethane(BCE)as starting material,bis-(2,6-dimethoxyphenol)triethyleneglycolether(Stab-5)was synthesized via the reactions of substitution with the yield of 85.5%.The structure of the title compound was characterized by 1H NMR,13 C NMR,FTIR,MS and elementary analysis.The synthetic conditions of substitution were optimized as following:n(catalyst)∶n(BG)is 2.5∶1,n(BG)∶n(BCE)is 2.4∶1,the reaction temperature is at 80℃.The refining process of the product was improved by using anhydrous ether and petroleum ether mixed solvent.The optimum volume ratio of anhydrous ether to petroleum ether is 2∶1,and the purity of the product obtained is more than 98.7%.The Stab-5 is low in toxicity and non-carcinogentic,it is expected to be used as a stabilizer in double base soild propellants.