用三氟化硼乙醚络合物合成硼酸三甲酯

Synthesis of Trimethyl Borate Using Boron Trifluoride Etherate

试验研究了常压下,在甲醇介质中,用甲醇钠与三氟化硼乙醚络合物反应制备硼酸三甲酯的工艺流程,并探索其最佳工艺条件。结果利用气相色谱、色谱-质谱联用、红外光谱等分析表征手段,鉴定反应产物确实是硼酸三甲酯。并摸索其最佳工艺条件为:反应温度55℃;回流时间32 h。然后分馏,收集硼酸三甲酯甲醇恒沸物。最后用LiCl盐析法提纯硼酸三甲酯,得到硼酸三甲酯的含量在99%以上。

The preparation process of trimethyl borate with the reaction of boron trifluoride etherate and an alcoholic solution of alkali metal alkoxide was studied and the optimum condition was chosen by experiments. By means of gas chromatography, mass spectrometry and IR spectrum, the product was confirmed to be trimethyl borate. By studying the effects of reaction conditions, the optimum conditions were that the reaction should take place at 55℃ for 32 h. Then the product was fractionated for two or three times and salted out using LiCl Finally the concentration of trimethyl borate can be up to 99 %.