硼-10酸的合成

为了开发经济高效的硼-10酸生产路线,文中对于以工业生产得到的三氟化硼-10-乙醚络合物为原料生产硼-10酸的工艺进行了初步研究。首先采用三氟化硼-10-乙醚络合物与甲醇钠反应生成硼-10酸三甲酯,之后水解合成硼-10酸。分别讨论并优化了酯化反应和水解反应的工艺条件。在无水甲醇中,n(甲醇钠)∶n(三氟化硼-10-乙醚络合物)=4.4条件下,于55℃酯化反应32 h,硼-10酸三甲酯收率为87.43%。在n(水)∶n(硼-10酸三甲酯)=7.5条件下,硼-10酸三甲酯于室温下进行水解反应,硼-10酸收率可达97.13%,纯度大于99.0%。

Synthesis of boric-10 acid

In order to develop an economic and effective route of producing boric-10,the process of preparing boric-10 was studied by taking boron-10 trifluoride-ether complex from industrial production as a material.The steps were as follows: trimethyl borate-10 was synthesized from boron-10 trifluoride-ether complex and sodium methylate,which was hydrolyzed to synthetize boric-10 acid.The conditions of esterification and hydrolysis were discussed and optimized,respectively.The yield of trimethyl borate-10 reached 87.43% at 55 ℃ for 32 h in methanol with n(sodium methylate) ∶n(boron-10 trifluoride-ether complex)=4.4.Under the conditions of n(water) ∶n(trimethyl borate-10)=7.5,boric-10 acid was obtained at room temperature,with the yield of 97.13% and the purity higher than 99.0%.