硼-10酸的合成

Synthesis of boric-10 acid

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%。

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 rt （ 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%.