Department of Materials Engineering, Faculty of Engineering, Kasetsart University, Bangkok 10900, Thailand.
Molecules. 2012 Jan 5;17(1):511-26. doi: 10.3390/molecules17010511.
A series of benzoxazine monomer supramolecules with different substituted groups on their benzene ring was prepared with a Mannich reaction and characterized by FTIR, 1H-NMR and MS. The obtained products were 3,4-dihydro-3-(2'-hydroxyethylene)-6-methyl-2H-benzoxazine (BM1), 3,4-dihydro-3-(2'-hydroxyethylene)-6-ethyl-2H-benz-oxazine (BM2), and 3,4-dihydro-3-(2'-hydroxyethylene)-6-methoxy-2H-benzoxazine (BM3). The efficiency of alkali metal ion extraction from the products was determined with Pedersen's technique, while the complexation of the Ce(III) ion was confirmed by the Job's and the mole ratio methods. The evidence of complex formation between benzoxazine monomers and Ce(III) ions was obtained with FTIR and a computational simulation. Single phase ceria (CeO₂) as observed with XRD was successfully prepared by calcinating the Ce(III)-benzoxazine monomer complexes at 600 °C for 2 h. In addition, the geometry of the ceria nanoparticles confirmed by TEM is spherical, with an average diameter of 10-20 nm.
我们用曼尼希反应制备了一系列苯环上带有不同取代基的苯并恶嗪单体超分子，并通过傅里叶变换红外光谱（FTIR）、1H-NMR 和 MS 对其进行了表征。得到的产物分别为 3,4-二氢-3-(2'-羟乙基)-6-甲基-2H-苯并恶嗪（BM1）、3,4-二氢-3-(2'-羟乙基)-6-乙基-2H-苯并恶嗪（BM2）和 3,4-二氢-3-(2'-羟乙基)-6-甲氧基-2H-苯并恶嗪（BM3）。我们采用佩德森技术测定了从产物中提取碱金属离子的效率，并用乔布法和摩尔比法证实了铈（III）离子的络合。我们通过傅里叶变换红外光谱和计算模拟获得了苯并恶嗪单体与铈（III）离子形成配合物的证据。在 600°C 下煅烧 2 小时，成功地从 Ce(III)-苯并恶嗪单体配合物中制备出了单相氧化铈（CeO₂），XRD 观察到。此外，TEM 证实了氧化铈纳米粒子的几何形状为球形，平均直径为 10-20nm。
