Zhang Jing-Yu, Bai Zhi-Min, Zhao Dong
China University of Geosciences, Beijing, China.
Guang Pu Xue Yu Guang Pu Fen Xi. 2013 Mar;33(3):704-8.
The pattern of X-ray diffraction, the Raman and infrared spectra of organic borate intercalated hydrotalcite were discussed. The well crystallized zinc-aluminum layered double hydroxides (Zn-Al LDHs) intercalated by carbonate ions and borate ions were respectively prepared by co-precipitation method. Patterns of X-ray diffraction showed that the (003) reflection of borate-LDHs was sharp and symmetric and shifted to lower angle than that of carbonate-LDHs. The gallery height of borate-LDHs increased from 0. 28 nm to 0.42 nm after intercalation, indicating that interlayered carbonate ions were substituted by borate anions. The Raman and IR spectra showed that specific bands of carbonate ions in the borate-LDHs disappeared, but with the presence of B3O3(OH)4- X B4O5(OH)4(2-) and B(OH)4- in the interlayer galleries. The hydroxide interlayer anions had a significant influence on the band positions in Raman and infrared spectra of modes related to the hydroxyl group. Our results indicate that single phase and pure borate-pillared LDHs can be obtained using tributyl orthoborate as intercalating agents, and the change in the structure and nature of hydrotalcite can be detected precisely by Raman spectroscopy.
讨论了有机硼酸盐插层水滑石的X射线衍射、拉曼光谱和红外光谱特征。采用共沉淀法分别制备了碳酸根离子和硼酸根离子插层的结晶良好的锌铝层状双氢氧化物（Zn-Al LDHs）。X射线衍射图谱表明，硼酸根-LDHs的（003）反射峰尖锐且对称，且相较于碳酸根-LDHs向低角度偏移。插层后硼酸根-LDHs的层间距从0.28 nm增加到0.42 nm，表明层间碳酸根离子被硼酸根阴离子取代。拉曼光谱和红外光谱表明，硼酸根-LDHs中碳酸根离子的特定谱带消失，但层间存在B3O3(OH)4- X B4O5(OH)4(2-)和B(OH)4-。氢氧化物层间阴离子对与羟基相关模式的拉曼光谱和红外光谱中的谱带位置有显著影响。我们的结果表明，使用原硼酸三丁酯作为插层剂可以获得单相且纯净的硼酸根柱撑LDHs，并且通过拉曼光谱可以精确检测水滑石结构和性质的变化。
