Abstract: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,B4O5(OH)2-4 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.
[1] DUAN Xue, ZHANG Fa-zhi(段 雪, 张法智). Intercalated Assembling Functional Materials(插层组装与功能材料). Beijing: Chemical Industry Press(化学工业出版社), 2007. 7, 120. [2] Constantino V R L, Thomas J H. Inorg. Chem. 1995, 34: 883. [3] Bouraada M, Jah M L, Ouali M S, et al. Journal of Hazardous Materials, 2008, 153: 911. [4] Ay A N, Birgül Z K, Temel A, Mafra L. Applied Clay Science, 2011, 51: 308. [5] Ling S, Li D Q, Wang J R, et al. Clays and Clay Minerals, 2005, 53(3): 294. [6] Nyambo C, Wilkie C A. Polymer Degradation and Stability, 2009, 94(4): 506. [7] Nyambo C, Kandare E, Wilkie C A. Polymer Degradation and Stability, 2009, 94: 513. [8] WANG Shi-xia, ZHENG Hai-fei(王世霞,郑海飞). Acta minetalogica Sinicas(矿物学报), 2011, 31(2): 230. [9] Kloprogge J T, Hickey L, Frost R L. Applied Clay Science,2001, 18: 37. [10] Jubri Z B, Bin Hussein M Z, Yahaya A H, et al. J. Porous Mater.,2012, 19: 45. [11] Ambrogi V, Perioli L, Nocchetti M, et al. Journal of Physics and Chemistry of Solids, 2012, 73: 94. [12] Kloprogge J T, Frost R L. Journal of Solid State Chemistry,1999, 146: 506. [13] XIE Xian-mei , WU Xu, DU Ya-li, et al(谢鲜梅, 吴 旭, 杜亚丽,等). Modern Chemical Industry(现代化工), 2006, 26(2): 92. [14] Prevot V, Forano C, Besse J P. Inorg. Chem., 1998, 37: 4293. [15] JIAO Qing-ze, ZHAO Yun, XIE Hui, et al(矫庆泽,赵 芸,谢 晖, 等). Chinese Journal of Applied Chemistry(应用化学), 2002, 19(10): 1011. [16] Kloprogge J T, Hickey L, Frost R L. Journal of Raman Spectroscopy, 2004, 35: 967. [17] GOU Guo-jing, MA Pei-hua, CHU Min-xiong(苟国敬, 马培华, 褚敏雄). Chemical Journal of Chinese Universities(高等学校化学学报), 2005, 26(3): 497. [18] YANG Xu-gang, WU Qi-lin(杨序纲,吴琪琳). Raman Spectrospcopy Analysis and Application(拉曼光谱的分析与应用). Beijing: Nation Defense Industry Press(北京:国防工业出版社), 2008. 10. [19] Palmer S J, Soisonard A, Frost R L. Journal of Colloid and Interface Science, 2009, 329: 404. [20] Liu Z H, Gao S Y, Xia S P. Spectrochimica Acta, 2003, 59: 265. [21] Li J, Xia S P, Gao S Y. Spectrochimica Acta, 1995, 51A(4): 519.