在水热条件下,考察了1NiCl2·6H2O-mH3PO4-nNH4F-pNH3·H2O-40H2O(n=0、3) 体系中空旷结构过渡金属磷酸镍材料的合成影响因素(原料、pH值、Ni/P比、模板剂和矿化剂等),并给出了材料的晶化区域图.在实验过程中得到的产物包括已知结构的24元环微孔材料VSB-1[1]和VSB-5[2]、12元环微孔材料A、层状材料B[3]、氢键型微孔材料C[4].采用XRD、FT-IR和TG对所合成的材料进行了表征.所合成几种材料的XRD图都在较低的2θ角处出现了衍射峰,表明它们可能具有比较空旷的骨架结构.实验证明该体系中矿化剂、pH 值和Ni/P比对产物的影响较大.值得说明的是文献报道在没有F离子的情况下不能合成出VSB-1[1],而我们在没有F离子的条件下合成了VSB-1.
Under hydrothermal synthetic conditions and from 1NiCl2·6H2O-mH3PO4-nNH4F-pNH3·H2O-40H2O(n=0, 3) system, we synthesized five kinds of materials
containing microporous VSB-1 and VSB-5 with 24 member rings, microporous sample A Ni12(HPO4)6(PO4)2(OH)6 with 12 member rings, layered
structural sample B NH4NiPO4·H2O, and microporous sample C (C2H10N2)[Ni(H2O)6](HPO4)2 with 8 member rings linked
by hydrogen bonds. They were characterized by XRD, FT-IR and TG. The effect factors of raw materials, pH, Ni/P ratio, template agents, and mineralization agent on synthetic products were investigated. The phase maps were also provided.
The effect factors of pH, Ni/P ratio, and mineralization agent play important roles in the synthetic processes. It is important that we synthesized VSB-1
without F ions.
参考文献
| [1] | Guillou N, Gao Q, Nogues M, et al. C.R. Acad. Sci. Paris, t.2, Serie?Ⅱ c,p., 1999. 387--392. [2] Guillou N, Gao Q, Forster P M, et al. Angew. Chem. Int. Ed., 2001, 40 (15): 2831--2834. [3] Goni A, Pizarro J L, Lezama L M, et al. J. Mater. Chem., 1996, 6 (3): 421--427. [4] Escobal J, Pizarro J L, Mesa J L, et al. J. Solid. State Chem., 2000, 154: 460--465. [5] Cheetham A K, Férey G, Loiseau T. Angew. Chem. Int. Ed., 1999, 38: 3268--3292. [6] Le Meins J M. Solid State Sci., 2000, 2 (2): 299--306. [7] Bonhomme F, Thomas S G, Rodriguez M A. Microporous. Mesoporous. Mater., 2001, 47 (2-3): 185--194. [8] Chippindale A M, Brech S J, Cowley A R. Chem. Mater., 1996, 8 (9): 2259--2264. [9] Bontchev R P, Iliev M N, Dezaneti L M. Solid State Sci., 2001, 3 (1-2): 133--142. [10] Zhou Y, Zhang L, You X, et al. Inter. J. Inorg. Mater., 2001, 3 (4-5): 373--379. [11] Guesdon A, Raveau B. Solid State Sci., 2000, 2 (8): 855--860. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%