采用微波辅助水热法快速合成了介孔磷酸镍(MW-NiPO-2),详细研究了在微波水热条件下微波晶化温度、微波辐射时间、碱度及Ni/P摩尔比对MW-NiPO-2合成的影响,优化了合成条件.并利用ICP、FT-IR、TEM和N2吸附等手段对比研究了溶胶-凝胶法和微波水热法合成样品的结构组成、比表面和孔道特征.研究结果表明:在微波辅助水热条件下,存较低温度下(60℃)即可形成MW-NiPO-2;在100℃下,0.25 h即有MW-NiPO-2生成.在微波辐射1h,碱度(OH/P)为2.0、原料Ni/P比为0.7条件下,能够合成有序度较高的MW-NiPO-2.MW-NiPO-2和SG-NiPO-2具有相似的骨架结构和组成,但其纳米管簇结构特征不明显,表现出类似虫孔结构的状态.微波辅助水热法合成的MW-NiPO-2较溶胶-凝胶法合成样品具有更大的比表面和孔容,分别为334.4 m2/g和0.318 cm3/g.
参考文献
| [1] | Schüth F.Non-siliceous mesostructured and mesoporous materials.Chem.Mater,2001,13(10):3184-3195. |
| [2] | Cao J M,Feng J,Deng S G,et al.Microwave-assisted solid-state synthesis of hydroxyapatite nanorods at room temperature.Mater.Lett.,2005,40(23):6311-6313. |
| [3] | Yang P D,Zhao D Y,Margolese D I,et al.Generalized syntheses of large-pore mesoporous metal oxides with semicrystalline framework.Nature,1998,396(6707):152-155. |
| [4] | Pan C L,Yuan S,Zhang W X.A neutral templating route to mesoporous titanium phosphate molecular sieves with enhanced thermal stability.Appl.Catal.A:General,2006,312:186-193. |
| [5] | Yu J,Wang A J,Tan J,et al.Synthesis of novel nanotubular mesoporous nickel phosphates with high performance in epoxidation.J.Mater.Chem.,2008,18(30):3601-3607. |
| [6] | Choi J Y.Kim J,Jhung S H,et al.Microwave synthesis of a porous metal-organic framework,zinc terephthalate MOF 5.Bull.Korean Chem.Soc.,2006,27(10):1523-1524. |
| [7] | Park S E,Kim D S,Chang J S,et al.Synthesis of MCM-41 using microwave heating with ethylene glycol.Catal.Today,1998,44(1-4):301-308. |
| [8] | Wu C G,Bein T.Microwave synthesis of molecular sieve MCM-41.Chem.Commun.,1996,8:925-926. |
| [9] | Fantini M C A,Matos J R,Cides da Silva L C,et al.Ordered mesoporous silica:microwave synthesis.Mater.Sci.Eng.B,2004,112(2/3):106-110. |
| [10] | Bandyopadhyay M,Gies H.Synthesis of MCM-48 by microwavehydrothermal process.C.R.Chim.,2005,8(3/4):621-626. |
| [11] | Newalkar B L,Komarneni S,Katsuki H.Rapid synthesis of mesoporous SBA-15 molecular sieve by a microwavehydrothermal process.Chem.Commun.,2000,23:2389-2390. |
| [12] | Hwang Y K,Chang J S,Kwon Y U,et al.Microwave synthesis of cubic mesoporous silica SBA 16.Microporous Mesoporous Mater.,2004,68(1/2/3):21-27. |
| [13] | Wang H W,Kuo C H,Lin H C,et al.Rapid formation of active mesoporous TiO2 photocatalysts via micelle in a microwave hydrothermal process.J. Am. Ceram. Soc., 2006, 89(11):3388-3392. |
| [14] | Zawadzki M.Microwave-assisted synthesis and characterization of ultrafine neodymium oxide particles.J.Alloys Compd.,2008,451(1/2):297-300. |
| [15] | Deshmane A C,Jasinski B J,Carreon A M.Microwave-assisted synthesis of nanocrystalline mesoporous gallium oxide.Microporous Mesoporous Mater,2010,130(1/2/3):97-102. |
| [16] | 王业红,谭涓,刘靖,等(WANG Ye-Hong,et al),萃取法脱除介孔磷酸镍模板剂的研究.化学学报(Acta Chim.Sinica),2010,68(23):2471-2476. |
| [17] | Jhung S H,Yoon J W,Hwang Y K,et al.Morphology control of the nanoporous nickel phosphate VSB-5 from large crystals to nanocrystals.Microporous Mesoporous Mater.,2006,89(1/2/3):9-15. |
| [18] | 牟群英,李贤军.微波加热技术的应用与研究进展.物理学和高新技术,2004,33(6):438-442. |
| [19] | Bhaumik A,Inagaki S.Mesoporous titanium phosphate molecularsieves with ion-exchangc capacity.J.Am.Chem.Soc.,2001,123(4):691-696. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%