以甲基三甲氧基硅烷为偶联剂,用化学接枝法对MCM-48分子筛进行改性,制备了甲基官能化的MCM-48分子筛. 利用FT-IR、XRD、低温N2吸附/脱附等手段对产物进行结构和性能分析. 实验结果表明,硅甲基取代了MCM-48分子筛表面和孔道内羟基,成功接枝到MCM-48表面上,膜孔径、比表面积及孔体积均减小,但MCM-48保留原有立方有序结构. MCM-48分子筛甲基硅烷化改性后表面疏水性提高,水热稳定性提高.

Methyl-functionalized MCM-48 molecular sieve was prepared by grafting method using methyltrimethoxysilane as coupling agent. The prepared product was characterized by Fourier transform infrared (FT-IR), X-ray diffraction (XRD) and nitrogen adsorption-desorption. The experiment results indicated that the silyl group was substituted for the Si-OH group on the pore surface of MCM-48, and then the modified MCM-48 molecular sieve with reduced pore diameter, surface area and pore volume was successfully acquired by silylation. However, the modified MCM-48 remains the cubic ordered mesoporous structure. The hydrothermal stability and hydrophobicity of MCM-48 molecular sieve were improved by the silylation.

[1] Beck J S, Vartuli J C, Roth W J, et al. A new family of mesoporous molecular sieves prepared with liquid crystal templates[J]. J Am Chem Soc , 1992, 114 (27) :10834-10843.
[2] Kresge C T, Leonowicz M E, Roth W J, et al. Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism[J]. Nature , 1992, 359 (6397) :710-712.
[3] Xia Y D, Mokaya R. Aluminosilicate MCM-48 materials with enhanced stability via simple post-synthesis treatment in water[J]. Micropor Mesopor Mater , 2004 , 68 (1-3) :1-10.
[4] Galarneau A, Driole M F, Petitto C, et al. Effect of post-synthesis treatment on the stability and surface properties of MCM-48 silica[J]. Micropor Mesopor Mater , 2005, 83 (1-3) :172-180.
[5] Zhao W, Hao Z P, Hu C. Synthesis of MCM-48 with a high thermal and hydrothermal stability[J]. Mater Res Bull , 2005, 40 (10) :1775-1780.
[6] Matsumoto A, Tsutsumi K, Schumacher K, et al. Surface functionalization and stabilization of mesoporous silica spheres by silanization and their adsorption characteristics[J]. Langmuir , 2002, 18 (10) :4014-4019.
[7] 杨 佳, 何 静, 段 雪,等. 硅甲基接枝改性MCM-48 的结构特征及表面性质[J] . 无机化学学报 , 2002 , 9 (9) :879-886.
[8] Li Y S, Shi J L, Chen H R, et al. One-step synthesis of hydrothermally stable cubic mesoporous aluminosilicates with a novel particle structure[J] . Micropor Mesopor Mater , 2003, 60 (1-3):51-56.
[9] 刘 建, 杨启华, 张 磊, 等. 有机-无机杂化氧化硅基介孔材料[J] . 化学进展 , 2005 , 17 (5) :809-817.
[10] Ji H, Fan Y Q, Jin W Q, et al. Synthesis of Si-MCM-48 membrane by solvent extraction of the surfactant template[J]. J Non-Cryst Solids , 2008, 354 (18):2010-2016.
[11] Xu D K, Fan Y Q. Mesoporous Si-MCM-48 membrane prepared by pore-filling method[J]. Sci China Tech Sci , 2010, 53 (4):1064-1068.
[12] Gao N W, Li M, Jing W H, et al. Improving the filtration performance of ZrO2 membrane in non-polar organic solvents by surface hydrophobic modification[J]. J Membr Sci , 2011, 375 :276-283.
[13] Park D H, Nishiyama N, Egashira Y, et al. Enhancement of hydrothermal stability and hydrophobicity of a silica MCM-48 membrane by silylation[J]. Ind Eng Chem Res , 2001, 40 (26) :6105-6110.
[14] Koyano K A, Tatsumi T, Tanaka Y, et al. Stabilization of mesoporous molecular sieves by trimethylsilylation[J]. J Phys Chem B , 1997, 101 :9436-9440.