Rapid synthesis of MFI zeolite nanocrystals

被引:98
作者
Hsu, CY
Chiang, AST
Selvin, R
Thompson, RW
机构
[1] Natl Cent Univ, Dept Chem & Mat Engn, Chungli 32054, Taiwan
[2] Worcester Polytech Inst, Dept Chem Engn, Worcester, MA 01609 USA
关键词
D O I
10.1021/jp0526391
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
A rapid synthesis procedure for nonagglomerated silicalite nanocrystals has been developed. This was achieved by concentrating the precursor sol before 10-12 h of aging at 80 degrees C, followed by hydrothermal synthesis at 175 degrees C for 90 min. The high silica concentration in the concentrated sol accelerated the aggregation of primary units that were present early in the system. Thus, little silica nutrients were left for growth when the secondary particles were converted to zeolite during hydrothermal reaction. As a result, fully dispersible nanocrystals were obtained within a day instead of weeks as reported previously. The aggregation of primary units during the 80 degrees C aging process as well as the conversion of these aggregates into zeolite has been followed by DLS, XRD, and FTIR. In light of the new results, the nucleation and growth mechanisms of MFI zeolite that have been under debate in the literature were reexamined.
引用
收藏
页码:18804 / 18814
页数:11
相关论文
共 43 条
  • [1] Low temperature synthesis and properties of ZSM-5 aggregates formed by ultra-small nanocrystals
    Aguado, J
    Serrano, DP
    Escola, JM
    Rodríguez, JM
    [J]. MICROPOROUS AND MESOPOROUS MATERIALS, 2004, 75 (1-2) : 41 - 49
  • [2] Some observations on the preparation and properties of colloidal silicalites Part II: Preparation, characterisation and properties of colloidal silicalite-1, TS-1, silicalite-2 and TS-2
    Cundy, CS
    Forrest, JO
    [J]. MICROPOROUS AND MESOPOROUS MATERIALS, 2004, 72 (1-3) : 67 - 80
  • [3] Some observations on the preparation and properties of colloidal silicalites. Part 1: synthesis of colloidal silicalite-1 and titanosilicalite-1 (TS-1)
    Cundy, CS
    Forrest, JO
    Plaisted, RJ
    [J]. MICROPOROUS AND MESOPOROUS MATERIALS, 2003, 66 (2-3) : 143 - 156
  • [4] In situ observation of nucleation and crystal growth in zeolite synthesis. A small-angle X-ray scattering investigation on Si-TPA-MFI
    de Moor, PPEA
    Beelen, TPM
    van Santen, RA
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 1999, 103 (10) : 1639 - 1650
  • [5] Si-MFI crystallization using a "dimer" and "trimer" of TPA studied with small-angle X-ray scattering
    de Moor, PPEA
    Beelen, TPM
    van Santen, RA
    Beck, LW
    Davis, ME
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 2000, 104 (32): : 7600 - 7611
  • [6] Standard nitrogen adsorption data for characterization of nanoporous silicas
    Jaroniec, M
    Kruk, M
    Olivier, JP
    [J]. LANGMUIR, 1999, 15 (16) : 5410 - 5413
  • [7] Identification of precursor species in the formation of MFI zeolite in the TPAOH-TEOS-H2O system
    Kirschhock, CEA
    Ravishankar, R
    Verspeurt, F
    Grobet, PJ
    Jacobs, PA
    Martens, JA
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 1999, 103 (24) : 4965 - 4971
  • [8] Mechanism of transformation of precursors into nanoslabs in the early stages of MFI and MEL zeolite formation from TPAOH-TEOS-H2O and TBAOH-TEOS-H2O mixtures
    Kirschhock, CEA
    Ravishankar, R
    Van Looveren, L
    Jacobs, PA
    Martens, JA
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 1999, 103 (24) : 4972 - 4978
  • [9] Aggregation mechanism of nanoslabs with zeolite MFI-type structure
    Kirschhock, CEA
    Ravishankar, R
    Jacobs, PA
    Martens, JA
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 1999, 103 (50) : 11021 - 11027
  • [10] New evidence for precursor species in the formation of MFI zeolite in the tetrapropylammonium hydroxide-tetraethyl orthosilicate-water system
    Kirschhock, CEA
    Kremer, SPB
    Grobet, PJ
    Jacobs, PA
    Martens, JA
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 2002, 106 (19) : 4897 - 4900