Synthesis, characterization and control of proportion of polymorph C in ITQ-16 and ITQ-17 films

Abstract

Continuous ITQ-16 and ITQ-17 films on silicon wafer were prepared in fluoride media using TEAOH as organic structure-directing agent. The proportion of polymorph C in the as-synthesized ITQ-16 and ITQ-17 films was determined via X-ray diffraction characterization. The proportion of polymorph C in the ITQ-16 and ITQ-17 films was controlled via optimizing the compositions of the reaction mixtures and reaction conditions, such as varying the Si/Ge molar ratio and adding n-propyl alcohol as a solvent in the reaction mixture. The Ge atoms in the reaction media strongly increased the crystallization of polymorph C in ITQ-16 and ITQ-17 films. Moreover, the stabilizing and buffering effect of n-propyl alcohol on crystal growth further enhanced the proportion of polymorph C in the ITQ-16 and ITQ-17 films. For potential catalytic applications, Al was incorporated into the framework of polymorph C, and a pure phase of polymorph C in Al-ITQ-17 film was achieved from the synthesis gel in the n-propyl alcohol phase.

Keywords

Zeolite beta / ITQ-16 / ITQ-17 / Polymorph C

References

[1] Higgins J. B., LaPierre R. B., Schlenker J. L., Rohrman A. C., Wood J. D., Kerr G. T. Zeolites, 1988, 8(6): 446.

[2] Toktarev A. V., Malysheva L. V., Paukshtis E. A. Kinet. Catal., 2010, 51(51): 318.

[3] Shi L., Yu T. T., Lin S., Yuan Y. B., Wang J. K., Zhang N. Chem. J. Chinese Universities, 2015, 36(8): 1467.

[4] Wang L., Yu S. B., Mi Z. T., Chen H. F. React. Kinet. Catal. Lett., 2002, 77(1): 147.

[5] Camblor M. A., Corma A., Valencia S. Chem. Commun., 1996, 20: 2365.

[6] Bouizi Y., Diaz I., Rouleau L., Valtchev V. P. Adv. Funct. Mater., 2005, 15(12): 1955.

[7] Treacy M. M. J., Newsam J. M., Deem M. W. Proc. R. Soc. London, Ser. A, 1991, 433(1889): 499.

[8] Treacy M. M. J., Newsam J. M. Nature, 1988, 332(6161): 249.

[9] Newsam J. M., Treacy M. M. J., Koetsier W. T., de Gruyter C. B. Proc. R. Soc. London, Ser. A, 1988, 420(1859): 375.

[10] Corma A., Navarro M. T., Rey F., Valencia S. Chem. Commun., 2001, 18: 1720.

[11] Sastre G., Vidal-Moya J. A., Blasco T., Rius J., Jordá J. L., Navarro M. T., Rey F., Corma A. Angew. Chem. Int. Ed., 2002, 41(24): 4722.

[12] Alvaro M., Atienzar P., Corma A., Ferrer B., Garcia H., Navarro M. T. J. Phys. Chem. B, 2005, 109(8): 3696.

[13] Villaescusa L. A., Barrett P. A., Camblor M. A. Angew. Chem. Int. Ed., 1999, 38(38): 1997.

[14] Botella P., Corma A., Navarro M. T., Rey F., Sastre G. J. Catal., 2003, 217(2): 406.

[15] Díaz-Cabañas M. J., Villaescusa L. A., Camblor M. A. Chem. Commun., 2000, 9: 761.

[16] Corma A., Diaz U., Domine M. E., Fornés V. Angew. Chem. Int. Ed., 2000, 39(13): 2346.

[17] Corma A., Díaz-Cabañas M. J., Domine M. E., Rey F. Chem. Commun., 2000, 18: 1725.

[18] Corma A., Navarro M. T., Rey F., Rius J., Valencia S. Angew. Chem. Int. Ed., 2001, 40(12): 2277.

[19] Tomlinson S. M., Jackson R. A., Catlow C. R. A. J. Chem. Soc. Chem. Commun., 1990, 11: 813.

[20] Chen Y., Zhu G., Peng Y., Bi H., Feng J., Qiu S. Microporous Mesoporous Mater., 2009, 123(1–3): 45.

[21] Corma A., Navarro M. T., Rey F., Valencia S. Chem. Commun., 2001, 16: 1486.

[22] Morris M., Dixon A. G., Sacco A. Jr., Thompson R. W. Zeolite, 1993, 13(2): 113.

[23] Blasco T., Corma A., Díaz-Cabañas M. J., Fernando R., Vidal-Moya J. A., Zicovich-Wilson C. M. J. Phys. Chem. B, 2002, 106(10): 2634.

[24] Qiu S., Yu J., Zhu G., Terasaki O., Nozue Y., Pang W., Xu R. Microporous Mesoporous Mater., 1998, 21(4–6): 245.

[25] Oumi Y., Kakinaga Y., Kodaira T., Teranishi T., Sano T. J. Mater. Chem., 2003, 13(13): 181.

[26] Sano T., Wakabayashi S., Oumi Y., Uozumi T. Microporous Mesoporous Mater., 2001, 46(1): 67.

[27] Piccione P. M., Laberty C., Yang S., Camblor M. A., Navrotsky A., Davis M. E. J. Phys. Chem. B, 2000, 104(43): 10001.

[28] Larlus O., Valtchev V. P. Chem. Mater., 2005, 17(4): 881.

[29] Hong S. B., Camblor M. A., Davis M. E. J. Am. Chem. Soc., 1997, 119(4): 761.

[30] Glinka Y. D., Krak T. B., Belyak Y. N., Degoda V. Y., Ogenko V. M. Colloids Surf. A, 1995, 104(1): 17.

[31] Glinka Y. D., Lin S. H., Chen Y. T. Phys. Rev. B: Condens. Matter, 2000, 62(7): 4733.