PREPARATION AND CHARACTERIZATION OF VANADO-, FERRI-, AND GALLOSILICATE CATALYSTS IN THE PRESENCE OF FLUORIDE IONS

Hong SB; Kim CG; Uh YS; Park YK; Woo SI

Korean Journal of Chemical Engineering, Vol.9, No.1, 16-22, January, 1992

Vanado-, ferri-, and gallosilicate catalysts were prepared from the mixtures containing colloidal silica, corresponding metal source, tetrapropylammonium bromide, and NH₄F by hydrothermal crystallization at 175℃ for 7 days. The pH value of the reaction mixture was low(pH<8) compared to the conventional methods. The metal compounds have higher solubilities in these conditions than conventional conditions (pH>10). The size distribution and the size of final products were found to be more homogeneous and larger than those of metallosilicates prepared in strong alkaline media. The characterization of metallosilicates with IR, X-ray diffraction, SEM, EPR, and ²⁹Si MAS NMR, indicated that corresponding metal atoms were successfully incorporated into the tetrahedral lattice sites of the ZSM-5 structure.

[References]

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[1] Derouane EG, Nagy J, Gabelica Z, Blom N, Zeolites, 2, 229 (1982)

[2] Kessler H, Chezeau JM, Guth JL, Strub H, Coudurier G, Zeolites, 7, 360 (1987)

[3] Guth JL, Kessler H, Wey R, "Proceedings of 7th International Conference on Zeolites, Tokyo, 1986," (Murakami, Y., Iijima, A. and Ward, J., eds.), p. 121, Elsevier, Tokyo (1986)

[4] Inui T, Medhanavyn D, Prasserthdam P, Fukuda K, Ukawa T, Sakamoto A, Miyamoto A, Appl. Catal., 18, 311 (1985)

[5] Borade RB, Zeolites, 7, 398 (1987)

[6] Szostak R, Thomas TL, J. Catal., 100, 555 (1986)

[7] Thomas JM, Lui XS, J. Phys. Chem., 90, 4843 (1986)

[8] Marat RK, Janzen AF, Can. J. Chem., 55, 3845 (1977)

[9] Busey RH, Schwartz E, Mesmer RE, Inorg. Chem., 19, 758 (1980)

[10] Miyamoto A, Medhanavyn D, Inui T, Appl. Catal. A: Gen., 28, 89 (1986)

[11] Szostak R, Thomas TL, J. Catal., 101, 549 (1986)

[12] Flanigen EM, Grose RW, Adv. Chem. Ser., 101, 76 (1971)

[13] Nyquist RA, Kagel RO, "Infrared Spectra of Inorganic Compounds," Academic, New York (1971)

[14] Inui T, Nagata H, Yamase O, Matsuda H, Kuroda T, Yoshikawa M, Takeguchi T, Miyamoto A, Appl. Catal., 24, 257 (1986)

[15] Fyfe CA, Gobbi GC, Klinowski J, Thomas JM, Ramdas S, Nature, 296, 530 (1982)

[16] Takahashi H, Shiotani M, Kobayashi H, Sohma J, J. Catal., 14, 134 (1969)

[17] Ball JW, Dwyer J, Garforth AA, Smith WJ, "Proceedings of 7th International Conference on Zeolites, Tokyo, 1986," (Murakami, Y, Iijima, A. and Ward, J., eds.), Elsevier, Tokyo, p. 137 (1986)

[18] Calis G, Frenken P, deBoer E, Swolfs A, Hefni MA, Zeolites, 7, 319 (1987)

[19] Hayashi S, Suzuki K, Shin S, Haymizu K, Yamamoto O, Bull. Chem. Soc. Jpn., 58, 52 (1985)