LTA |
GaPO4 |
P(50), Ga(50) |
Contributed by Henri Kessler and Abdallah Merrouche
Verified by P. Behrens, by P. Feng, by J. Chen, by R. Fricke, and by C. Ferey
Type Material [Ga12P12O48][(n-C3H7)2NH2F]3: (H2O)w (w ~ 6 [1])
Method A. Merrouche, J. Patarin, M. Soulare, H. Kessler, P. Anglerot [2]
Batch Composition 1 Ga2O3 : 1 P2O5 : 1 HF : 70 H2O : 6.5 DPA (DPA = di-n-propylamine)
Source Materials
phosphoric acid (Fluka, 85% H3PO4)
distilled water
gallium sulfate hydrate (Strem Chemicals, Ga2(SO4)3. xH2O (wt% Ga ~ 18))
hydrofluoric acid (Fluka, 40% HF)
di-n-propylamine (Fluka, 95%)
Batch Preparation (for 1 g dry product)
(1) [1.16 g phosphoric acid + 2.2 g water + 3.8 g gallium sulfate hydrate + 2.5 g water], stir until dissolved
(2) [(1) + 0.25 g hydrofluoric acid], mix thoroughly
(3) [(2) + 3.25 g di-n-propylamine], mix thoroughly. Initial pH = 4 to 4.5
Crystallization
Vessel: PTFE-lined autoclave
Temperature: 1400C
Time: 24 hours
Agitation: none
Product Recovery
(1) Filter; wash with distilled water
(2) Dry at 60¼C
(3) Yield: approximately 60% with respect to starting oxides
Product Characterization
XRD characteristic strong reflections at d = 12.02, 8.50, 6.94, 6.01 Å
Elemental Analysis (anhydrous form): Ga0.49P0.51O2(DPA)0.13F0.12
Crystal Size and Habit: cubes (5 - 40 um)
Click here to view XRD pattern
References
[1] A. Simmen, J. Patarin, C. Baerlocher, in Proceedings of the 9th International Zeolite Conference, Vol. 1, R. Von Ballmoos, J. B. Higgins, M. M. J. Treacy (eds.), Montreal, 1992, Butterworth-Heinemann, Stoneham, 1993, p. 433
[2] A. Merrouche, J. Patarin, M. Soulard, H. Kessler, D.Anglerot, in Molecular Sieves, Vol. 1, Synthesis of Microporous Materials, M. L Occelli, H. F. Robson (eds.), Van Nostrand Reinhold, New York, 1992, p. 384