CHA |
SAPO-44 |
Al(48), P(34), Si(18) |
Contributed by S. Ashtekar, S. V.V. Chilukuri and D. K.Chakrabarty
Verified by A. Prakash and by He Chang-Qing
Type Material 5.0 (C6H11NH2) [Si6.5Al17.3P12.2O72] wH2Oa
Method S. Ashtekar, S. V.V. Chilukuri, D. K. Chakrabarty [1]
Batch Composition Al2O3:1.0 P2O5:1.0 SiO2:1.9 R: 63 H2Ob (R = cyclohexylamine)
Source Materials
distilled water
orthophosphoric acid (85% H3PO4)
pseudoboehmite (Catapal-B, Vista, 70% Al2O3)
cyclohexylamine (99+%)
fumed silica (99+% SiO2)
Batch Preparation (for 16 g product)
(1) [90 g water + 34.59 g orthophosphoric acid + 21.86 g pseudoboehmite, mix thoroughly
(2) [60 g water + 28.27 g cyclohexylamine + 9 g fumed silica], mix thoroughly
(3) [(1) + (2)], mix thoroughly with vigorous agitation
Crystallization
Vessel: stainless steel autoclave
Temperature: 1900C
Time: 48 hours
Agitation: none
Product Recovery
(1) Filter and wash with distilled water
(2) Dry at 1100C
(3) Yield near 100% on Al2O3
Product Characterization
XRD: CHA; competing phase: SAPO-5 (when gel C6H11NH2/Al2O3 ratio < 1.9)
Elemental Analysis: (Si0.18Al0.48P0.34)O2a
Crystal Size and Habit: cubical morphology with 10-50 um diameter [1]
Click here to view XRD pattern
Reference
[1] S. Ashtekar, S. V. V. Chilukuri, D. K. Chakrabarty, J. Phys. Chem. 98 (1994) 4878
Notes
a. Cations assumed to be protonated amine or surface hydroxyl.
b. H2O includes water from pseudoboebmite and orthophosphoric acid.