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Cobalt Phosphate Based Zeolite Structures with the Edingtonite Framework Topology

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Cobalt Phosphate Based Zeolite Structures with the Edingtonite Framework Topology 2546 Chem. Mater. 1998, 10, 2546-2551 Cobalt Phosphate Based Zeolite Structures with the Edingtonite Framework Topology Xianhui Bu, Thurman E. Gier, Pingyun Feng, and Galen D. Stucky* Department of Chemistry, University of California, Santa Barbara, California 93106 Received April 24, 1998. Revised Manuscript Received June 23, 1998 Hydrothermal syntheses and crystal structures of five zeolite edingtonite analogues are presented. For the first time, the edingtonite framework topology is assembled using an amine-assisted synthesis approach with either 1,2-diaminopropane or 1,2-diamino-2- methylpropane. These materials are created in the cobalt phosphate system with a small concentration of trivalent cations (Al3+ and Ga3+) incorporated into the framework for the host-guest charge matching. ACP-EDI1 and GCP-EDI1 are monoclinic, whereas ACP-EDI2, ACP-EDI3, and GCP-EDI2 are tetragonal (ACP ) aluminum cobalt phosphate; GCP ) gallium cobalt phosphate). The difference in lattice symmetries between ACP-EDI1 and ACP-EDI2 (or GCP-EDI1 and GCP-EDI2) is related to the synthesis conditions. All five structures have three-dimensional 8-ring channels along the crystallographic [001], [110], and [1h10] directions, regardless of the difference in symmetry. Amine molecules are more ordered in the monoclinic phases than in the tetragonal phases, and the orientational disorder of amine molecules persists at a temperature of 150 K. Introduction channel systems have been found.9,12 These materials may be preferred for some applications, such as gas Zeolites are three-dimensional aluminosilicates with separation and ion exchange. open-framework structures. They originally exist as minerals, but their important commercial values have One of the challenges facing synthetic chemists is led to extensive academic and industrial research on whether all different zeolite topologies found in nature their syntheses, structures, and various properties.1 can be assembled using the amine-directed synthesis There are now many zeolite structures such as zeolite approach. We have previously reported the first amine- A that have no natural counterparts, in addition to a directed synthesis of thomsonite, phillipsite, merlinoite, variety of zeolite analogue materials with different and rho analogues, which represents a significant step 8,9,13,14 chemical compositions and framework symmetries.2-4 toward achieving that goal. In this work, we The discovery of a large family of aluminophosphate- report the first amine-directed synthesis of five struc- based zeolite-type materials in the early 1980s has tural analogues of a rare zeolite mineral, edingtonite. generated a widespread interest in non-aluminosilicate- Despite the large number of structures that have been 5 based microporous materials. A similar impressive found in the AlPO4-based system, the edingtonite success has also been achieved in materials containing analogue has until now defied numerous synthetic 6,7 15,16 nontetrahedral metal atoms such as V and Mn. efforts in either AlPO4 or substituted AlPO4 systems. Our efforts have been on the synthesis of zeolite Edingtonite (Ba2Al4Si6O20‚8H2O, space group P21212) structures by means of structure direction through represents one of three zeolite-type structures (thom- host-guest charge matching and hydrogen-bonding- sonite and natronite being the other two) that are called assisted self-assembly in highly charged phosphate fibrous zeolites because their structures comprise an systems.8-11 We are particularly interested in struc- unique chain denoted as the fi chain.17 So far, only the tures in which the average charge per tetrahedral atom is between 3.75 and 3.5. In such a charge domain, (8) Feng, P.; Bu, X.; Stucky, G. D. Nature 1997, 388, 735-741. where the framework is highly negatively charged, (9) Bu, X.; Feng, P.; Stucky, G. D. Science 1997, 278, 2271-2272. unusual framework structures with multidimensional (10) Feng, P.; Bu, X.; Stucky, G. D. Angew Chem. Int. Ed. Engl. 1995, 34, 1745-1747. (11) Bu, X.; Gier, T. E.; Feng, P.; Stucky, G. D. Microporous (1) Breck, D. W. Zeolite Molecular Sieves; Wiley: New York, 1974. Mesoporous Mater. 1998, 20, 371-379. (2) Meier, W. M.; Olson, D. H.; Baerlocher, Ch. Atlas of Zeolite (12) Gier, T. E.; Bu, X.; Feng, P.; Stucky, G. D. Nature In press. Structure Types; Elsevier: Amsterdam, 1996. (13) Feng, P.; Bu, X.; Stucky, G. D. Microporous Mesoporous Mater. (3) Flanigen, E. M. In Studies in Surface Science and Catalysis; In press. van Bekkum, H., Flanigen, E. M., Jansen, J. C., Eds.; Elsevier: (14) Feng, P.; Bu, X.; Gier, T. E.; Stucky, G. D. Microporous Amsterdam, 1991; Vol. 58, pp 13-34. Mesoporous Mater. In press. (4) Chen, J.; Jones, R. H.; Natarajan, S.; Hursthouse, M. B.; (15) Wilson, S. T.; Flanigen, E. M. In Zeolite Synthesis; ACS Thomas, J. M., Angew Chem. Int. Ed. Engl. 1994, 33, 639-640. Symposium Series 398; Occelli, M. L., Robson, H. E., Ed.; 1989; pp (5) Wilson, S. T.; Lok, B. M.; Messina, C. A.; Cannan, T. R.; 329-345. Flanigen, E. M. J. Am. Chem. Soc. 1982, 104, 1146-1147. (16) Kessler, H. In Comprehensive Supramolecular Chemistry; (6) Khan, M. I.; Meyer, L. M.; Haushalter, R. C.; Schweitzer, A. L.; Albert, G., Bein, T., Eds.; Pergamon: New York, 1996; Vol. 7, pp 425- Zubieta, J.; Dye, J. L. Chem. Mater. 1996, 8,43-53. 464. (7) Suib, S. T. Curr. Opin. Solid State Mate. Sci. 1998, 3,63-70. (17) Smith, J. V. Chem. Rev. 1988, 88, 149-182. S0897-4756(98)00308-1 CCC: $15.00 © 1998 American Chemical Society Published on Web 08/13/1998 Cobalt Phosphate Based Zeolite Structures Chem. Mater., Vol. 10, No. 9, 1998 2547 Table 1. A Summary of Crystal Data and Refinement Results name ACP-EDI1 GCP-EDI2 ACP-EDI2 ACP-EDI3 a formula (R1)2AlCo4P5O20 (R1)2GaCo4P5O20 (R1)2AlCo4P5O20 (R2)2AlCo4P5O20 habit blue plate blue needle blue needle blue prism size (µm) 133 × 133 × 40 400 × 80 × 80 133 × 67 × 67 53 × 40 × 27 temp (K) 293 150K 293 293 a (Å) 10.0103(5) 9.9937(4) 10.0317(2) 10.0873(3) b (Å) 9.9896(5) 9.9937(4) 10.0317(2) 10.0873(3) c (Å) 12.8520(7) 12.8519(7) 12.8837(4) 12.9358(5) â (deg) 91.113(1) 90 90 90 V (Å3) 1284.9(1) 1283.57 1296.55(5) 1316.26(8) Z2 2 2 2 space group P21 P4h21cP4h21cP4h21c 2θmax (deg) 50 50 45 45 total data 6646 6313 5076 5044 unique data 3928 1137 852 857 data, I > σ2(I) 3381 726 766 756 parameters 371 84 90 82 R(F) (%) 6.87 5.26 7.89 6.70 2 Rw(F ) (%) 17.0 12.7 17.4 12.9 GOF 1.17 1.13 1.28 1.31 a 2+ 2+ R1 ) [NH3CH2CH(NH3)CH3] ;R2) [NH3CH2C(CH3)2(NH3)] ; R(F) ) ∑||Fo| - |Fc||/∑|Fo| with Fo > 4.0 σ(F). crystal structure of aluminosilicate edingtonite has been water was added and the pouch was sealed and heated in an unambiguously determined from the mineral sample.2 autoclave at 160 °C/100 psi (autogenous, water support fluid) for 30 days. Recovery of the pouch contents via standard One beryllophosphate form (KBePO4‚H2O) has been reported to have the edingtonite topology on the basis ultrasonic/decantation/filtration techniques gave rise to the 18 major product, deep blue crystals, mixed with a small amount of its powder diffraction data. To our knowledge, no of unidentified pink crystalline phases. single-crystal study has been done on any synthetic GCP-EDI2. This phase was prepared by mixing CoCO ‚xH O material with the edingtonite-type topology, possibly 3 2 (0.70 g), 85% H3PO4 (1.34 g), Ga(NO3)3 (0.34 g), and 1,2- due to the difficulties in growing large crystals. diaminopropane (0.59 g) with ethylene glycol (13.52 g). The mixture was then heated at 180 °C for 4 days in a Teflon- Experimental Section coated steel autoclave. The product was recovered by filtration and washed with deionized water. Blue prismatic crystals Synthesis. ACP-EDI1. ACP-EDI1 was prepared by mixing were obtained. No unidentified impurity lines could be Co(NO3)2 (1.284 g), Al(NO3)3 (2.318 g),2MH3PO4 (2.716 g), detected from the X-ray powder diffraction pattern. and 1,2-diaminopropane (0.89 g) with water (10 mL) in a Elemental Analysis. Quantitative elemental analyses for Teflon pouch. After holding at 150 °C for 1 week at autogenous ACP-EDI1 and ACP-EDI2 were carried out on a Cameca SX- pressure in an autoclave, the pouch was recovered by standard 50 electron probe microanalyzer equipped with five wavelength filtration and drying techniques. Platelike blue crystals were dispersive (WD) X-ray spectrometers and one energy dispersive recovered from a colorless solution. No pink or red phases (ED) X-ray spectrometer. The instrument was controlled by containing nontetrahedral cobalt cations were present, but a SUN workstation, and the analyses for Al, Co, and P were X-ray powder diffraction data recorded from 3° to 60° (Cu KR) with a step size of 0.03° and a counting time of 1 s/step on a simultaneously performed on three WD spectrometers. The Scintag PAD X powder diffractometer revealed a few weak rough surface of ACP-EDI2 and the observed beam damage unidentified lines, in addition to peaks from ACP-EDI1. for ACP-EDI1 might affect the accuracy of the results. The energy dispersive spectrum for GCP-EDI2 showed a small, but ACP-EDI2. Solution A was prepared by mixing aluminum distinct, peak for Ga in addition to large Co and P peaks, isopropoxide (100.15 g) with 85% H3PO4 (101.74 g) and ethylene glycol (653.00 g), followed by stirring at room tem- confirming the substitution of Ga for Co.
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