RESUMEN
The framework structures of two closely related molecular sieves, SSZ-26 and SSZ-33, are described. These materials possess a previously missing but desired structural feature in a group of industrially significant zeolites. They contain a three-dimensional pore system that provides access to the crystal interior through both 10- and 12-rings. This property is a consequence of the organic structure-directing agents used in the synthesis of these materials. These materials are examples of the purposeful design of a micropore architecture. Both SSZ-26 and SSZ-33 contain the 4=4-1 building unit that had been previously found only in natural zeolites.
RESUMEN
The germanosilicate ITQ-24 (IWR framework type) was synthesized in fluoride medium using 1,3,5-tris(1,2-dimethylimidazolium) benzene as the structure directing agent (SDA). A structure analysis of the as-synthesized ITQ-24 material using synchrotron powder diffraction data and difference electron density calculations have allowed the fluoride ions and the germanium atoms to be located and the conformation of the SDA to be determined. The benzyl ring is perpendicular to the b axis with the three imidazolium moieties forming a "T-shaped" arrangement. Ge atoms replace some of the Si in the double-4-ring (d4r) and in one of the single-4-rings (s4r). The other s4r contains only Si. Fluoride ions are in the d4r units. Initially, the space group Cmmm (highest possible symmetry) was assumed, but the framework geometry was strained. An independent evaluation of the symmetry using the powder charge flipping algorithm in Superflip led to a successful refinement with reasonable geometry and a refined composition of |[(C6H3)(C7H10N2)3]2F2|[Si(40.2)Ge(15.8)O112] in the space group Pban.
RESUMEN
The synthesis of aluminosilicate zeolite, SSZ-25, is described using a two-component organic guest molecule strategy. This method has been recently described by us and is quite effective in crystallizing a variety of aluminosilicate zeolites with reduction in template cost. In this instance the original organic guest component used in the discovery of SSZ-25, N',N',N'-trimethyl-2-adamantammonium cation, is used in conjunction with a variety of smaller amines. The amine is the major organic component in the synthesis and the quaternary ammonium compound, while a minor component, is essential for structure direction to the desired zeolite product. Studies here show that the adamantyl component is preferentially taken up during crystal growth. Our studies showed that the use of the multi-organic component approach to synthesis resulted in a faster and cheaper route to crystallizing SSZ-25. The SSZ-25 has been described in the literature as having the MWW topology and as such has two different channel systems accessed by 10-ring openings; the channel systems do not intersect. One set of 10-rings open into large cavities. In this study we used NMR spectroscopy to examine the as-made materials and to see if the two organic components are used in different capacities in the synthesis, probing if the admantyl component is only found in these larger cavities. The crystalline products could be affected by solvent extraction with polar solvents like dimethylformamide: the X-ray powder patterns and elemental analyses changed with solvent treatment. The solvent-treated crystals were studied by NMR spectroscopy, elemental analysis, and argon adsorption. The two-component organic guest approach was also found to be quite flexible not only with regard to the amine, but also towards the quaternary ammonium compounds. Non-adamantyl polycyclic templates could be used, and polar but non-quaternized adamantyl derivatives also succeeded in directing towards SSZ-25 formation. On the other hand. in one instance it was shown that the two-component approach favors SSZ-25 as the kinetic product but at longer run times Ostwald ripening was observed, leading to the disappearance of SSZ-25 and formation of ferrierite zeolite and quartz.