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Process for making a germanium-zeolite. Atp MedicalLiterature - Series # 017. Source:http://www.sciencemag.org/cgi/content/full/304/5673/990
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characterizations of IM-
12, a thermally stablegermanium-containingzeolite . . . .)
Extra-Large-Pore Zeolites with Two-
Dimensional Channels Formed by14 and 12 RingsJean-Louis Paillaud,1* BogdanHarbuzaru,1 Jol Patarin,1 NicolasBats2
Stable zeolites that havelarger pore apertures and a three-dimensional pore topology are of
interest because they could be
used to adsorb largermolecules, particularly forapplication in oil
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refining.
Several large-pore zeoliticmaterials with channels formed byopenings of more than 12 rings areknown, but all of them have a one-dimensional channel system that
limits theiruse in catalysis.We report the synthesis and
some characterizations of IM-12, a
thermally stable
germanium-containingzeolite that contains the firsttwo-dimensional channel systemwith extra-large pores formed by 14-and 12-ring channels.
1 Laboratoire de MatriauxMinraux, UMR-CNRS 7016, EcoleNationale Suprieure de Chimie de
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Mulhouse, Universit de HauteAlsace, 3 rue Alfred Werner, 68093
Mulhouse Cedex, France.2 Institut Franais du Ptrole, IFP-Lyon, Bote Postale 3, 69390Vernaison, France.* To whom correspondence should
be addressed. E-mail:[email protected] of theirhigh
thermal stability, newzeolites are of interest inpetroleum refining, especially thosewith larger pores and systems ofintersecting channels that could
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potentially process
larger hydrocarbonmolecules. Two approacheshave led to larger pore systems.
One is the use offluoride
ions in place of OHspecies (13), because thefluoride appears to actas a structure-
directing agent (SDA)that plays a templating role (46).The other is the use of twosources of framework
atoms.For example, thesilicogermanates ITQ-12 (7), ITQ-17(8), ITQ-21 (9), and ITQ-22 (10)
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structures (13).Theoretical calculations
confirm this interpretation (14),together with the reportedpreferential occupation of thetetrahedral (T) sites of the D4R byGe in the zeolites obtained from Si-
and Ge-containing synthetic gels(1416), and also with the
observed fastercrystallization rate of
the ITQ-7 zeolite in itsSi- and Ge-containingform (14).
Scheme 1. One F-
containing D4Rcubic unit offormula T8O20, inwhich each T atom
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is at the center of atetrahedron and the
oxygen's atoms areat the vertices.[View LargerVersion of thisImage (32K GIFfile)]
We prepared the extra-largepore zeolite IM-12 (Institut Franais
du Ptrole/Mulhouse12), a Ge-containing zeolite, from afluoride-free synthesis medium inthe presence of organic (6R,10S)-6,10-dimethyl-5-azoniaspiro[4,5]decane cations as
SDA. This zeolitic materialdisplays a high
http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG1http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG18/14/2019 Www.muliply.com - 3.018 Blog - Zeolite Synthesis
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thermal stability and
high adsorptioncapacity.
Depending on thecrystallization conditions (17), the
silicogermanate IM-12shows two differentcrystal morphologies.
Under static conditions,aggregates of size 150 by 150 by
200 m (Fig. 1A) resulting from thesuperposition ofthin platelet-like crystals areformed.
Under stirring conditions,gypsum flower-type
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aggregates are
produced with moreisolated crystals, withsizes of 5 by 5 m and thicknessesof about 300 nm (Fig. 1B).
The chemical and the thermal
gravimetric and differential thermalanalyses of IM-12synthesized in this wayindicated a Si/Ge
atomic ratio of about4.5 and a total weightloss of 15.7%, respectively,which are consistent with theunitcell formula: |(C11H22N)4(H2O;OH)16|
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reported for the microporoussilicogermanates with the topologies
ISV, ITH, and AST (1416,18).Thus, each layer is essentiallysiliceous and constructed of fusedsmall [415462] and [5262] cages.
The topology of IM-12 is that
of a 2D channel system formed by14- and 12-ring intersectingchannels parallel to the cand baxes, respectively (Fig. 2). The
framework density of
IM-12 is 15.2 T atomsper 1000 3.This value is lower than that of
other zeolitic materials containing14-ring channels, such as UTD-1
(19), CIT-5 (20), SSZ-53, and SSZ-59 (18,21) but higher than thoserecently reported for ECR-34 (18-ring pores) (22) and OSB-1 (a
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beryllosilicate with 14- and 8-ringintersecting channels) (18).
The crystallographic data ofIM-12 led to a free-pore diameter of9.5 by 7.1 and 8.5 by 5.5 for thestraight elliptical 14- and 12-ringchannels, respectively; these values
are comparable to 9.3 by 7.6 ,which was observed for the 14-ringopening of the borosilicate SSZ-59(21).
A calcination at
550C under air forseveral hours was sufficientto empty the pore volume of IM-12.Moreover, after several cycles ofcalcination at 600C, the structure of
IM-12 remained intact.We evaluated the
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adsorption capacity of
this highly thermally stable materialby N2adsorptionmeasurements. The N2adsorption isotherm of IM-12, of typeIa, according to the International
Union of Pure and AppliedChemistry nomenclature (fig. S2)
(17), is characteristic of amicroporous material
that lacks secondarymicropores andmesopores.
The corresponding
Brunauer-Emmet-Teller surface area of670 m2 g1 and the
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microporous volume of 0.26 cm3 g1
are similar to those of wellknown
highly porous zeolites oftopology FAU or EMT(18).
The pore-size distribution is
rather narrow and centered on 10 (fig. S3) (17). This value is slightlyhigher than the one calculated fromthe crystallographic data; thedisparity may reflect thenoncylindrical shape of the pores or
the effect of the side pockets of the12-ring channel, which the modeldoes not take into account (Fig. 3).
Fig. 2. The 3Dstructure and the
2D channel systemof the IM-12 zeolite.The connection
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between thesilicogermanate
layers lying in the(100) plane showsthe 14-ring channelalong [001] (left)and the 12-ringchannel along [010](right). The darkgray circles are theGe atoms. Thereare no openingsdown [100]. [View
Larger Version ofthis Image (60KGIF file)]
Fig. 3. View down a
direction close to[001] reveals thetie-shaped
http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG3http://www.sciencemag.org/cgi/content/full/304/5673/990/FIG38/14/2019 Www.muliply.com - 3.018 Blog - Zeolite Synthesis
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The ability to
incorporate Alsuggests that thismaterial may havecatalytic applicationsas well.References and Notes
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(2002).[CrossRef][Medline] 10. A. Corma, F. Rey, S.
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Chem. Mater.15, 3921 (2003). 16. Y. Wang, J. Song, H. Gies,
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17. Materials and methods areavailable as supporting materialon Science Online.
18. All framework type codes arederived from the names of thetype materials and consist ofthree capital Roman letters. Formore information, see Ch.Baerlocher, W. M. Meier, D. H.Olson,Atlas of ZeoliteFramework Types (Elsevier,Amsterdam, ed. 5, 2001); alsoavailable atwww.iza-structure.org/databases.
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22. K. G. Strohmaier, D. E. W.
Vaughan, J. Am. Chem. Soc.125, 16035 (2003).[CrossRef][ISI][Medline]
23. We thank the InstitutFranais du Ptrole for providing
the germanium source. B.H.thanks the Ministre del'Education Nationale, de laRecherche et de la Technologiefor financial support.Supporting Online Material
www.sciencemag.org/cgi/content/full/304/5673/990/DC1
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