Synthesis of large single crystals of templated Y faujasite

Ferchiche, Samia; Valcheva-Traykova, Maria; Vaughan, D. E. W.; Warzywoda, Juliusz; Sacco, Albert

doi:10.1016/s0022-0248(00)00979-9

Cited by 56 publications

(37 citation statements)

References 5 publications

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“…This 18 The starting gel was prepared from fumed silica (99.8%, Sigma), sodium aluminate (technical, Wako), sodium hydroxide (98%, Aldrich), triethanolamine (TEA, 99+%, Acros), bis(2-hydroxyethyl)-dimethylammonium chloride (TCl, 99%, Acros), and distilled water (resistivity > 18.4 MΩ-cm). Further description on the synthetic procedure is available in reference.…”

Section: å)mentioning

confidence: 99%

Synthesis of Fully Dehydrated Partially Cs⁺-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs₄₅Na₃₀|[Si₁₁₇Al₇₅O₃₈₄]-FAU and Its Single-crystal Structure

Seo¹,

Kim²,

Lee³

et al. 2009

Bulletin of the Korean Chemical Society

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Large single crystals of zeolite, |Na75|[Si117Al75O384]-FAU (Na-Y, Si/Al = 1.56), were synthesized from gels with composition of 3.58SiO2 : 2.08NaAlO2 : 7.59NaOH : 455H2O : 5.06TEA : 2.23TCl. One of these, a colorless single-crystal was ion exchanged by allowing aqueous 0.02 M CsOH to flow past the crystal at 293 K for 3 days, followed by dehydration at 673 K and 1 × 10 -6 Torr for 2 days. The crystal structure of fully dehydrated partially Cs

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Section: å)mentioning

confidence: 99%

Synthesis of Fully Dehydrated Partially Cs⁺-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs₄₅Na₃₀|[Si₁₁₇Al₇₅O₃₈₄]-FAU and Its Single-crystal Structure

Seo¹,

Kim²,

Lee³

et al. 2009

Bulletin of the Korean Chemical Society

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“…23 A starting gel was prepared from fumed silica (99.8%, Sigma), sodium aluminate (technical, Wako), sodium hydroxide (96%, Wako), triethanolamine (TEA, 99+%, Acros), bis(2-hydroxyethyl)dimethylammonium chloride (TCl, 99%, Acros), and distilled water.…”

Section: Synthesis Of Large Single Crystals Of Zeolite Y (Fau)mentioning

confidence: 99%

Six Single-Crystal Structures Showing the Dehydration, Deamination, Dealumination, and Decomposition of NH₄⁺-Exchanged Zeolite Y (FAU) with Increasing Evacuation Temperature. Identification of a Lewis Acid Site

and¹,

Seo²,

and³

et al. 2007

J. Phys. Chem. C

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Single crystals of zeolite Y, |Na 71 |[Si 121 Al 71 O 384 ]-FAU, with diameters up to 0.20 mm were grown. They were ion exchanged to generate |(NH 4 ) 64 Na 5 K 2 |[Si 121 Al 71 O 384 ]-FAU. Crystals 1 through 6, respectively, were vacuum dehydrated at 323, 373, 423, 473, 523, and 573 K, and without reexposure to the atmosphere, their structures were determined crystallographically at 294 K using synchrotron X-radiation. Their compositions (best integers) are seen to be respectively |(NH 4 ) 59 H 5 Na 5 K 2 (H 2 O) 3 |[Si 121 Al 71 O 384 ]-FAU (incomplete dehydration and partial deamination), |(NH 4 ) 31 H 33 Na 5 K 2 |[Si 121 Al 71 O 384 ]-FAU (further deamination), |(NH 4 ) 2 H 62 Na 5 K 2 |[Si 121 -Al 71 O 384 ]-FAU (nearly complete deamination), |H 61 Na 5 K 2 (Al 2 O) 0.5 |[Si 122 Al 70 O 384 ]-FAU (onset of dealumination and framework reconstruction), |H 53 Na 5 K 2 (Al 2 O) 2 |[Si 124 Al 68 O 384 ]-FAU (further dealumination and reconstruction), and |H 51 Na 5 K 2 (Al 2 O) 2.5 |[Si 124 Al 68 O 384 ]-FAU. The extent of deamination of NH 4 + increases with increasing evacuation temperature until it is complete in crystal 4. In crystal 1, 59 NH 4 + ions per unit cell are found at two crystallographically distinct positions: 30 at site I′ (in sodalite cavities opposite D6Rs) and 29 at site II (in supercages opposite S6Rs). Three water molecules coordinate to Na + ions. In crystal 2, 17 NH 4 + ions per unit cell are found at site I′ and 13 at site II. In crystal 3, only 2 NH 4 + ions at site II are found. The extent of dealumination of the zeolite framework, seen in crystals 4, 5, and 6, also increases with temperature: 1, 4, and 5 Al 3+ ions per unit cell, respectively, are found at site I′ recessed slightly into D6Rs. Each Al 3+ ion coordinates trigonally (O-Al-O ) 119.3°) at ca. 1.85 Å to three framework oxygens. Pairs of these Al 3+ ions are each bridged by a nonframework oxide ion at the center of a D6R to give linear Al-O-Al groups (Al-O ) 1.62 Å). These Al 3+ ions are Lewis-acid sites and should be catalytically active when accessible. Five additional crystals vacuum dehydrated at 623 K and above showed no crystallinity, due presumably to further dealumination and dehydration (loss of H + and framework oxygen).

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“…Fixed weights were used initially; the final weights were assigned using the formula w = 1/[σ 2 Table 1). Atomic scattering 3 factors for K + , O − , and (Si,Al) 1.79+ were used.…”

Section: Structure Determinationmentioning

confidence: 99%

“…The growth of large single crystals of zeolite is of interest in order to obtain the 3-dimensional structural parameters of the framework, and the information on the exchangeable cations, and the adsorbate. For example, Sacco et al [1][2][3] synthesized the large single crystals of faujasite-type zeolites (Si/Al = 1.35~1.45, 1.71, and 1.90) with diameters of 95 to 340 μm from a reaction mixture composed of Na2O, Al2O3, SiO2, H2O, TEA, and/or TCl. They reported their synthesized single crystals were suitable for single-crystals X-ray diffraction experiments.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of the Large Single Crystal of Fully K⁺-exchanged Zeolite X (FAU), |K₈₀|[Si₁₁₂Al₈₀O₃₈₄]-FAU (Si/Al=1.41)

Lim

Jeong²,

Park

et al. 2007

Bulletin of the Korean Chemical Society

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Large colorless single crystals of sodium zeolite X, stoichiometry |Na80|[Si112Al80O384]-FAU, with diameters up to 200 μm and Si/Al = 1.41 have been synthesized from gels with the composition of 2.40SiO2 : 2.00NaAlO2 : 7.52NaOH : 454H2O : 5.00TEA. One of these, a colorless octahedron about 200 μm in cross-section has been treated with aqueous 0.1 M KNO3 for the preparation of K + -exchanged zeolite X. The crystal structure of |K80|[Si112Al80O384]-FAU per unit cell, a = 24.838(4) Å, dehydrated at 673 K and 1 × 10 −6 Torr, has been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd at 294 K. The structure was refined using all intensities to the final error indices (using only the 707 reflections for which Fo > 4σ (Fo)) R1 = 0.075 (based on F) and R2 = 0.236 (based on

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Synthesis of large single crystals of templated Y faujasite

Cited by 56 publications

References 5 publications

Synthesis of Fully Dehydrated Partially Cs⁺-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs₄₅Na₃₀|[Si₁₁₇Al₇₅O₃₈₄]-FAU and Its Single-crystal Structure

Synthesis of Fully Dehydrated Partially Cs⁺-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs₄₅Na₃₀|[Si₁₁₇Al₇₅O₃₈₄]-FAU and Its Single-crystal Structure

Six Single-Crystal Structures Showing the Dehydration, Deamination, Dealumination, and Decomposition of NH₄⁺-Exchanged Zeolite Y (FAU) with Increasing Evacuation Temperature. Identification of a Lewis Acid Site

Synthesis and Characterization of the Large Single Crystal of Fully K⁺-exchanged Zeolite X (FAU), |K₈₀|[Si₁₁₂Al₈₀O₃₈₄]-FAU (Si/Al=1.41)

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Synthesis of large single crystals of templated Y faujasite

Cited by 56 publications

References 5 publications

Synthesis of Fully Dehydrated Partially Cs+-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs45Na30|[Si117Al75O384]-FAU and Its Single-crystal Structure

Synthesis of Fully Dehydrated Partially Cs+-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs45Na30|[Si117Al75O384]-FAU and Its Single-crystal Structure

Six Single-Crystal Structures Showing the Dehydration, Deamination, Dealumination, and Decomposition of NH4+-Exchanged Zeolite Y (FAU) with Increasing Evacuation Temperature. Identification of a Lewis Acid Site

Synthesis and Characterization of the Large Single Crystal of Fully K+-exchanged Zeolite X (FAU), |K80|[Si112Al80O384]-FAU (Si/Al=1.41)

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Synthesis of Fully Dehydrated Partially Cs⁺-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs₄₅Na₃₀|[Si₁₁₇Al₇₅O₃₈₄]-FAU and Its Single-crystal Structure

Synthesis of Fully Dehydrated Partially Cs⁺-exchanged Zeolite Y (FAU, Si/Al = 1.56), |Cs₄₅Na₃₀|[Si₁₁₇Al₇₅O₃₈₄]-FAU and Its Single-crystal Structure

Six Single-Crystal Structures Showing the Dehydration, Deamination, Dealumination, and Decomposition of NH₄⁺-Exchanged Zeolite Y (FAU) with Increasing Evacuation Temperature. Identification of a Lewis Acid Site

Synthesis and Characterization of the Large Single Crystal of Fully K⁺-exchanged Zeolite X (FAU), |K₈₀|[Si₁₁₂Al₈₀O₃₈₄]-FAU (Si/Al=1.41)