Colloidal Defect-Free Silicalite-1 Single Crystals: Preparation, Structure Characterization, Adsorption, and Separation Properties for Alcohol/Water Mixtures

Zhou, Han; Mouzon, Johanne; Farzaneh, Amirfarrokh; Antzutkin, Oleg N.; Grahn, Mattias; Hedlund, Jonas

doi:10.1021/acs.langmuir.5b02520

Cited by 30 publications

(22 citation statements)

References 36 publications

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“…The BJH micropore area and the micropore volume were 21.89 m 2 g −1 and 0.302 cm 3 g −1 , respectively. These values correspond well with literature values for silicalite‐1 crystals …”

Section: Resultssupporting

confidence: 92%

“…These values correspond well with literature values for silicalite-1 crystals. [53][54][55][56] The extent of membrane formation through silicalite-1 pore plugging synthesis was examined using SEM ( Figure 3) and EDS (Figure 4) analysis of the cross-section for four different support pore sizes. Cross-sectional analysis of the membrane is an effective assessment of the formation of the zeolite selective layer via pore plugging synthesis, since the formation of a zeolite film on the surface is not the goal of this approach.…”

Section: Morphological and Compositional Analysismentioning

confidence: 99%

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Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO₂ supports: Effect of support pore size on membrane performance

et al. 2018

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In this study, we present a detailed synthesis procedure and characterization of porous inorganic silicalite‐1 membranes. The membranes were synthesized in‐situ using a pore plugging method with the inclusion of a 12 h thermal break promoting secondary growth within the active layer pores of the tubular TiO2 supports. The effect of the support pore size on membrane performance was examined with pore sizes ranging from 0.3 μm to 1.4 μm. Characterization using SEM and EDS analysis confirm the penetration and formation of silicalite‐1 crystals within porous supports up to a depth of 10–12 µm for all membranes. With the exception of the membranes synthesized on the support with 1.4 μm pore size, all membranes were more permeable to probe gas N2 compared to He. The highest ideal N2/He selectivity of 2.3 ± 0.5 was observed for the membranes synthesized on supports with 0.8 μm pore size. Single gas permeance for the membranes was high, ranging between 3.7 × 10−7 and 1.3 × 10−5 mol/m2sPa, and was independent of gas kinematic diameter with the order of permeation being CH4 > CO2 > N2 > He. Binary equimolar CO2/N2 separation experiments show better membrane CO2/N2 permselectivity compared to the ideal selectivity calculated from the single gas experiments. Comparing the observed membrane gas diffusivity and the adsorbate gas uptake rate within the zeolite material alone shows that these favourable selective properties are the result of adsorption surface diffusion and that Knudsen diffusion is minimized.

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Section: Resultssupporting

confidence: 92%

Section: Morphological and Compositional Analysismentioning

confidence: 99%

Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO₂ supports: Effect of support pore size on membrane performance

et al. 2018

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“…Indeed, decreasing the crystal size induces a distribution of SieO bonds and SieOeSi angles that broadens the lines. The same observation was recently reported for nanosized silicalite-1 prepared in fluoride media [28]. Further huge broadening is noted upon changing the morphology to lamellar as we already stated it (Fig.…”

Section: Resultssupporting

confidence: 89%

Influence of downsizing of zeolite crystals on the orthorhombic ↔ monoclinic phase transition in pure silica MFI-type

Kabalan

Michelin

Rigolet

et al. 2016

Solid State Sciences

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“…The MFI crystals grown in alkaline media (Si‐MFI‐OH) adsorb 0.11 g butanol g −1 crystals, which is similar to previously reported . A slightly higher butanol adsorption (0.12–0.13 g g −1 ) is observed for MFI crystals grown in fluoride media, indicating that these crystals are more hydrophobic than crystals grown in OH − media . A butanol adsorption of 0.16 g g −1 zeolite was observed for the 5000 nm large Si‐CHA crystals grown in F − media.…”

Section: Figuresupporting

confidence: 86%

Facile Preparation of Hydrophobic Colloidal MFI and CHA Crystals and Oriented Ultrathin Films

Zhou

Hedlund

2018

Angewandte Chemie

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We report novel routes for synthesis of defect-free, hydrophobic and monodispersed 10 nm (5 unit cells) thick MFI crystals and 100 nm CHA crystals.T he crystals are obtained in high yield and displayv ery high 1-butanol adsorption from aqueous solution. These crystals are assembled in monolayers for the growth of ultrathin and uniformly oriented films with thicknesses of 36 nm and 330 nm, respectively,u sing as ynthesis gel in the form of ap owder.T his method is very simple and may open up for industrial preparation of materials with improved performances.Increasing efforts have been devoted to synthesizing zeolites with enhanced accessibility to their micropores. [1,2] The particle size reduction of zeolites to the nanometer scale leads to significant changes in properties such as increased external surface areas and decreased diffusion path lengths and the possibility to use for preparation of ultrathin films. However,t he synthesis of nanosized zeolites in hydroxide media brings less desired properties of silanol groups as surface defects.The synthesis of zeolites in fluoride media was developed to alleviate these problems by preparing silanolfree zeolites.H owever,t he zeolite crystals harvested in fluoride media usually have as ize of several micrometers. Consequently,t here is an eed to produce silanol-free zeolite crystals with nanometer size.Here,wereport on the preparation of very small and welldefined, colloidal nanocrystals using straightforward conventional methods in fluoride media. Approaches for synthesis of nanosized zeolite can be classified into two distinct categories:1 )b ottom-up,b ye ngineering of the crystallization process,s uch as controlling the kinetics of nucleation versus crystal growth, [3,4] introducing organic additives [5] or confinedspace synthesis; [6] 2) top-down, that is,p ost-treatment using mechanical force to break large zeolite crystals into nanosized units,t he disadvantages of this method, like partial amorphization and broader particle size distribution, can be remedied by recrystallization. [7,8] Here,weadopted the two approaches and successfully synthesized 10 nm thick pure silica MFI crystals through the bottom-up approach and 100 nm pure silica CHA crystals by the top-down approach. Them ono-dispersed and silanol-free crystals prepared in the present work are the smallest ever reported.The10nmthick MFI crystals are comparable to the 5nm (2.5 unit cells) thick nanosheets produced by seeded growth in hydroxide (OH À )m edia with an on-commercially available template. [9] Our defect-free,h ydrophobic MFI crystals produced in fluoride medium displays very high adsorption capacity of 1-butanol (0.13 gg À1 zeolite) from aw ater solution, equal to the equilibrium adsorption ability estimated by Monte Carlo simulations. [10] The1 00 nm CHA crystal shows very high 1-butanol adsorption (0.18 gg À1 zeolite) from aqueous solution, which is two times higher than the reported adsorption of micrometer sized Si-CHA crystals from vaporphase. [11] Furthermore,t he MFI crystals are o...

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Colloidal Defect-Free Silicalite-1 Single Crystals: Preparation, Structure Characterization, Adsorption, and Separation Properties for Alcohol/Water Mixtures

Cited by 30 publications

References 36 publications

Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO₂ supports: Effect of support pore size on membrane performance

Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO₂ supports: Effect of support pore size on membrane performance

Influence of downsizing of zeolite crystals on the orthorhombic ↔ monoclinic phase transition in pure silica MFI-type

Facile Preparation of Hydrophobic Colloidal MFI and CHA Crystals and Oriented Ultrathin Films

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Colloidal Defect-Free Silicalite-1 Single Crystals: Preparation, Structure Characterization, Adsorption, and Separation Properties for Alcohol/Water Mixtures

Cited by 30 publications

References 36 publications

Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO2 supports: Effect of support pore size on membrane performance

Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO2 supports: Effect of support pore size on membrane performance

Influence of downsizing of zeolite crystals on the orthorhombic ↔ monoclinic phase transition in pure silica MFI-type

Facile Preparation of Hydrophobic Colloidal MFI and CHA Crystals and Oriented Ultrathin Films

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Product

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Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO₂ supports: Effect of support pore size on membrane performance

Pore plugging synthesis and characterization of silicalite‐1 membranes using tubular TiO₂ supports: Effect of support pore size on membrane performance