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Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme

View Article: PubMed Central - PubMed

ABSTRACT

Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, 29Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g−1 in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

No MeSH data available.


HRSEM images of FDU-12-H prepared at 100 °C (A), (B) and 200 °C (C), (D) for an aging duration of 2 h.
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Figure 5: HRSEM images of FDU-12-H prepared at 100 °C (A), (B) and 200 °C (C), (D) for an aging duration of 2 h.

Mentions: The surface morphology of the calcined FDU-12 samples prepared at different temperatures was obtained using SEM and the images are shown in figure 5. The images obtained show a spherical morphology for the FDU-12 samples indicating the high morphological order of the synthesized materials. From the SEM images, the morphology of the spherical structures seems to exhibit an enlargement in the size of the particles from 1.95 μm for FDU-12-H100 to 2.35 μm for FDU-12-H200 which is in concordance with the insights derived from XRD and BET. The possible reasoning would be that at high reaction temperatures, through liquid crystal assembly, the charged surfactant molecules and the interaction between the silica species are quite notably enhanced. In addition, the enlargement of the surfactant micelles reduces the surface curvature which also results in an increase of the particle size for the sample prepared at high temperature. However, it should be noted that the particles are agglomerated and the spherical shape which is typically obtained for FDU-12 samples is not clear for these samples. This could be due to the short aging time and the high energy at high temperature that favours quick condensation with the neighbouring particles. This would significantly affect the morphological ordering of the samples [31].


Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme
HRSEM images of FDU-12-H prepared at 100 °C (A), (B) and 200 °C (C), (D) for an aging duration of 2 h.
© Copyright Policy - open-access
Related In: Results  -  Collection

License 1 - License 2
Show All Figures
getmorefigures.php?uid=PMC5036462&req=5

Figure 5: HRSEM images of FDU-12-H prepared at 100 °C (A), (B) and 200 °C (C), (D) for an aging duration of 2 h.
Mentions: The surface morphology of the calcined FDU-12 samples prepared at different temperatures was obtained using SEM and the images are shown in figure 5. The images obtained show a spherical morphology for the FDU-12 samples indicating the high morphological order of the synthesized materials. From the SEM images, the morphology of the spherical structures seems to exhibit an enlargement in the size of the particles from 1.95 μm for FDU-12-H100 to 2.35 μm for FDU-12-H200 which is in concordance with the insights derived from XRD and BET. The possible reasoning would be that at high reaction temperatures, through liquid crystal assembly, the charged surfactant molecules and the interaction between the silica species are quite notably enhanced. In addition, the enlargement of the surfactant micelles reduces the surface curvature which also results in an increase of the particle size for the sample prepared at high temperature. However, it should be noted that the particles are agglomerated and the spherical shape which is typically obtained for FDU-12 samples is not clear for these samples. This could be due to the short aging time and the high energy at high temperature that favours quick condensation with the neighbouring particles. This would significantly affect the morphological ordering of the samples [31].

View Article: PubMed Central - PubMed

ABSTRACT

Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, 29Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g−1 in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

No MeSH data available.