Limits...
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.


HRTEM images of FDU-12-H200.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Figure 6: HRTEM images of FDU-12-H200.

Mentions: The TEM images in figure 6 give a much clearer picture of the FDU-12-H200 synthesized at 200 °C with a greater magnification where we can infer the presence of well defined, uniform cubic structure with Fm3m symmetry with highly ordered array pores over large domains. In FDU-12-H200, the highly ordered pores are arranged in an orderly fashion and connected over significantly large-scale domains. Moreover, due to the short aging duration, even at high temperatures such as 200 °C, the internal porous network remains stable without any detrimental effect. A high magnification of the TEM image also confirms that the mesopores are organized in a 3D network, and the value of the pore diameter is almost similar to that obtained using nitrogen adsorption analysis. All these results reveal that the FDU-12 materials with 3D structure and large pore and pore volumes can be prepared within a short duration by simply increasing the synthesis temperature above 180 °C.


Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme
HRTEM images of FDU-12-H200.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Figure 6: HRTEM images of FDU-12-H200.
Mentions: The TEM images in figure 6 give a much clearer picture of the FDU-12-H200 synthesized at 200 °C with a greater magnification where we can infer the presence of well defined, uniform cubic structure with Fm3m symmetry with highly ordered array pores over large domains. In FDU-12-H200, the highly ordered pores are arranged in an orderly fashion and connected over significantly large-scale domains. Moreover, due to the short aging duration, even at high temperatures such as 200 °C, the internal porous network remains stable without any detrimental effect. A high magnification of the TEM image also confirms that the mesopores are organized in a 3D network, and the value of the pore diameter is almost similar to that obtained using nitrogen adsorption analysis. All these results reveal that the FDU-12 materials with 3D structure and large pore and pore volumes can be prepared within a short duration by simply increasing the synthesis temperature above 180 °C.

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.