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.


(A) XRD patterns of (A) FDU-12-H200 prepared at the aging durations of (a) 1 h (b) 2 h and (c) 4 h, and (B) FDU-12-H prepared at different temperatures with an aging duration of 2 h. (a) 100 °C, (b) 130 °C, (c) 150 °C, (d) 180 °C, and (e) 200 °C.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Figure 1: (A) XRD patterns of (A) FDU-12-H200 prepared at the aging durations of (a) 1 h (b) 2 h and (c) 4 h, and (B) FDU-12-H prepared at different temperatures with an aging duration of 2 h. (a) 100 °C, (b) 130 °C, (c) 150 °C, (d) 180 °C, and (e) 200 °C.

Mentions: Since the synthesis was done at high temperatures for a shorter duration, it is important to check the mesostructure of the prepared samples in order to make sure that the structure of the samples is developed. Initially, the effect of synthesis time affecting the structural and textural properties of FDU-12 samples was studied by preparing FDU-12 samples at a synthesis temperature of 200 °C under different aging periods ranging from 1 to 4 h. Figure 1(A) shows the XRD patterns of FDU-12-H200 samples prepared at different aging periods. It can be seen that irrespective of such rapid aging duration, each of the FDU-12-H200 samples exhibited a characteristic (111) peak followed by reflections corresponding to (220), (311), (331) and (442) lattice planes, which is the characteristic behaviour of the face centred cubic structure [7]. Among the FDU-12-H200 samples prepared at different aging times, the sample prepared with the aging time of 2 h seemed better than those with the aging time of 1 and 4 h as reflected from their respective XRD peak intensities and the well-ordered structure formation. This was due to the fact that the synthesis time of 1 h is not enough for the structure formation, which is due to the poor condensation of silica species, and the synthesis period of 4 h is too long as it destroys the structure at the reaction temperature of 200 °C.


Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme
(A) XRD patterns of (A) FDU-12-H200 prepared at the aging durations of (a) 1 h (b) 2 h and (c) 4 h, and (B) FDU-12-H prepared at different temperatures with an aging duration of 2 h. (a) 100 °C, (b) 130 °C, (c) 150 °C, (d) 180 °C, and (e) 200 °C.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Figure 1: (A) XRD patterns of (A) FDU-12-H200 prepared at the aging durations of (a) 1 h (b) 2 h and (c) 4 h, and (B) FDU-12-H prepared at different temperatures with an aging duration of 2 h. (a) 100 °C, (b) 130 °C, (c) 150 °C, (d) 180 °C, and (e) 200 °C.
Mentions: Since the synthesis was done at high temperatures for a shorter duration, it is important to check the mesostructure of the prepared samples in order to make sure that the structure of the samples is developed. Initially, the effect of synthesis time affecting the structural and textural properties of FDU-12 samples was studied by preparing FDU-12 samples at a synthesis temperature of 200 °C under different aging periods ranging from 1 to 4 h. Figure 1(A) shows the XRD patterns of FDU-12-H200 samples prepared at different aging periods. It can be seen that irrespective of such rapid aging duration, each of the FDU-12-H200 samples exhibited a characteristic (111) peak followed by reflections corresponding to (220), (311), (331) and (442) lattice planes, which is the characteristic behaviour of the face centred cubic structure [7]. Among the FDU-12-H200 samples prepared at different aging times, the sample prepared with the aging time of 2 h seemed better than those with the aging time of 1 and 4 h as reflected from their respective XRD peak intensities and the well-ordered structure formation. This was due to the fact that the synthesis time of 1 h is not enough for the structure formation, which is due to the poor condensation of silica species, and the synthesis period of 4 h is too long as it destroys the structure at the reaction temperature of 200 °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.