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Novel and facile synthesis of transparent-monolithic TiO2 gels by sol-gel method based on an esterification reaction

Kais Elghniji
Kais Elghniji
, 
Zohra Anna-Rabah
Zohra Anna-Rabah
 and 
Elimame Elaloui
Elimame Elaloui
   | Sep 21, 2016
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Article Category: Research Article
Published Online: Sep 21, 2016
Page range: 633 - 640
Received: Jan 08, 2016
Accepted: Jul 17, 2016
DOI: https://doi.org/10.1515/msp-2016-0091
Keywords
© 2016 Kais Elghniji et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.

Fig. 1

Flow chart of the synthesis of transparent and translucent gels.
Flow chart of the synthesis of transparent and translucent gels.

Fig. 2

FT-IR spectra of (a) acetic acid, (b) isopropanol, (c) isopropyl acetate, (d) water. The dashed lines correspond to the bands of isopropyl acetate.
FT-IR spectra of (a) acetic acid, (b) isopropanol, (c) isopropyl acetate, (d) water. The dashed lines correspond to the bands of isopropyl acetate.

Fig. 3

FT-IR spectra of: (a) Ti(OC3H7)4, (b) mixture of esterification components, (c) transparent solution obtained after the addition of Ti(OC3H7)4 to the mixture of esterification after 30 min, (d) after 120 min.
FT-IR spectra of: (a) Ti(OC3H7)4, (b) mixture of esterification components, (c) transparent solution obtained after the addition of Ti(OC3H7)4 to the mixture of esterification after 30 min, (d) after 120 min.

Fig. 4

FT-IR spectra of xerogels obtained after drying the gels at T = 90 °C: (a) xerogels obtained from the solution (30 min); (b) (120 min); (c) pure TiO2 xerogel.
FT-IR spectra of xerogels obtained after drying the gels at T = 90 °C: (a) xerogels obtained from the solution (30 min); (b) (120 min); (c) pure TiO2 xerogel.

Fig. 5

XRD patterns of as-prepared samples obtained: (a) during 120 min, after drying at T = 90 °C; (b) sample with AcOH/Ti = 10, heated at 90 °C; (c) calcined at 250 °C; (d) at 450 °C.
XRD patterns of as-prepared samples obtained: (a) during 120 min, after drying at T = 90 °C; (b) sample with AcOH/Ti = 10, heated at 90 °C; (c) calcined at 250 °C; (d) at 450 °C.

Fig. 6

UV-Vis absorption spectra of: (a) transparent TiO2 xerogel (obtained during 120 min after drying at T = 90 °C) and (b) TiO2 anatase (commercial).
UV-Vis absorption spectra of: (a) transparent TiO2 xerogel (obtained during 120 min after drying at T = 90 °C) and (b) TiO2 anatase (commercial).

Fig. 7

(a) transparent monolithic gel obtained after one week (two different volumes); (b) transparent gel coated on a glass Petri dish; (c) transparent xerogel obtained after heating at 90 °C; (d) optical gel transformation from transparent to transluscent (1: transparent solution prepared for 120 min, obtained after three days), (3: transluscent gel with 3 mL of water), (4: transluscent gel with 6 mL of water).
(a) transparent monolithic gel obtained after one week (two different volumes); (b) transparent gel coated on a glass Petri dish; (c) transparent xerogel obtained after heating at 90 °C; (d) optical gel transformation from transparent to transluscent (1: transparent solution prepared for 120 min, obtained after three days), (3: transluscent gel with 3 mL of water), (4: transluscent gel with 6 mL of water).

Vibration frequencies of isopropyl acetate identified by infrared spectrometry after esterification reaction time 60 min at 75 °C.

Frequency vibration [cm-1]AttributionFrequency vibration [cm-1]Attribution
617–1184νC–C
870–1250νC–O
935–1378νsymC–H
1016–1448νanti–symC–H
1120–1754νC=O

Quantity of reagents and products in the esterification mixture after reaction time 60 min at 75 °C.

AcOH+iPrOH↔iPrOAc+H2O
T = 0 min ni (mol)0.340.3400
T= 60min nf(mol)0.19–0.150.15
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Language:
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Journal Subjects:
Materials Sciences, other, Nanomaterials, Functional and Smart Materials, Materials Characterization and Properties
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