Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite

Layered organic-inorganic hybrid nanocomposites were prepared by using pamoate ion (PA) as a guest into Zn-Al layered double hydroxide (Zn-Al-LDH) inorganic host by co-precipitation technique. Two methods of aging used in the synthesis process were conventional oil bath and microwave-assisted method...

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Main Author: Jubri @ Mohd Zufri, Zaemah
Format: Thesis
Language:English
English
Published: 2006
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Online Access:http://psasir.upm.edu.my/id/eprint/533/1/600382_fs_2006_19_abstrak_je__dh_pdf_.pdf
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spelling my-upm-ir.5332013-05-27T06:49:04Z Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite 2006-11 Jubri @ Mohd Zufri, Zaemah Layered organic-inorganic hybrid nanocomposites were prepared by using pamoate ion (PA) as a guest into Zn-Al layered double hydroxide (Zn-Al-LDH) inorganic host by co-precipitation technique. Two methods of aging used in the synthesis process were conventional oil bath and microwave-assisted methods. The Zn to Al molar ratio of the mother liquor was kept constant at 4 at the beginning of the synthesis with concentration of PA, 0.02 M. As the result of successful intercalation of pamoate ion into the interlayer structure of Zn-Al-LDH, an expansion of the interlayer spacing from 8.9 Å in the layered double hydroxide (ZAL) to 18.1 Å in the nanocomposite (ZAP) could be observed in the powder X-ray diffractogram. The advantage of using microwave-assisted method is that the time for aging process is shortened to only 15 to 30 minutes to achieve a well-ordered layered nanocomposite materials compared to 18 hours to age the sample if conventional oil bath method is used to synthesis the nanocomposite. Nanocomposite prepared using various Zn to Al molar ratios 2, 3, 4, 5, 6, 7 and 8 gave a well-ordered nanolayered structure. The effect of various Zn to Al ratios on the properties of layered organic-inorganic hybrid nanocomposite materials show that the BET surface area increases as the Zn to Al molar ratio increases. Nanocomposite prepared from various Zn to Al molar ratios using ion-exchange method, resulted in less ordered nanocomposite materials, with BET surface area in the range of (20.6 - 27.4) m2/g. Thermal decomposition of the nanocomposite was studied by heating the sample at 100-1000˚C under atmospheric condition. The layered structure of the nanocomposite collapsed when the sample was heated at 350˚C or higher and the formation of ZnO phase was observed at 400˚C or higher. Further heating at 1000˚C, resulted in the formation of ZnAl2O4 phase. It was also found that the release of PA anions from the interlamellae of the nanocomposite was controlled by the first order kinetics at least at the beginning of the reaction up to 7 hours. At the end of rapid release rate, the amount of PA released into the aqueous solution at various initial pH values was 16%, 20% and 30% for pH 2, pH 11 and pH 12, respectively. Nanocomposites (Materials). Layered double hydroxides. 2006-11 Thesis http://psasir.upm.edu.my/id/eprint/533/ http://psasir.upm.edu.my/id/eprint/533/1/600382_fs_2006_19_abstrak_je__dh_pdf_.pdf application/pdf en public phd doctoral Universiti Putra Malaysia Nanocomposites (Materials). Layered double hydroxides. Faculty of Science English
institution Universiti Putra Malaysia
collection PSAS Institutional Repository
language English
English
topic Nanocomposites (Materials).
Layered double hydroxides.

spellingShingle Nanocomposites (Materials).
Layered double hydroxides.

Jubri @ Mohd Zufri, Zaemah
Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite
description Layered organic-inorganic hybrid nanocomposites were prepared by using pamoate ion (PA) as a guest into Zn-Al layered double hydroxide (Zn-Al-LDH) inorganic host by co-precipitation technique. Two methods of aging used in the synthesis process were conventional oil bath and microwave-assisted methods. The Zn to Al molar ratio of the mother liquor was kept constant at 4 at the beginning of the synthesis with concentration of PA, 0.02 M. As the result of successful intercalation of pamoate ion into the interlayer structure of Zn-Al-LDH, an expansion of the interlayer spacing from 8.9 Å in the layered double hydroxide (ZAL) to 18.1 Å in the nanocomposite (ZAP) could be observed in the powder X-ray diffractogram. The advantage of using microwave-assisted method is that the time for aging process is shortened to only 15 to 30 minutes to achieve a well-ordered layered nanocomposite materials compared to 18 hours to age the sample if conventional oil bath method is used to synthesis the nanocomposite. Nanocomposite prepared using various Zn to Al molar ratios 2, 3, 4, 5, 6, 7 and 8 gave a well-ordered nanolayered structure. The effect of various Zn to Al ratios on the properties of layered organic-inorganic hybrid nanocomposite materials show that the BET surface area increases as the Zn to Al molar ratio increases. Nanocomposite prepared from various Zn to Al molar ratios using ion-exchange method, resulted in less ordered nanocomposite materials, with BET surface area in the range of (20.6 - 27.4) m2/g. Thermal decomposition of the nanocomposite was studied by heating the sample at 100-1000˚C under atmospheric condition. The layered structure of the nanocomposite collapsed when the sample was heated at 350˚C or higher and the formation of ZnO phase was observed at 400˚C or higher. Further heating at 1000˚C, resulted in the formation of ZnAl2O4 phase. It was also found that the release of PA anions from the interlamellae of the nanocomposite was controlled by the first order kinetics at least at the beginning of the reaction up to 7 hours. At the end of rapid release rate, the amount of PA released into the aqueous solution at various initial pH values was 16%, 20% and 30% for pH 2, pH 11 and pH 12, respectively.
format Thesis
qualification_name Doctor of Philosophy (PhD.)
qualification_level Doctorate
author Jubri @ Mohd Zufri, Zaemah
author_facet Jubri @ Mohd Zufri, Zaemah
author_sort Jubri @ Mohd Zufri, Zaemah
title Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite
title_short Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite
title_full Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite
title_fullStr Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite
title_full_unstemmed Synthesis and Physicochemical Characterization of Pamoate-Intercalated Zinc-Aluminium Layered Double Hydroxide Hybrid Nanocomposite
title_sort synthesis and physicochemical characterization of pamoate-intercalated zinc-aluminium layered double hydroxide hybrid nanocomposite
granting_institution Universiti Putra Malaysia
granting_department Faculty of Science
publishDate 2006
url http://psasir.upm.edu.my/id/eprint/533/1/600382_fs_2006_19_abstrak_je__dh_pdf_.pdf
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