Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions

Natural biopolymers such as chitosan have high potential as sorbents for a wide range of applications. However, these materials present significant limitations that require appropriate modifications. In this study, chitosan was modified by crosslinking and grafting and the newly prepared grafted cop...

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Main Author:	Sutirman, Zetty Azalea
Format:	Thesis
Language:	English
Published:	2017
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/81621/1/ZettyAzaleaSutirmanPFS2017.pdf
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spelling	my-utm-ep.816212019-09-10T01:50:07Z Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions 2017 Sutirman, Zetty Azalea QD Chemistry Natural biopolymers such as chitosan have high potential as sorbents for a wide range of applications. However, these materials present significant limitations that require appropriate modifications. In this study, chitosan was modified by crosslinking and grafting and the newly prepared grafted copolymers were evaluated as sorbents for the removal of a selected dye, Orange G (OG) and several heavy metal ions (Pb(II), Cu(II) and Cd(II)) from aqueous solutions. Chitosan beads were produced from their commercial form and crosslinked with glutaraldehyde to enhance their stability in acidic medium. The crosslinked chitosan beads were then grafted separately with two different monomers, namely methacrylamide and Nvinyl- 2-pyrrolidone by conventional free radical polymerization using ammonium persulfate as an initiator. The modified chitosan beads were characterized using Fourier transform infrared (FTIR) spectroscopy, solid state 13C nuclear magnetic resonance (13C NMR) spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and CHN analysis to provide evidence of successful crosslinking and grafting. The solubility and swelling of the grafted copolymers and chitosan beads were investigated. The optimum percentage grafting (263.5%) for the preparation of crosslinked chitosangraft- poly(methacrylamide) (cts(x)-g-PMAm) was obtained at reaction temperature of 60°C, reaction time of 3 h, 2.63 x 10-1 mol L-1 of ammonium persulfate, 17.62 x 10-1 mol L-1 of methacrylamide and 1 g of crosslinked chitosan beads. Meanwhile, the optimum percentage grafting (138%) for the preparation of crosslinked chitosangraft- poly(N-vinyl-2-pyrrolidone) (cts(x)-g-PNVP), was achieved using reaction temperature of 60°C, reaction time of 2 h, 2.63 x 10-1 mol L-1 of ammonium persulfate, 26.99 x 10-1 mol L-1 of N-vinyl-2-pyrrolidone and 1.5 g of crosslinked chitosan beads. It was found that (cts(x)-g-PMAm) and (cts(x)-g-PNVP) beads showed significantly higher maximum adsorption capacities, qmax, for OG (25.8 mg g-1 and 63.7 mg g-1, respectively) as compared to that of unmodified chitosan beads (1.7 mg g-1). It was also proven that the Langmuir model fitted very well with the experimental adsorption data for OG and the selected heavy metal ions with R2 of nearly unity, while the adsorption kinetics were well described by the pseudo-second order kinetic model. In addition, the adsorbent-adsorbate interactions were elucidated by means of FTIR and X-ray photoelectron spectroscopy (XPS). This study concludes that both cts(x)-g-PMAm and cts(x)-g-PNVP beads are potentially useful as sorbents for the removal of pollutants from water and wastewater. 2017 Thesis http://eprints.utm.my/id/eprint/81621/ http://eprints.utm.my/id/eprint/81621/1/ZettyAzaleaSutirmanPFS2017.pdf application/pdf en public phd doctoral Universiti Teknologi Malaysia Chemistry
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	QD Chemistry
spellingShingle	QD Chemistry Sutirman, Zetty Azalea Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
description	Natural biopolymers such as chitosan have high potential as sorbents for a wide range of applications. However, these materials present significant limitations that require appropriate modifications. In this study, chitosan was modified by crosslinking and grafting and the newly prepared grafted copolymers were evaluated as sorbents for the removal of a selected dye, Orange G (OG) and several heavy metal ions (Pb(II), Cu(II) and Cd(II)) from aqueous solutions. Chitosan beads were produced from their commercial form and crosslinked with glutaraldehyde to enhance their stability in acidic medium. The crosslinked chitosan beads were then grafted separately with two different monomers, namely methacrylamide and Nvinyl- 2-pyrrolidone by conventional free radical polymerization using ammonium persulfate as an initiator. The modified chitosan beads were characterized using Fourier transform infrared (FTIR) spectroscopy, solid state 13C nuclear magnetic resonance (13C NMR) spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and CHN analysis to provide evidence of successful crosslinking and grafting. The solubility and swelling of the grafted copolymers and chitosan beads were investigated. The optimum percentage grafting (263.5%) for the preparation of crosslinked chitosangraft- poly(methacrylamide) (cts(x)-g-PMAm) was obtained at reaction temperature of 60°C, reaction time of 3 h, 2.63 x 10-1 mol L-1 of ammonium persulfate, 17.62 x 10-1 mol L-1 of methacrylamide and 1 g of crosslinked chitosan beads. Meanwhile, the optimum percentage grafting (138%) for the preparation of crosslinked chitosangraft- poly(N-vinyl-2-pyrrolidone) (cts(x)-g-PNVP), was achieved using reaction temperature of 60°C, reaction time of 2 h, 2.63 x 10-1 mol L-1 of ammonium persulfate, 26.99 x 10-1 mol L-1 of N-vinyl-2-pyrrolidone and 1.5 g of crosslinked chitosan beads. It was found that (cts(x)-g-PMAm) and (cts(x)-g-PNVP) beads showed significantly higher maximum adsorption capacities, qmax, for OG (25.8 mg g-1 and 63.7 mg g-1, respectively) as compared to that of unmodified chitosan beads (1.7 mg g-1). It was also proven that the Langmuir model fitted very well with the experimental adsorption data for OG and the selected heavy metal ions with R2 of nearly unity, while the adsorption kinetics were well described by the pseudo-second order kinetic model. In addition, the adsorbent-adsorbate interactions were elucidated by means of FTIR and X-ray photoelectron spectroscopy (XPS). This study concludes that both cts(x)-g-PMAm and cts(x)-g-PNVP beads are potentially useful as sorbents for the removal of pollutants from water and wastewater.
format	Thesis
qualification_name	Doctor of Philosophy (PhD.)
qualification_level	Doctorate
author	Sutirman, Zetty Azalea
author_facet	Sutirman, Zetty Azalea
author_sort	Sutirman, Zetty Azalea
title	Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
title_short	Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
title_full	Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
title_fullStr	Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
title_full_unstemmed	Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
title_sort	poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions
granting_institution	Universiti Teknologi Malaysia
granting_department	Chemistry
publishDate	2017
url	http://eprints.utm.my/id/eprint/81621/1/ZettyAzaleaSutirmanPFS2017.pdf
_version_	1747818373257887744

Poly(methacrylamide) and poly(n-vinyl-2-pyrrolidone) grafted crosslinked chitosan for removal of orange g and selected heavy metal ions from aqueous solutions

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