Malaysian
Journal of Analytical Sciences Vol 18 No 2 (2014): 415 - 422
SYNTHESIS OF CHITOSAN-GRAFTED-POLY(METHYL
METHACRYLATE) WITH FENTON’S REAGENT (Fe2+ - H2O2)
AS A REDOX INITIATOR
(Sintesis Kitosan-Cangkuk-Poli(Metil
Metakrilat) Dengan Reagen Fenton (Fe2 + - H2O2)
Sebagai Pemula Redoks)
Nur Azmyra Abdul Aziz*, Aznizam
Abu Bakar, Azman Hassan, Nurulhusna Azmi
Enhanced Polymer
Research Group (ENPRO),
Department of
Polymer Engineering, Faculty of Chemical Engineering,
Universiti
Teknologi Malaysia, 81310 UTM Skudai, Johor, Malaysia.
*Corresponding author: azmyra_aziz@yahoo.com
Abstract
Graft
copolymerization of poly(methyl methacrylate)(PMMA) onto chitosan fiber has
been successfully carried out using Fenton’s Reagent which is consisted of
hydrogen peroxide(H2O2) as initiator and ferrous ammonium
sulphate(FAS) as co-catalyst under inert atmosphere in an aqueous medium. The
PMMA homopolymer formed during the reaction was removed from the grafted
copolymer by Soxhlet extraction using acetone as the solvent. The grafting
percentage and efficiency obtained were 449.16% and 85.94%, respectively. The
maximum grafting percentage and efficiency were achieved when 0.3 g chitosan
copolymerized with 3 mL monomer at 70oC for 120 minutes with [FAS] =
6 x 10-5 M, [H2O2] = 6 x 10-3 M and
8 mL water. The grafted copolymers were characterized by using FTIR, DSC, TGA
and SEM analysis. The presence of absorbance band at 1724 cm-1
provided strong evidence of grafting.
Keywords: graft
copolymers, chitosan, monomers, radical polymerization
Abstrak
Pengkopolimeran
cangkuk poli(metil metakrilat)(PMMA) terhadap gentian kitosan telah berjaya
dilakukan dengan menggunakan Reagen Fenton yang terdiri daripada hidrogen
peroksida (H2O2) sebagai pemula dan ferus ammonium sulfat
(FAS) sebagai ko-mangkin pada persekitaran atmosfera lengai dalam medium
berair. Homopolimer PMMA terbentuk semasa tindakbalas telah disingkirkan
daripada kopolimer cangkuk melalui kaedah pengekstrakan Soxhlet dengan
menggunakan aseton sebagai pelarut. Peratusan pencangkukan dan peratusan
kecekapan pencangkukan yang diperolehi masing-masing ialah 449.16% dan 85.94%.
Peratusan maksima pencangkukan dan kecekapan pencangkukan diperolehi apabila
0.3 g kitosan dikopolimer dengan 3 mL monomer pada 70oC selama 120
minit dengan mengunakan [FAS] = 6 x 10-5 M, [H2O2]
= 6 x 10-3 M dan 8 ml air. Kopolimer tercangkuk telah dicirikan
dengan menggunakan analisis FTIR, DSC, TGA dan SEM. Kehadiran kumpulan
penyerapan pada 1724 cm-1 menunjukkan bukti kukuh berlakunya
pencangkukan.
Kata kunci: kopolimer
cangkuk, kitosan, monomer, radikal pempolimeran
References
1.
Liu,
Z., Wu, G. & Liu, Y. (2006). Graft copolymerization of methyl acrylate onto
chitosan initiated by potassium diperiodatoargentate (III). Journal of Applied Polymer Science. 101
(1): 799-804.
2.
Flores-Ramirez,
N., Luna-Barcenas, G., Vasquez-Garcia, S., Munoz-Saldana, J., Elizalde-Pena,
E., Gupta, R., Sanchez, I., Gonzalez-Hernandez, J., Garcia-Gaitan, B. &
Villasenor-Ortega, F. (2008). Hybrid natural-synthetic chitosan resin: thermal
and mechanical behavior. Journal of
Biomaterials Science, Polymer Edition. 19 (2): 259-273.
3.
Radhakumary,
C., Nair, P. D., Mathew, S. & Nair, C. P. R. (2005). Biopolymer composite
of chitosan and methyl methacrylate for medical applications. Trends Biomater. Artif. Organs. 18 (2):
117-124.
4.
Bledzki,
A. K., Reihmane, S. & Gassan, J. (1996). Properties and modification
methods for vegetable fibers for natural fiber composites. Journal of Applied Polymer Science. 59 (8): 1329-1336.
5.
Prashanth,
K. V. H. & Tharanathan, R. N. (2003). Studies on graft copolymerization of
chitosan with synthetic monomers. Carbohydrate
Polymers. 54 (3): 343-351.
6.
Gupta,
K., Sahoo, S. & Khandekar, K. (2002). Graft copolymerization of ethyl
acrylate onto cellulose using ceric ammonium nitrate as initiator in aqueous
medium. Biomacromolecules. 3 (5): 1087-1094.
7.
Lagos,
A. & Reyes, J. (1988). Grafting onto chitosan. I. Graft copolymerization of
methyl methacrylate onto chitosan with Fenton's reagent (Fe2+−H2O2)
as a redox initiator. Journal of Polymer Science
Part A: Polymer Chemistry. 26 (4): 985-991.
8.
Prashanth,
K. & Tharanathan, R. (2003). Studies on graft copolymerization of chitosan
with synthetic monomers. Carbohydrate
Polymers. 54 (3): 343-351.
9.
Harish
Prashanth, K., Lakshman, K., Shamala, T. & Tharanathan, R. (2005).
Biodegradation of chitosan-graft-polymethylmethacrylate films. International Biodeterioration &
Biodegradation. 56 (2): 115-120.
10.
Abu
Bakar, A., Nik Mat, N. S. & Isnin, M. K. (2008). Optimized conditions for
the grafting reaction of poly (methyl methacrylate) onto oil-palm empty fruit
bunch fibers. Journal of Applied Polymer Science.
110 (2): 847-855.
11.
Das,
R. K., Basu, D. & Banerjee, A. (1999). Study of methyl-methacrylate-viscose
fiber graft copolymerization and the effect of grafting on thermal properties. Journal of Applied Polymer Science. 72
(1): 135-140.