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Sains Malaysiana 46(12)(2017): 2433–2440 http://dx.doi.org/10.17576/jsm-2017-4612-19
Ammonium Persulfate-initiated Graft Copolymerization
of Methacrylamide onto Chitosan: Synthesis, Characterization
and Optimization (Cangkukan Kopempolimeran Metakrilamida
ke Kitosan oleh Ammonium Persulfat: Sintesis, Pencirian dan
Pengoptimuman) ZETTY AZALEA
SUTIRMAN1,
MOHD
MARSIN
SANAGI1,2*,
AHMEDY
ABU
NAIM1,
KHAIRIL JUHANNI
ABD
KARIM1
& WAN AINI WAN
IBRAHIM1 1Department of Chemistry, Faculty
of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru,
Johor Darul Takzim, Malaysia 2Centre for Sustainable Nanomaterials,
Ibnu Sina Institute for Scientific and Industrial Research Universiti Teknologi Malaysia, 81310
UTM Johor Bahru, Johor Darul Takzim, Malaysia Diserahkan: 11 September 2015/Diterima:
28 Julai 2016 ABSTRACT
Ammonium persulfate (APS)-initiated
grafting of methacrylamide (MAM) onto chitosan was successfully
prepared for the first time by free radical mechanism. Both
chitosan and chitosan-graft-poly(methacrylamide) (chitosan-g-PMAM)
were characterized using Fourier transform infrared spectroscopy
(FTIR),
solid state 13C NMR, thermogravimetric analysis (TGA),
differential scanning calorimetry (DSC) and scanning electron microscopy
(SEM). Important factors affecting graft copolymerization
such as reaction time, temperature and concentrations of APS,
MAM
and chitosan were investigated and optimized to
obtain maximum grafting parameters. The optimum values for grafting
percentage and yield of graft copolymerization were achieved
under the following conditions: chitosan (1 g), MAM (4
g), APS (0.6 g), time reaction (4 h) and temperature (70ºC).
Keywords: Ammonium persulfate;
chitosan; free radical; graft copolymerization; methacrylamide
ABSTRAK
Cangkukan metakrilamida (MAM)
kepada kitosan dimulakan oleh ammonium persulfat (APS)
telah berjaya disediakan buat kali pertama melalui mekanisme
radikal bebas. Kedua-dua kitosan dan kitosan-cangkuk-polimetakrilamida
(kitosan-g-PMAM)
telah dicirikan menggunakan spektrometri inframerah transformasi
Fourier (FTIR),
13C
NMR
keadaan pepejal, analisis termogravimetri (TGA),
kalorimetri imbasan kebedaan (DSC) dan mikroskopi imbasan elektron
(SEM). Faktor penting dalam kopempolimeran cangkuk seperti
masa tindak balas, suhu dan kepekatan APS, MAM dan
kitosan telah dikaji dan dioptimum bagi memperoleh parameter
cangkukan maksima. Peratus cangkukan dan perolehan tertinggi
diperoleh dengan keadaan berikut: kitosan (1 g), MAM (4 g), APS (0.6
g), masa tindak balas (4 j) dan suhu (70ºC). Kata kunci: Ammonium persulfat; kitosan; kopempolimeran cangkuk;
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*Pengarang untuk surat-menyurat; email: marsin@kimia.fs.utm.my
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