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

 

Received: 11 September 2015/Accepted: 28 July 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; metakrilamida; radikal bebas

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*Corresponding author; email: marsin@kimia.fs.utm.my

 

 

 

 

 

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