Roslan , Rohaizu
(2015)
Isolation And Characterization Tempo Oxidized Nanocrystalline Cellulose From Oil Palm Empty Fruit Bunch.
PhD thesis, Universiti Sains Malaysia.
Abstract
Selulosa nanokristal daripada tandan buah kelapas sawit kosong (OPEFB-NCC) telah berjaya diasingkan, dengan hasil sebanyak 67% daripada OPEFB-MCC, melalui proses kimia dan mekanikal menggunakan pengoksidaan 4-acetamido-TEMPO/NaBr/NaClO dengan bantuan ultrasonik. Imej-imej TEM menunjukkan morfologi bagi OPEFB-NCC-MCC adalah kristal selulosa yang lurus dengan panjang 122 ± 45 nm, dan lebar seragam 4 ± 2 nm. Analisis FTIR dan 13C-NMR/MAS keadaan pepejal mencadangkan pengoksidaan berlaku di kumpulan hidroksil primer (C6) rantai selulosa dan OPEFB-NCC yang terhasil kebanyakannya terdiri daripada selulosa kristal jenis I. XRD dan 13C-NMR/MAS menunjukkan bahawa NCC mempunyai indeks kristal yang lebih rendah barbanding bahan permulaan. Analisis terma menunjukkan OPEFB-NCC terurai pada suhu rendah berbanding OPEFB-MCC, tetapi menghasilkan kadar arang yang tinggi iaitu 46% berbanding 7% bagi OPEFB-MCC.
Oil palm empty fruit bunch nanocrystalline cellulose (OPEFB-NCC) has been successfully isolated, with yields of 67%, from OPEFB-MCC via a chemical and mechanical process using 4-acetamido-TEMPO/NaBr/NaClO oxidation and ultrasonic treatment. TEM images indicate the morphology of OPEFB-NCC as straight crystals of cellulose with lengths 122 ± 45 nm, and uniform widths of 4 ± 2 nm. FTIR and 13C-NMR/MAS solid state analysis suggests that oxidation occurred at the site of the primary (C6) hydroxyl groups on the cellulose chain and that OPEFB-NCC consists primarily of crystalline cellulose I. XRD and 13C-NMR/MAS indicated that OPEFB-NCC had a lower crystallinity index than the OPEFB-MCC starting material. Thermal analysis revealed that OPEFB-NCC degraded at lower temperature than OPEFB-MCC, but had a much higher char content of 46% to the 7% of OPEFB-MCC.
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