Kirigiti, Emmanuel Abel (2026) Isolation Of Nanocellulose Crystals From Mature Coconut Shell (Cocos Nucifera) Biomass Via Organic And Inorganic Acid Hydrolysis: Structural, Morphological And Thermal Characterization. Masters thesis, Institut Teknologi Sepuluh Nopember.
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Abstract
Valorizing lignocellulosic waste into high-value nanomaterials provides a sustainable route for renewable bio-based materials. This study investigated mature coconut shell (Cocos nucifera) biomass as a precursor for nanocellulose crystals (NCC) through sequential chemical pretreatment and comparative acid hydrolysis. Raw coconut shell underwent alkaline treatment (5% NaOH, 75 °C, 4 h), followed by two-stage bleaching (1% and 4% sodium hypochlorite, at 75 °C for 5h and 3h, respectively) to remove non-cellulosic components. XRD showed the crystallinity index increased from 39.51% to 40.13% after alkalization and 67.43% after bleaching, confirming crystalline cellulose enrichment. FTIR confirmed enrichment by showing O-H (3410 cm-1), C-H (2908 cm-1), C-O-C/C-O (1159, 1050 cm-1), and β-glycosidic (893 cm-1) bands, alongside with reduced lignin and hemicellulose bands. SEM revealed a cleaner, rougher, and fibrillated cellulose surface. Purified cellulose was hydrolyzed using 6M lactic, acetic, hydrochloric, and sulfuric acids to produce nanocellulose (NC) referred to as NC-LA, NC-AA, NC-HA, and NC-SA, respectively, followed by ultrasonication. The NC FTIR spectra retained main cellulose bands, while NC-SA showed surface sulfate ester groups. NCC exhibited crystallinity indices of 68.51%, 70.53%, 72.70%, and 75.15%, with average TEM diameters of 20.4, 24.7, 15.6, and 12.1 nm. TGA-DTG showed improved thermal stability, with onset degradation increasing from 263.4, 293.5, to 300.6 °C for waste, alkalized, and bleached samples. NCC showed acid-dependent thermal behavior, with onset degradation at 290.4, 305.7, 298.3, and 283.9 °C for NC-LA, NC-AA, NC-HA, and NC-SA, respectively. Coconut shell biomass was successfully transformed into NCC with tunable properties, demonstrating potential for sustainable nanocellulose production.
Keywords Mature coconut shell; Nanocellulose crystals (NCC); Biomass valorization; Acid hydrolysis; Nanocellulose characterization
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Pemanfaatan limbah lignoselulosa menjadi nanomaterial bernilai tinggi memberikan jalur berkelanjutan untuk material berbasis bio terbarukan. Studi ini meneliti biomassa tempurung kelapa tua (Cocos nucifera) sebagai prekursor untuk kristal nanoselulosa (NCC) melalui pra-perlakuan kimia berurutan dan hidrolisis asam komparatif. Tempurung kelapa mentah menjalani perlakuan alkali (5% NaOH, 75 °C, 4 jam), diikuti dengan pemutihan dua tahap (1% dan 4% natrium hipoklorit, pada 75 °C selama 5 jam dan 3 jam, masing-masing) untuk menghilangkan komponen non-selulosa. XRD menunjukkan indeks kristalinitas meningkat dari 39,51% menjadi 40,13% setelah alkalinisasi dan 67,43% setelah pemutihan, yang mengkonfirmasi pengayaan selulosa kristalin. FTIR mengkonfirmasi pengayaan dengan menunjukkan pita O-H (3410 cm-1), C-H (2908 cm-1), C-O-C/C-O (1159, 1050 cm-1), dan β-glikosidik (893 cm-1), bersamaan dengan pita lignin dan hemiselulosa yang berkurang. SEM mengungkapkan permukaan selulosa yang lebih bersih, kasar, dan berserat. Selulosa murni dihidrolisis menggunakan asam laktat, asetat, klorida, dan sulfat 6M untuk menghasilkan nanoselulosa (NC) yang masing-masing disebut NC-LA, NC-AA, NC-HA, dan NC-SA, kemudian dilanjutkan dengan ultrasonikasi. Spektrum FTIR NCC mempertahankan pita selulosa utama, sedangkan NC-SA menunjukkan gugus ester sulfat permukaan. NCC menunjukkan indeks kristalinitas sebesar 68,51%, 70,53%, 72,70%, dan 75,15%, dengan diameter TEM rata-rata 20,4, 24,7, 15,6, dan 12,1 nm. TGA/DTG menunjukkan peningkatan stabilitas termal, dengan awal degradasi meningkat dari 263,4, 293,5, hingga 300,6 °C untuk sampel limbah, alkali, dan pemutih. NCC menunjukkan perilaku termal yang bergantung pada asam, dengan awal degradasi pada 290,4, 305,7, 298,3, dan 283,9 °C untuk NC-LA, NC-AA, NC-HA, dan NC-SA, masing-masing. Biomassa tempurung kelapa berhasil diubah menjadi NCC dengan sifat yang dapat disesuaikan, menunjukkan potensi untuk produksi nanoselulosa berkelanjutan. Kata kunci:Tempurung kelapa tua; Kristal nanoselulosa (NCC); Pemanfaatan biomassa; Hidrolisis asam; Karakterisasi nanoselulosa
| Item Type: | Thesis (Masters) |
|---|---|
| Uncontrolled Keywords: | Mature coconut shell; Nanocellulose crystals (NCC); Biomass valorization; Acid hydrolysis; Nanocellulose characterization |
| Subjects: | Q Science > QD Chemistry > QD1 Oxidation-reduction reaction. Q Science > QD Chemistry > QD320 Cellulose. Hydrolysis Q Science > QD Chemistry > QD481 Chemical structure. |
| Divisions: | Faculty of Science and Data Analytics (SCIENTICS) > Chemistry > 47101-(S2) Master Thesis |
| Depositing User: | Emmanuel Abel Kirigiti |
| Date Deposited: | 05 Aug 2026 01:56 |
| Last Modified: | 05 Aug 2026 01:56 |
| URI: | http://repository.its.ac.id/id/eprint/143872 |
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