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  1. Kian LK, Saba N, Jawaid M, Fouad H
    Int J Biol Macromol, 2020 Aug 01;156:347-353.
    PMID: 32278601 DOI: 10.1016/j.ijbiomac.2020.04.015
    Olive fiber is a renewable natural fiber which has potential as an alternative biomass for extraction of microcrystalline cellulose (MCC). MCC has been widely applied in various industries owing to its small dimensional size for ease of reactive fabrication process. At present study, a serial treatments of bleaching, alkaline and acid hydrolysis was employed to extract OL-BLF, OL-PUF, and OL-MCC respectively from olive stem fiber. In morphology examination, a feature of short micro-crystallite particles was obtained for OL-MCC. The particle size was found gradually reducing from OL-PUF (305.31 μm) to OL-MCC (156.06 μm) due to the disintegration of cellulose fibrils. From physicochemical analysis, most lignin and hemicellulose components had been removed from OL-BLF to form OL-PUF with individually fibril structure. The elemental analysis revealed that highly pure cellulose component was obtained for OL-MCC. Also, the rigidity had been improved from OL-BLF to OL-PUF, while with the highest for OL-MCC with 74.2% crystallinity, endowing it as a reliable load-bearing agent. As for thermal analysis, OL-MCC had the most stable heat resistance in among the chemically-treated fibers. Therefore, olive MCC could act as a promising reinforcing agent to withstand harsh conditions for variety fields of composite applications.
  2. Kian LK, Saba N, Jawaid M, Sultan MTH
    Int J Biol Macromol, 2019 Jan;121:1314-1328.
    PMID: 30208300 DOI: 10.1016/j.ijbiomac.2018.09.040
    The utilization of nanocellulose has increasingly gained attentions from various research fields, especially the field of polymer nanocomposites owing to the growing environmental hazardous of petroleum based fiber products. Meanwhile, the searching of alternative cellulose sources from different plants has become the interests for producing nanocellulose with varying characterizations that expectedly suit in specific field of applications. In this content the long and strong bast fibers from plant species was gradually getting its remarkable position in the field of nanocellulose extraction and nanocomposites fabrications. This review article intended to present an overview of the chemical structure of cellulose, different types of nanocellulose, bast fibers compositions, structure, polylactic acid (PLA) and the most probable processing techniques on the developments of nanocellulose from different bast fibers especially jute, kenaf, hemp, flax, ramie and roselle and its nanocomposites. This article however more focused on the fabrication of PLA based nanocomposites due to its high firmness, biodegradability and sustainability properties in developed products towards the environment. Along with this it also explored a couple of issues to improve the processing techniques of bast fibers nanocellulose and its reinforcement in the PLA biopolymer as final products.
  3. Kian LK, Jawaid M, Alamery S, Vaseashta A
    Nanomaterials (Basel), 2021 Jan 20;11(2).
    PMID: 33498162 DOI: 10.3390/nano11020255
    The development of membrane technology from biopolymer for water filtration has received a great deal of attention from researchers and scientists, owing to the growing awareness of environmental protection. The present investigation is aimed at producing poly(D-lactic acid) (PDLA) membranes, incorporated with nanocrystalline cellulose (NCC) and cellulose nanowhisker (CNW) at different loadings of 1 wt.% (PDNC-I, PDNW-I) and 2 wt.% (PDNC-II PDNW-II). From morphological characterization, it was evident that the nanocellulose particles induced pore formation within structure of the membrane. Furthermore, the greater surface reactivity of CNW particles facilitates in enhancing the surface wettability of membranes due to increased hydrophilicity. In addition, both thermal and mechanical properties for all nanocellulose filled membranes under investigation demonstrated significant improvement, particularly for PDNW-I-based membranes, which showed improvement in both aspects. The membrane of PDNW-I presented water permeability of 41.92 L/m2h, when applied under a pressure range of 0.1-0.5 MPa. The investigation clearly demonstrates that CNWs-filled PDLA membranes fabricated for this investigation have a very high potential to be utilized for water filtration purpose in the future.
  4. Aziman N, Kian LK, Jawaid M, Sanny M, Alamery S
    Polymers (Basel), 2021 Jan 27;13(3).
    PMID: 33513665 DOI: 10.3390/polym13030391
    The development of antimicrobial film for food packaging application had become the focus for researchers and scientists. This research aims to study the characteristics and antimicrobial activity of novel biofilms made of poly (butylene succinate) (PBS) and tapioca starch (TPS) added with 1.5% or 3% of Biomaster-silver (BM) particle. In morphological examination, the incorporation of 3% BM particle was considerably good in forming well-structured PBS film. Meanwhile, the functional groups analysis revealed the 3% BM particle was effectively interacted with PBS molecular chains. The flame retard behavior of BM metal particle also helped in enhancing the thermal stability for pure PBS and PBS/TPS films. The nucleating effect of BM particles had improved the films crystallinity. Small pore size features with high barrier property for gas permeability was obtained for BM filled PBS/TPS films. From antimicrobial analysis, the BM particles possessed antimicrobial activity against three bacteria Staphylococcus aureus, Escherichia coli, and Salmonella Typhimurium in which PBS/TPS 3% BM film exhibited strong antimicrobial activity against all tested bacteria, however, PBS/TPS 1.5% BM film exhibited strong antimicrobial activity against E. coli only. Hence, the incorporation of BM into PBS/TPS film could be a sustainable way for developing packaging films to preserve food products.
  5. Kian LK, Saba N, Jawaid M, Alothman OY, Fouad H
    Carbohydr Polym, 2020 Aug 01;241:116423.
    PMID: 32507177 DOI: 10.1016/j.carbpol.2020.116423
    Olive fiber is a sustainable material as well as alternative biomass for extraction of nanocrystalline cellulose (NCC), which has been widely applied in various industries. In the present study, ONC-I, ONC-II, and ONC-III were extracted from olive stem fiber at different hydrolysis reaction times of 30 min, 45 min, and 60 min, respectively. The nanoparticle size was found gradually reducing from ONC-I (11.35 nm width, 168.28 nm length) to ONC-III (6.92 nm width, 124.16 nm length) due to the disintegration of cellulose fibrils. ONC-II and ONC-III possessed highly pure cellulose compartments and enhanced crystals structure. This study also showed that rigidity increased from ONC-I to ONC-II. ONC-III showed the highest crystallinity of 83.1 %, endowing it as a potentially reliable load-bearing agent. Moreover, ONC-III exhibited highest stable heat resistance among the chemically-isolated nanocellulose. We concluded that olive NCC could be promising materials for a variety of industrial applications in various fields.
  6. Azum N, Jawaid M, Kian LK, Khan A, Alotaibi MM
    Polymers (Basel), 2021 Sep 08;13(18).
    PMID: 34577931 DOI: 10.3390/polym13183030
    Washingtonia is a desert plant with great sustainability and renewability in nature and is abundantly cultivated across global urban regions. Its fibre biomass comprises cellulose as the major structural part, and this is why it can be potentially utilized as an alternative biomaterial for manufacturing microcrystalline cellulose (MCC) products that can be widely applied in industrial fields. In the present study, NaOH-treated Washingtonia fibre (WAKL), NaClO2-treated Washingtonia fibre (WBLH), and Washingtonia microcrystalline cellulose (WMCC) were extracted through combined treatments of alkalization, bleaching, and acidic hydrolysis, respectively. The obtained chemically treated fibre samples were subjected to characterization to investigate their morphology, physico-chemistry, and thermal stability. In a morphological examination, the large bunch WAKL fibre reduced into small size WMCC fibrils, evidencing that the lignin and hemicellulose components were greatly eliminated through chemical dissolution. The elemental composition revealed that almost all impurities of anions and cations had been removed, particularly for the WMCC sample, showing its high purity of cellulose content. Additionally, the WMCC sample could attain at 25% yield, giving it the advantage for feasible economic production. Furthermore, the physicochemical analysis, Fourier Transform Infrared-ray (FTIR), indicated the presence of a crystalline cellulose region within the WMCC structure, which had promoted it with high crystallinity of 72.6% as examined by X-ray diffraction (XRD). As for thermal analysis, WMCC showed greater thermal stability comparing to WAKL and WBLC samples at high temperature. Therefore, Washingtonia fibre can be a reliable biosubstituent to replace other plant material for MCC production in the future.
  7. Kian LK, Jawaid M, Ariffin H, Alothman OY
    Int J Biol Macromol, 2017 Oct;103:931-940.
    PMID: 28549863 DOI: 10.1016/j.ijbiomac.2017.05.135
    In this study, microcrystalline cellulose (MCC) was extracted from roselle fiber through acid hydrolysis treatment and its properties were compared with those of commercially available MCC. The physicochemical and morphological characteristics, elemental composition, size distribution, crystallinity and thermal properties of the obtained MCC were analyzed in this work. Fourier transform infrared spectroscopy (FTIR) analysis provided clear evidence that the characteristic peak of lignin was absent in the spectrum of the MCC prepared from roselle fiber. Rough surface and slight aggregation of MCC were observed by scanning electron microscopy (SEM). Energy dispersive X-ray (EDX) analysis showed that pure MCC with small quantities of residues and impurities was obtained, with a similar elemental composition to that of commercial MCC. A mean diameter of approximately 44.28μm was measured for MCC by using a particle size analyzer (PSA). X-ray diffraction (XRD) showed the crystallinity increased from 63% in roselle pulp to 78% in roselle MCC, the latter having a slightly higher crystallinity than that of commercial MCC (74%). TGA and DSC results indicated that the roselle MCC had better thermal stability than the roselle pulp, whereas it had poorer thermal stability in comparison with commercial MCC. Thus, the isolated MCC from roselle fibers will be going to use as reinforcing element in green composites and may be a precursor for future roselle derived nanocellulose, and thus a promising subject in nanocomposite research.
  8. Kian LK, Jawaid M, Nasef MM, Fouad H, Karim Z
    Int J Biol Macromol, 2021 Dec 01;192:654-664.
    PMID: 34655581 DOI: 10.1016/j.ijbiomac.2021.10.042
    In this study, poly(lactic acid) (PLA)/poly(butylene succinate) (PBS) dual-layer membranes filled with 0-3 wt% cellulose nanowhisker (CNWs) were fabricated with aim to remove metal ions from wastewater. An integrated method was employed in the membrane fabrication process by combining water vapor-induced and crystallization-induced phase inversions. The membrane thickness was measured in between 11 and 13 μm, which did not pose significant flux deviation during filtration process. The 3% CNW filled membrane showed prominent and well-laminated two layers structure. Meanwhile, the increase in CNWs from 0 to 3% loadings could improve the membrane porosity (43-74%) but reducing pore size (2.45-0.54 μm). The heat resistance of neat membrane enhanced by 1% CNW but decreased with loadings of 2-3% CNWs due to flaming behavior of sulphated nanocellulose. Membrane with 3% CNW displayed the tensile strength (23.5 MPa), elongation at break (7.1%), and Young's modulus (0.75 GPa) as compared to other samples. For wastewater filtration performance, the continuous operation test showed that 3% CNW filled membrane exhibited the highest removal efficiency for both cobalt and nickel metal ions reaching to 83% and 84%, respectively. We concluded that CNWs filled dual-layer membranes have potential for future development in the removal of heavy metal ions from wastewater streams.
  9. Kian LK, Jawaid M, Ariffin H, Karim Z
    Int J Biol Macromol, 2018 Jul 15;114:54-63.
    PMID: 29551511 DOI: 10.1016/j.ijbiomac.2018.03.065
    Roselle fiber is a renewable and sustainable agricultural waste enriched with cellulose polysaccharides. The isolation of Nanocrystalline cellulose (NCC) from roselle-derived microcrystalline cellulose (MCC) is an alternative approach to recover the agricultural roselle plant residue. In the present study, acid hydrolysis with different reaction time was carried out to degrade the roselle-derived MCC to form NCC. The characterizations of isolated NCC were conducted through Fourier Transform Infrared Ray (FTIR), Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS), Energy Dispersive Spectroscopy (EDS), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). As evaluated from the performed morphological investigations, the needle-like shape NCC nanostructures were observed under TEM and AFM microscopy studies, while irregular rod-like shape of NCC was observed under FESEM analysis. With 60min hydrolysis time, XRD analysis demonstrated the highest NCC crystallinity degree with 79.5%. In thermal analysis by TGA and DSC, the shorter hydrolysis time tended to produce NCC with higher thermal stability. Thus, the isolated NCC from roselle-derived MCC has high potential to be used in application of pharmaceutical and biomedical fields for nanocomposite fabrication.
  10. Mohamad N, Mazlan MM, Tawakkal ISMA, Talib RA, Kian LK, Fouad H, et al.
    Int J Biol Macromol, 2020 Nov 15;163:1451-1457.
    PMID: 32738328 DOI: 10.1016/j.ijbiomac.2020.07.209
    The growing global awareness for environmental protection has inspired the exploration on producing active packaging films from bio-based materials. In present work, three types of active agents were studied by incorporating thymol(T), kesum(K), and curry(C) (10% wt.) into polylactic acid (PLA) to produce PLA-10T, PLA-10K, and PLA10-C packaging films via solvent casting method. The morphology, functional chemistry, thermal stability, permeability, and antimicrobial properties were evaluated for PLA films. Functional chemical analysis confirmed the presence of interfacial bonding between aromatic groups of active agents and PLA carbonyl group. PLA-10K exhibited the highest thermal resistance comparing to PLA-10T and PLA-10C while water vapor barrier was enhanced after incorporation of active agents. Qualitative observation had indicated that chicken meat could be preserved in the active films until 15 days, while odourless and firm texture properties retained in food sample. For disc diffusion assay (in vitro), it showed positive results against Gram-positive bacteria (Staphylococcus aureus) whereas with negative results against Gram-negative bacteria (Escherichia coli) and Aspergillus Brasiliensis due to embedded active agents within PLA matrix. We concluded that produced active agents filled PLA films potential to use in food packaging application to enhance the shelf life of meats, fruits and vegetables product.
  11. Fouad H, Kian LK, Jawaid M, Alotaibi MD, Alothman OY, Hashem M
    Polymers (Basel), 2020 Dec 07;12(12).
    PMID: 33297332 DOI: 10.3390/polym12122926
    Conocarpus fiber is an abundantly available and sustainable cellulosic biomass. With its richness in cellulose content, it is potentially used for manufacturing microcrystalline cellulose (MCC), a cellulose derivative product with versatile industrial applications. In this work, different samples of bleached fiber (CPBLH), alkali-treated fiber (CPAKL), and acid-treated fiber (CPMCC) were produced from Conocarpus through integrated chemical process of bleaching, alkaline cooking, and acid hydrolysis, respectively. Characterizations of samples were carried out with Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDX), Fourier Transform Infrared-Ray (FTIR), X-ray Diffraction (XRD), Thermogravimetric (TGA), and Differential Scanning Calorimetry (DSC). From morphology study, the bundle fiber feature of CPBLH disintegrated into micro-size fibrils of CPMCC, showing the amorphous compounds were substantially removed through chemical depolymerization. Meanwhile, the elemental analysis also proved that the traces of impurities such as cations and anions were successfully eliminated from CPMCC. The CPMCC also gave a considerably high yield of 27%, which endowed it with great sustainability in acting as alternative biomass for MCC production. Physicochemical analysis revealed the existence of crystalline cellulose domain in CPMCC had contributed it 75.7% crystallinity. In thermal analysis, CPMCC had stable decomposition behavior comparing to CPBLH and CPAKL fibers. Therefore, Conocarpus fiber could be a promising candidate for extracting MCC with excellent properties in the future.
  12. Khan A, Jawaid M, Kian LK, Khan AAP, Asiri AM
    Polymers (Basel), 2021 Jun 01;13(11).
    PMID: 34206136 DOI: 10.3390/polym13111835
    Conocarpus fiber is a lignocellulosic biomass rich in cellulose potentially used for producing nanocrystalline cellulose (NCC), a biomaterial extensively employed in various application fields. In the present work, different hydrolysis times of 10, 20 and 30 min were applied to chemically pre-treated Conocarpus fiber to produce CPNC1, CPNC2, and CPNC3 particles. With acid hydrolysis treatment, the yield of NCC product was successfully retained at 17-19%. Individual, rod-like shapes of NCC particles could be clearly observed under microscopy examination. From chemical composition analysis, a relatively pure cellulose compartment was produced for all NCC samples with substantial removal of lignin and hemicellulose. The physicochemical analysis proved that each nanoparticle sample possessed strong cellulose crystalline structure. For thermal analyses, the heat resistance of NCCs was gradually enhanced with the increased hydrolysis times. Therefore, the extracted NCC product from Conocarpus fiber could be a green nano-filler for developing nanocomposite material in the future.
  13. Hachaichi A, Kouini B, Kian LK, Asim M, Fouad H, Jawaid M, et al.
    Materials (Basel), 2021 Sep 15;14(18).
    PMID: 34576536 DOI: 10.3390/ma14185313
    Date palm fiber (Phoenix dactylifera L.) is a natural biopolymer rich in lignocellulosic components. Its high cellulose content lends them to the extraction of tiny particles like microcrystalline cellulose (MCC) and nanocrystalline cellulose (NCC). These cellulose-derived small size particles can be used as an alternative biomaterial in wide fields of application due to their renewability and sustainability. In the present work, NCC (A) and NCC (B) were isolated from date palm MCC at 60 min and 90 min hydrolysis times, respectively. The isolated NCC product was subjected to characterization to study their properties differences. With the hydrolysis treatment, the yields of produced NCC could be attained at between 22% and 25%. The infrared-ray functional analysis also revealed the isolated NCC possessed a highly exposed cellulose compartment with minimized lignoresidues of lignin and hemicellulose. From morphology evaluation, the nanoparticles' size was decreased gradually from NCC (A) (7.51 nm width, 139.91 nm length) to NCC (B) (4.34 nm width, 111.51 nm length) as a result of fragmentation into cellulose fibrils. The crystallinity index was found increasing from NCC (A) to NCC (B). With 90 min hydrolysis time, NCC (B) showed the highest crystallinity index of 71% due to its great cellulose rigidity. For thermal analysis, NCC (B) also exhibited stable heat resistance, in associating with its highly crystalline cellulose structure. In conclusion, the NCC isolated from date palm MCC would be a promising biomaterial for various applications such as biomedical and food packaging applications.
  14. Yusof NL, Mutalib NA, Nazatul UK, Nadrah AH, Aziman N, Fouad H, et al.
    Foods, 2021 Oct 08;10(10).
    PMID: 34681430 DOI: 10.3390/foods10102379
    Food contamination leading to the spoilage and growth of undesirable bacteria, which can occur at any stage along the food chain, is a significant problem in the food industry. In the present work, biopolymer polybutylene succinate (PBS) and polybutylene succinate/tapioca starch (PBS/TPS) films incorporating Biomaster-silver (BM) and SANAFOR® (SAN) were prepared and tested as food packaging to improve the lifespan of fresh chicken breast fillets when kept in a chiller for seven days. The incorporation of BM and SAN into both films demonstrated antimicrobial activity and could prolong the storability of chicken breast fillets until day 7. However, PBS + SAN 2%, PBS/TPS + SAN 1%, and PBS/TPS + SAN 2% films showed the lowest microbial log growth. In quality assessment, incorporation of BM and SAN into both film types enhanced the quality of the chicken breast fillets. However, PBS + SAN 1% film showed the most notable enhancement of chicken breast fillet quality, as it minimized color variation, slowed pH increment, decreased weight loss, and decelerated the hardening process of the chicken breast fillets. Therefore, we suggest that the PBS + SAN and PBS/TPS + SAN films produced in this work have potential use as antimicrobial packaging in the future.
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