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A special issue of Polymers (ISSN 2073-4360). This special issue belongs to the section "Circular and Green Polymer Science".

Deadline for manuscript submissions: closed (29 February 2024) | Viewed by 20766

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Dr. Marta Fernandes

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Centre for Textile Science and Technology (2C2T), Campus de Azurém, Universidade do Minho, 4800-058 Guimaraes, Portugal
Interests: textile functionalization; bacterial nanocellulose; composites; nanomaterials; natural dyes; plasma functionalization
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Dr. Jorge Padrão

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Centre for Textile Science and Technology (2C2T), University of Minho, 4800-058 Guimarães, Portugal
Interests: textile materials; biotechnology; biomaterials; antimicrobials; bioreactor optimization; nanotechnology; environmental biotechnology; industrial biotechnology
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Dear Colleagues,

Today's world is witnessing a growing concern for the environment as a result of global warming, energy crises, and waste generation. The growing demand for products with a low environmental impact has led to a greater focus on sustainable and renewable materials by the scientific community. In this scenario, cellulose is one of the most prominent candidates for use in different fields of applications in a sustainable manner, with regard to its abundant availability from various resources. In particular, nanocellulose presents outstanding characteristics, such as renewability, a high aspect ratio, good mechanical properties, excellent biocompatibility, hydrogen-bonding capacity, reinforcing potential, and degradability.

The scope of this Special Issue is to report recent achievements in the advanced preparation and emerging applications of cellulose-based materials. In particular, topics of interest include, but are not limited to, the following:

Healthcare;
Water purification;
Energy storage;
Filtration;
Environment;
Automotive;
Aerospace;
Defence;
Sensors;
Adhesives;
Packaging;
Food;
Construction.

Dr. Marta Fernandes
Dr. Jorge Padrão
Guest Editors

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Polymers is an international peer-reviewed open access semimonthly journal published by MDPI.

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Related Special Issue

Advanced Preparation and Application of Cellulose: 2nd Edition in Polymers

Published Papers (13 papers)

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Research

19 pages, 2296 KiB

Open AccessArticle

Production and Characterization of Nanocellulose from Maguey (Agave cantala) Fiber

by Erwin C. Sumarago, Mary Frahnchezka M. dela Cerna, Andrea Kaylie B. Leyson, Noel Peter B. Tan and Kendra Felizimarie Peñol Magsico

Polymers 2024, 16(10), 1312; https://doi.org/10.3390/polym16101312 - 7 May 2024

Viewed by 512

Abstract

Plant fibers have been studied as sources of nanocellulose due to their sustainable features. This study investigated the effects of acid hydrolysis parameters, reaction temperature, and acid concentration on nanocellulose yield from maguey (Agave cantala) fiber. Nanocellulose was produced from the fibers via the removal of non-cellulosic components through alkali treatment and bleaching, followed by strong acid hydrolysis for 45 min using sulfuric acid (H₂SO₄). The temperature during acid hydrolysis was 30, 40, 50, and 60 °C, and the H₂SO₄ concentration was 40, 50, and 60 wt. % H₂SO₄. Results showed that 53.56% of raw maguey fibers were isolated as cellulose, that is, 89.45% was α-cellulose. The highest nanocellulose yield of 81.58 ± 0.36% was achieved from acid hydrolysis at 50 °C using 50 wt. % H₂SO₄, producing nanocellulose measuring 8–75 nm in diameter and 72–866 nm in length, as confirmed via field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) analysis. Fourier-transform infrared spectroscopy (FTIR) analysis indicated the chemical transformation of fibers throughout the nanocellulose production process. The zeta potential analysis showed that the nanocellulose had excellent colloidal stability with a highly negative surface charge of −37.3 mV. Meanwhile, X-ray diffraction (XRD) analysis validated the crystallinity of nanocellulose with a crystallinity index of 74.80%. Lastly, thermogravimetric analysis (TGA) demonstrated that the inflection point attributed to the cellulose degradation of the produced nanocellulose is 311.41 °C. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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21 pages, 2986 KiB

Open AccessArticle

Determining the Relationship between Delivery Parameters and Ablation Distribution for Novel Gel Ethanol Percutaneous Therapy in Ex Vivo Swine Liver

by Erika Chelales, Katriana von Windheim, Arshbir Singh Banipal, Elizabeth Siebeneck, Claire Benham, Corrine A. Nief, Brian Crouch, Jeffrey I. Everitt, Alan Alper Sag, David F. Katz and Nirmala Ramanujam

Polymers 2024, 16(7), 997; https://doi.org/10.3390/polym16070997 - 5 Apr 2024

Viewed by 564

Abstract

Ethyl cellulose–ethanol (ECE) is emerging as a promising formulation for ablative injections, with more controllable injection distributions than those from traditional liquid ethanol. This study evaluates the influence of salient injection parameters on forces needed for infusion, depot volume, retention, and shape in a large animal model relevant to human applications. Experiments were conducted to investigate how infusion volume (0.5 mL to 2.5 mL), ECE concentration (6% or 12%), needle gauge (22 G or 27 G), and infusion rate (10 mL/h) impacted the force of infusion into air using a load cell. These parameters, with the addition of manual infusion, were investigated to elucidate their influence on depot volume, retention, and shape (aspect ratio), measured using CT imaging, in an ex vivo swine liver model. Force during injection increased significantly for 12% compared to 6% ECE and for 27 G needles compared to 22 G. Force variability increased with higher ECE concentration and smaller needle diameter. As infusion volume increased, 12% ECE achieved superior depot volume compared to 6% ECE. For all infusion volumes, 12% ECE achieved superior retention compared to 6% ECE. Needle gauge and infusion rate had little influence on the observed depot volume or retention; however, the smaller needles resulted in higher variability in depot shape for 12% ECE. These results help us understand the multivariate nature of injection performance, informing injection protocol designs for ablations using gel ethanol and infusion, with volumes relevant to human applications. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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15 pages, 2867 KiB

Open AccessArticle

Determination of the Mass Fractions of the Heavy Metals in the Recycled Cellulose Pulp

by Mia Klemenčić, Ivana Bolanča Mirković, Nenad Bolf and Marinko Markić

Polymers 2024, 16(7), 934; https://doi.org/10.3390/polym16070934 - 29 Mar 2024

Viewed by 916

Abstract

In the process of paper recycling, certain amounts of metals can be found in the cellulose suspension, the source of which is mainly printing inks. The paper industry often uses different technologies to reduce heavy metal emissions. The recycling of laminated packaging contributes to the formation of sticky particles, which affects the concentration of heavy metals. This study aimed to determine the mass fraction of metals in the different phases of the deinking process to optimize the cellulose pulp’s quality and design healthy correct packaging products. In this research, the deinking flotation of laminated and non-laminated samples was carried out by the Ingede 11 method. As a result of the study, the mass fractions of metals in cellulose pulp were divided into four groups according to the mass fraction’s increasing value and the metals’ increasing electronegativity. The quantities of metals were analyzed using Inductively Coupled Mass Spectrometry (ICP-MS). The separation of metals from cellulose pulp is influenced by the presence of adhesives and the electronegativity of the metal. The results of the study show that the recycling process removes certain heavy metals very well, which indicates the good recycling potential of pharmaceutical cardboard samples. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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15 pages, 4155 KiB

Open AccessArticle

Electrical Conduction Mechanisms in Ethyl Cellulose Films under DC and AC Electric Fields

by Jesús G. Puente-Córdova, Juan F. Luna-Martínez, Nasser Mohamed-Noriega and Isaac Y. Miranda-Valdez

Polymers 2024, 16(5), 628; https://doi.org/10.3390/polym16050628 - 26 Feb 2024

Cited by 1 | Viewed by 740

Abstract

This work reports the dielectric behavior of the biopolymer ethyl cellulose (EC) observed from transient currents experiments under the action of a direct current (DC) electric field (~10⁷ V/m) under vacuum conditions. The viscoelastic response of the EC was evaluated using dynamic mechanical analysis (DMA), observing a mechanical relaxation related to glass transition of around ~402 K. Furthermore, we propose a mathematical framework that describes the transient current in EC using a fractional differential equation, whose solution involves the Mittag–Leffler function. The fractional order, between 0 and 1, is related to the energy dissipation rate and the molecular mobility of the polymer. Subsequently, the conduction mechanisms are considered, on the one hand, the phenomena that occur through the polymer–electrode interface and, on the other hand, those which manifest themselves in the bulk material. Finally, alternating current (AC) conductivity measurements above the glass transition temperature (~402 K) and in a frequency domain from 20 Hz to 2 MHz were carried out, observing electrical conduction described by the segmental movements of the polymeric chains. Its electrical properties also position EC as a potential candidate for electrical, electronics, and mechatronics applications. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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15 pages, 3659 KiB

Open AccessArticle

Low-Frequency Ultrasound Effects on Cellulose Nanocrystals for Potential Application in Stabilizing Pickering Emulsions

by Louise Perrin, Stephane Desobry, Guillaume Gillet and Sylvie Desobry-Banon

Polymers 2023, 15(22), 4371; https://doi.org/10.3390/polym15224371 - 10 Nov 2023

Viewed by 995

Abstract

Cellulose, in the form of cellulose nanocrystals (CNCs), is a promising biomaterial for stabilizing Pickering emulsions (PEs). PEs are commonly formed using low-frequency ultrasound (LFU) treatment and impact CNC properties. The present study investigated the specific effects of LFU treatment on CNCs’ chemical and physical properties. CNCs were characterized using dynamic light scattering, ζ;-potential determination, Fourier transform infrared spectroscopy, X-ray diffraction, and contact angle measurement. CNC suspensions were studied using rheological analysis and static multiple light scattering. LFU treatment broke CNC aggregates and modified the rheological behavior of CNC suspensions but did not affect the CNCs’ chemical or crystallographic structures, surface charge, or hydrophilic properties. During the storage of CNC suspensions and PEs, liquid crystal formation was observed with cross-polarized light. Hypotheses related to the impact of liquid crystal CNCs on PE stability were proposed. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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16 pages, 8600 KiB

Open AccessArticle

Superhydrophobic, Magnetic Aerogels Based on Nanocellulose Fibers Derived from Harakeke for Oily Wastewater Remediation

by Yitong Zhai and Xiaowen Yuan

Polymers 2023, 15(19), 3941; https://doi.org/10.3390/polym15193941 - 29 Sep 2023

Cited by 1 | Viewed by 1014

Abstract

Cellulose-based aerogels have been seen as a promising sorbent for oil and organic pollutant cleaning; however, their intrinsic hydrophilicity and difficulty of recycling has hindered their practical application. In this work, a superhydrophobic, magnetic cellulose-based aerogel was fabricated as a highly efficient sorbent for the adsorption of oils and organic solvents. The aerogel was prepared via a simple freeze-drying method, followed by chemical vapor deposition (CVD). The incorporation of Fe₃O₄ nanoparticles into the aerogel not only makes it responsive to external magnetic field, but also contributes to the better hydrophobicity of the aerogel, in which the water contact angle (WCA) was about 20° higher than the aerogel without loading with Fe₃O₄ nanoparticles. The adsorption test showed that the resultant aerogel can selectively adsorb a wide range of oils and organic solvents from oil/water mixtures with a high adsorption capacity (up to 113.49 g/g for silicone oil). It can retain about 50% of its adsorption capacity even after 10 adsorption–squeezing cycles, which indicates its outstanding reusability. Moreover, the aerogels can be easily controlled by an external magnet, which is preferred for the adsorption of oily contaminants in harsh environments and enhanced the recyclability of the aerogel. We believe that this study provides a green and convenient approach for the practical fabrication of cellulose-based oil sorbents. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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13 pages, 2774 KiB

Open AccessArticle

The Evaluation of Cellulose Acetate Capsules Functionalized for the Removal of Cd(II)

by Irma Pérez-Silva, Gladis D. Canales-Feliciano, José A. Rodríguez, Luis H. Mendoza-Huizar, Salvador Pérez-Estrada, Israel S. Ibarra and M. Elena Páez-Hernández

Polymers 2023, 15(19), 3917; https://doi.org/10.3390/polym15193917 - 28 Sep 2023

Viewed by 794

Abstract

Cellulose acetate is derived from cellulose and has the characteristics of biodegradability and reusability. So, it has been used for the elimination of toxic compounds capable of producing different diseases, such as cadmium, that result from human and industrial activity. For this reason, capsules functionalized with Cyanex 923 were prepared and characterized by FTIR spectroscopy, Energy Dispersive X-ray Spectroscopy (EDX), and SEM. The functionalized capsules were used for removing and recovering Cd(II) by modifying variables such as HCl concentration in the extraction medium and carrier content in the capsules, among others. The extraction of cadmium from battery leachates and the three isotherm models, Langmuir, Freundlich, and Dubinin Radushkevich, were also tested to model the cadmium removal process. The results showed a favorable physical sorption with a good capacity for extraction and the possibility of reusing the capsules for up to seven cycles without a decrease in the percentage of cadmium recovery. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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16 pages, 6181 KiB

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Lithium Iron Phosphate/Carbon (LFP/C) Composite Using Nanocellulose as a Reducing Agent and Carbon Source

by Macarena Kroff, Samuel A. Hevia, James N. O’Shea, Izaskun Gil de Muro, Verónica Palomares, Teófilo Rojo and Rodrigo del Río

Polymers 2023, 15(12), 2628; https://doi.org/10.3390/polym15122628 - 9 Jun 2023

Cited by 1 | Viewed by 2357

Abstract

Lithium iron phosphate (LiFePO₄, LFP) is the most promising cathode material for use in safe electric vehicles (EVs), due to its long cycle stability, low cost, and low toxicity, but it suffers from low conductivity and ion diffusion. In this work, we present a simple method to obtain LFP/carbon (LFP/C) composites with different types of NC: cellulose nanocrystal (CNC) and cellulose nanofiber (CNF). Microwave-assisted hydrothermal synthesis was used to obtain LFP with nanocellulose inside the vessel, and the final LFP/C composite was achieved by heating the mixture under a N₂ atmosphere. The resulting LFP/C indicated that the NC in the reaction medium not only acts as the reducing agent that aqueous iron solutions need (avoiding the use of other chemicals), but also as a stabiliser of the nanoparticles produced in the hydrothermal synthesis, obtaining fewer agglomerated particles compared to synthesis without NC. The sample with the best coating—and, therefore, the best electrochemical response—was the sample with 12.6% carbon derived from CNF in the composite instead of CNC, due to its homogeneous coating. The utilisation of CNF in the reaction medium could be a promising method to obtain LFP/C in a simple, rapid, and low-cost way, avoiding the waste of unnecessary chemicals. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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16 pages, 8271 KiB

Open AccessArticle

Bacterial Nanocellulose from Komagataeibacter Medellinensis in Fique Juice for Activated Carbons Production and Its Application for Supercapacitor Electrodes

by Juliana Villarreal-Rueda, Zulamita Zapata-Benabithe, Laia Posada, Estefanía Martínez, Sara Herrera, Stiven López, Ana B. J. Sobrido and Cristina I. Castro

Polymers 2023, 15(7), 1760; https://doi.org/10.3390/polym15071760 - 1 Apr 2023

Viewed by 1394

Abstract

This paper presents the results obtained from the chemical activation of bacterial nanocellulose (BCN) using fique juice as a culture medium. BNC activation (BNCA) was carried out with H₃PO₄ and KOH at activation temperatures between 500 °C to 800 °C. The materials obtained were characterized morphologically, physicochemically, superficially, and electrochemically, using scanning electron microscopy, X-ray photoelectron spectroscopy (XPS), the physisorption of gases N₂ and CO₂ at 77 K and 273 K, respectively, cyclic voltammetry, chronopotentiometry, and electrochemical impedance spectroscopy (EIS). The samples activated with H₃PO₄ presented specific surface areas (S_BET) around 780 m² g⁻¹, while those activated with KOH values presented specific surface areas between 680 and 893 m² g⁻¹. The XPS analysis showed that the P_XPS percentage on the surface after H₃PO₄ activation was 11 wt%. The energy storage capacitance values ranged between 97.5 F g⁻¹ and 220 F g⁻¹ by EIS in 1 M H₂SO₄. The samples with the best electrochemical performance were activated with KOH at 700 °C and 800 °C, mainly due to the high S_BET available and the accessibility of the microporosity. The capacitance of BNCAs was mainly improved by electrostatic effects due to the S_BET rather than that of pseudocapacitive ones due to the presence of phosphorus heteroatoms. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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14 pages, 2143 KiB

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Aryloxy Ionic Liquid-Catalyzed Homogenous Esterification of Cellulose with Low-Reactive Acyl Donors

by Akina Yoshizawa, Chie Maruyama, Samuel Budi Wardhana Kusuma, Naoki Wada, Kosuke Kuroda, Daisuke Hirose and Kenji Takahashi

Polymers 2023, 15(2), 419; https://doi.org/10.3390/polym15020419 - 13 Jan 2023

Cited by 3 | Viewed by 2389

Abstract

Ionic liquids (ILs) are recyclable, non-volatile, and can dissolve cellulose, a natural polymer that is insoluble in versatile solvents. Therefore, ILs have been used to modify cellulose. However, 1-ethyl-3-methylimidazolium acetate (EmimOAc), a commercially available IL often used to dissolve and modify cellulose to prepare cellulose-based materials, causes the undesired introduction of an acetyl group derived from the acetate anion of EmimOAc onto the hydroxy group of cellulose during esterification. In this study, for cellulose esterification, we prepared aryloxy ILs as non-carboxylate-type and basic ILs, which can theoretically prevent the undesired introduction of an acyl group from the IL onto the hydroxy group of cellulose. The optimized 1-ethyl-3-methylimidazolium 2-pyridinolate (Emim2OPy) and mixed solvent system achieved rapid cellulose esterification (within 30 min) with an excellent degree of substitution (DS) value (up to >2.9) derived from the employed low-reactive vinyl esters and bio-based unsaturated aldehydes, without any undesired substituent introduction from side reactions. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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13 pages, 2388 KiB

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Room-Temperature Cholesteric Liquid Crystals of Cellulose Derivatives with Visible Reflection

by Yuki Ogiwara, Tatsuya Suzuki, Naoto Iwata and Seiichi Furumi

Polymers 2023, 15(1), 168; https://doi.org/10.3390/polym15010168 - 29 Dec 2022

Cited by 3 | Viewed by 1567

Abstract

Hydroxypropyl cellulose (HPC) derivatives with alkanoyl side chains have attracted attention as bio-based cholesteric liquid crystal (CLC) materials with reflection colors. By taking advantage of the ability to change the reflection color in response to external stimuli, the thermotropic CLCs can be applied to a wide variety of photonic devices for a sustainable society of future generations. However, the thermotropic CLCs of HPC derivatives substituted with only one kind of alkanoyl group are not suitable for such applications because they do not exhibit visible reflection at room temperature. In this report, we describe a promising strategy to control the reflection colors of HPC derivatives at room temperature by introducing two kinds of alkanoyl groups with different lengths into the side chains of HPCs, which also enables the fine control of temperature dependence on the reflection wavelength. By chemically optimizing the side chain, we successfully prepared room-temperature thermotropic CLCs of HPC derivatives with visible reflection. This report would contribute toward the development of versatile photonic applications by CLCs produced from biomass. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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18 pages, 2890 KiB

Open AccessArticle

Stiffness-Controlled Hydrogels for 3D Cell Culture Models

by Arto Merivaara, Elle Koivunotko, Kalle Manninen, Tuomas Kaseva, Julia Monola, Eero Salli, Raili Koivuniemi, Sauli Savolainen, Sami Valkonen and Marjo Yliperttula

Polymers 2022, 14(24), 5530; https://doi.org/10.3390/polym14245530 - 17 Dec 2022

Cited by 7 | Viewed by 2964

Abstract

Nanofibrillated cellulose (NFC) hydrogel is a versatile biomaterial suitable, for example, for three-dimensional (3D) cell spheroid culturing, drug delivery, and wound treatment. By freeze-drying NFC hydrogel, highly porous NFC structures can be manufactured. We freeze-dried NFC hydrogel and subsequently reconstituted the samples into a variety of concentrations of NFC fibers, which resulted in different stiffness of the material, i.e., different mechanical cues. After the successful freeze-drying and reconstitution, we showed that freeze-dried NFC hydrogel can be used for one-step 3D cell spheroid culturing of primary mesenchymal stem/stromal cells, prostate cancer cells (PC3), and hepatocellular carcinoma cells (HepG2). No difference was observed in the viability or morphology between the 3D cell spheroids cultured in the freeze-dried and reconstituted NFC hydrogel and fresh NFC hydrogel. Furthermore, the 3D cultured spheroids showed stable metabolic activity and nearly 100% viability. Finally, we applied a convolutional neural network (CNN)-based automatic nuclei segmentation approach to automatically segment individual cells of 3D cultured PC3 and HepG2 spheroids. These results provide an application to culture 3D cell spheroids more readily with the NFC hydrogel and a step towards automatization of 3D cell culturing and analysis. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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17 pages, 3345 KiB

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Conformation and Structure of Hydroxyethyl Cellulose Ether with a Wide Range of Average Molar Masses in Aqueous Solutions

by Misato Yoshida, Hiroki Iwase and Toshiyuki Shikata

Polymers 2022, 14(21), 4532; https://doi.org/10.3390/polym14214532 - 26 Oct 2022

Cited by 3 | Viewed by 2676

Abstract

The solution properties of a water-soluble chemically modified cellulose ether, hydroxyethyl cellulose (HeC), were examined using static light scattering (SLS), dynamic light scattering (DLS), small-to-wide-angle neutron scattering (S-WANS), small-to-wide-angle X-ray scattering (S-WAXS) and viscometric techniques at 25 °C. The examined HeC samples had average molar substitution numbers ranging from 2.36 to 2.41 and weight average molar masses (M_w) that fell within a wide range from 87 to 1500 kg mol⁻¹. Although the relationship between the determined radius of gyration (R_g) and M_w was described as R_g ∝ M_w^~0.6, as is observed usually in flexible polymer solutions in good solvents, the observed scattering vector (q) dependencies of excess Rayleigh ratios were well interpreted using a rigid rod particle model, even in high-M_w samples. Moreover, the ratios of the formed particle length (L) evaluated assuming the model for rigid rods to the determined R_g showed the relationship LR_g⁻¹ ~ 3.5 irrespective of M_w and were close to those theoretically predicted for rigid rod particle systems, i.e., LR_g⁻¹ =

\sqrt{12}

. The observed SLS behavior suggested that HeC molecules behave just like rigid rods in aqueous solution. As the L values were not simply proportional to the average molecular contour length calculated from the M_w, the chain conformation or structure of the formed particles by HeC molecules in aqueous solution changed with increasing M_w. The q dependencies of excess scattering intensities observed using the S-WANS and S-WAXS experiments demonstrated that HeC molecules with M_w less than 200 kg mol⁻¹ have a diameter of ~1.4 nm and possess an extended rigid rod-like local structure, the size of which increases gradually with increasing M_w. The observed M_w dependencies of the translational and rotational diffusion coefficients and the intrinsic viscosity of the particle suspensions strongly support the idea that the HeC molecules behave as rigid rod particles irrespective of their M_w. Full article

(This article belongs to the Special Issue Advanced Preparation and Application of Cellulose)

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