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The modification of chitosan represents a challenging task in obtaining biopolymeric materials with enhanced removal capacity for heavy metals. In the present work, the adsorption characteristics of chitosan modified with carboxyl groups (CTS-CAA) towards copper (II) and zinc (II) ions have been tested. The efficacy of the synthesis of CTS-CAA has been evaluated by studying various properties of the modified chitosan. Specifically, the functionalized chitosan has been characterized by using several techniques, including thermal analyses (differential scanning calorimetry and thermogravimetry), spectroscopies (FT-IR, XRD), elemental analysis, and scanning electron microscopy. The kinetics and the adsorption isotherms of CTS-CAA towards both Cu (II) and Zn (II) have been determined in the aqueous solvent under variable pH. The obtained results have been analyzed by using different adsorption models. In addition, the experiments have been conducted at variable temperatures to explore the thermodynamics of the adsorption process. The regeneration of CTS-CAA has been investigated by studying the desorption process using different eluents. This paper reports an efficient protocol to synthesize chitosan-based material perspective as regenerative adsorbents for heavy metals.

Chitosan is one of the most studied cationic polysaccharides. Due to its unique characteristics of being water soluble, biocompatible, biodegradable, and non-toxic, this macromolecule is highly attractive for a broad range of applications. In addition, its complex behavior and the number of ways it interacts with different components in a system result in an astonishing variety of chitosan-based materials. Herein, we present recent advances in the field of chitosan-based materials from a physico-chemical perspective, with focus on aqueous mixtures with oppositely charged colloids, chitosan-based thin films, and nanocomposite systems. In this review, we focus our attention on the physico-chemical properties of chitosan-based materials, including solubility, mechanical resistance, barrier properties, and thermal behaviour, and provide a link to the chemical peculiarities of chitosan, such as its intrinsic low solubility, high rigidity, large charge separation, and strong tendency to form intra- and inter-molecular hydrogen bonds.

A new adsorbent, sulfated crosslinked chitosan (SGCH), has been synthesized for the effective extraction of beryllium ions from their aqueous solutions. In recent times, beryllium extraction has been of great importance because beryllium can be used in many applications such as in nuclear reactor, heat shields, high-technology ceramics, alloys and electronic heat sinks. SGCH has been synthesized by two successive phases. The first is the conversion of chitosan (CH) into non-soluble cross-linked chitosan (GCH) through the interaction between chitosan and glutaraldehyde. The second step is the formation of functional sulfonate groups onto the adsorbent material through the interaction of GCH with chlorosulfonic acid (sulfating agent). The role played by the sulfonate groups in the adsorption process was analyzed using FT-IR and SEM. Also, the role played by the solution pH, time, beryllium concentration and temperature on the batch adsorption process was investigated. Our results point to the successful preparation of SGCH adsorbent with high affinity for beryllium ions. The maximum sorption values of beryllium ions on the investigated biosorbent is 40.6 mg/g. The desorption of the loaded beryllium ions from the SGCH was achieved by using 1.5 M urea acidified by 0.6 M H 2 SO 4 ., (Copyright © 2019 Elsevier B.V. All rights reserved.)

The effect of the preparation protocol of chitosan (CHI) based films filled with wax microparticles stabilized by halloysite nanotubes (HNTs) in Pickering emulsions (PE) is investigated. The obtained results show that the addition of acetic acid (before or after the preparation of wax/HNT microspheres) affects the properties of the composite films as well as the colloidal stability of PE. The colloidal behavior of CHI/HNT/wax PE by optical microscopy and sedimentation tests are studied. On the other hand, the corresponding composite films (prepared by solvent casting method) are characterized through several techniques, including Scanning Electron Microscopy, UV–vis spectrometer, water permeability, and contact angle measurements. Dynamic Mechanical Analysis allows this to estimate the effect of wax microparticles on the tensile performances of CHI‐based films. As a general consideration, the filling of the CHI matrix with wax/HNT improves the physicochemical properties of the films. Finally, the efficacy of the films as adsorbents of n‐dodecane vapors is explored. Due to the presence of hydrophobic domains (wax embedded in CHI), the composite films possess higher adsorption efficiencies compared to pristine CHI. Accordingly, it can be stated that the combination of CHI with wax/HNT microparticles is promising to obtain biocompatible composite films useful for remediation purposes. [ABSTRACT FROM AUTHOR]

In the last two decades, the naturally occurring polysaccharides have gained great attention because of their potential applications in different sectors, for example, from food to biomedical sectors. Chitosan is a cationic polysaccharide with good transparency, and currently, it has been considered also as suitable material for the formulation film and coating in cultural heritage protection. In this work, the chitosan films (Ch), with and without natural antioxidant such as citric acid (CA), are formulated considering two different processing techniques: (i) conventional solvent casting and (ii) compression molding, that is an unconventional method for this polysaccharide, giving the possibility to formulate films with extended surface and constant thickness. The effects of processing conditions and antioxidant presence on the properties and performance are evaluated by thermo‐gravimetric analysis, FTIR and UV–visible spectroscopy, water contact angle measurements and tensile test. Besides, the durability of all investigated Ch and Ch/CA has been evaluated subjecting thin film to UVB exposure and monitoring their structural changes by FTIR analysis in time. All obtained results suggest that the chitosan films can be processed successfully by both solvent casting and compression molding techniques. Further, the CA presence in Ch films has a beneficial effect on the thermal resistance and durability and no negative effect on the transparency and optical properties. [ABSTRACT FROM AUTHOR]

This work is a contribution to the design of multilayer biocomposites based on halloysite nanotubes (HNTs) and chitosan. Both the polymer and nanotubular inorganic additive have been selected among easily available green materials. An innovative preparation procedure based on the sequential casting of chitosan and HNTs has been proposed in order to obtain multilayer composite biofilms. A physico-chemical investigation (contact angle measurements, differential scanning calorimetry, thermogravimetry) has been conducted to characterize the bionanocomposites. As evidenced by scanning electron microscopy, the nanocomposites possess an intermediate halloysite layer between the chitosan ones. The multilayer morphology of the prepared chitosan/HNT nanocomposites has been confirmed by water contact angle measurements, which revealed that the hybrid films present a hydrophobic surface. The peculiar sandwich-like morphology of the chitosan/HNT hybrid materials has been correlated to their thermal behavior under inert and oxidative atmospheres. The kinetic aspects of chitosan degradation have been studied by a non-isothermal thermogravimetric approach (Friedman's method), while the suitability of HNTs as flame retardant fillers of multilayer nanocomposites has been estimated by the thermodynamic parameters of oxidative degradation. According to the thermogravimetric data, the formation of a well-compacted middle layer of HNTs has induced a reliable decrease in the activation energy of the degradation of chitosan. Differential scanning calorimetry experiments showed that the nanocomposites possess an enhanced ignition temperature compared with pure chitosan. This paper opens new sustainable prospects for the preparation of novel nanocomposites with layered structures that can be strategic for packaging, tissue engineering, and pharmaceutical applications. [ABSTRACT FROM AUTHOR]

In the last two decades, the naturally occurring polysaccharides, such as chitosan and pectin, have gained great attention having potential applications in different sectors, from biomedical to new generation packaging. Currently, the chitosan and pectic have been proposed as suitable materials also for the formulation of films and coatings for cultural heritage protection, as well as packaging films. Therefore, the formulation of biopolymer films, considering only naturally occurring polymers and additives, is a current challenging trend. This work reports on the formulation of chitosan (CS), pectin (PC), and chitosan:pectin (CS:PC) films, also containing natural crosslinking and reinforcement agents, such as citric acid (CA) and halloysite nanotubes (HNT), through the solvent casting technique. The produced films are characterized through water contact angle measurements, infrared and UV–visible spectroscopy and tensile test, while the durability of the CS:PC films is evaluated subjecting the film to accelerated UVB exposure and monitoring the photo-oxidation degradation in time though infrared spectroscopy. All obtained results suggest that both crosslinking and reinforcement agents have beneficial effects on the wettability, rigidity, and photo-oxidation resistance of biopolymer films. Therefore, these biopolymer films, also containing naturally occurring additives, have good properties and performance and they are suitable as coverage films for cultural heritage protection. [ABSTRACT FROM AUTHOR]

In the last decade, the interest toward the formulation of polymer films for cultural heritage protection continuously grew, and these films must be imperatively transparent, removable, and should not react/interact with surface of the artworks. In this research, bionanocomposite films, based on chitosan (Ch) and pectin (P) and containing naturally occurring fillers and antioxidants, were formulated by solvent casting methods and were accurately characterized. The natural halloysite nanotubes (HNT) have a two-fold role, specifically, physical compatibilizer and antioxidant carrier. Therefore, the theoretical solubility between Ch and P was estimated considering Hoy's method for solubility of polymers, while the optimum ratio between biopolymer constituents was assessed by ζ-potential measurements. The transparency, wettability, and mechanical behavior of Ch:P films, also in presence of HNT without and with antioxidants, were investigated. The beneficial effects of natural antioxidants, such as vanillic acid (VA) and quercetin (Q), on Ch:P/HNT durability were found. [ABSTRACT FROM AUTHOR]

In this work, we have developed a novel strategy to prepare hybrid nanostructures with controlled release properties towards khellin by exploiting the electrostatic interactions between chitosan and halloysite nanotubes (HNT). Firstly, khellin was loaded into the HNT lumen by the vacuum-assisted procedure. The drug confinement within the halloysite cavity has been proved by water contact angle experiments on the HNT/khellin tablets. Therefore, the loaded nanotubes were coated with chitosan as a consequence of the attractions between the cationic biopolymer and the halloysite outer surface, which is negatively charged in a wide pH range. The effect of the ionic strength of the aqueous medium on the coating efficiency of the clay nanotubes was investigated. The surface charge properties of HNT/khellin and chitosan/HNT/khellin nanomaterials were determined by ζ potential experiments, while their morphology was explored through Scanning Electron Microscopy (SEM). Water contact angle experiments were conducted to explore the influence of the chitosan coating on the hydrophilic/hydrophobic character of halloysite external surface. Thermogravimetry (TG) experiments were conducted to study the thermal behavior of the composite nanomaterials. The amounts of loaded khellin and coated chitosan in the hybrid nanostructures were estimated by a quantitative analysis of the TG curves. The release kinetics of khellin were studied in aqueous solvents at different pH conditions (acidic, neutral and basic) and the obtained data were analyzed by the Korsmeyer–Peppas model. The release properties were interpreted on the basis of the TG and ζ potential results. In conclusion, this study demonstrates that halloysite nanotubes wrapped by chitosan layers can be effective as drug delivery systems. [ABSTRACT FROM AUTHOR]

The use of nanocomposites based on biopolymers and nanoparticles for controlled drug release is an attractive notion. We used halloysite nanotubes that were promising candidates for the loading and release of active molecules due to their hollow cavity. Gel beads based on chitosan with uniformly dispersed halloysite nanotubes were obtained by a dropping method. Alginate was used to generate a coating layer over the hybrid gel beads. This proposed procedure succeeded in controlling the morphology at the mesoscale and it had a relevant effect on the release profile of the model drug from the nanotube cavity. [ABSTRACT FROM AUTHOR]