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Volume 12, January

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Polymers, Volume 12, Issue 2 (February 2020) – 238 articles

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Cover Story (view full-size image) The thermophoretic response of a protein is sensitive to ligand binding, provides access to [...] Read more.
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Open AccessArticle
Dynamic Compression Induced Solidification
Polymers 2020, 12(2), 488; https://doi.org/10.3390/polym12020488 (registering DOI) - 22 Feb 2020
Abstract
This study presents a method for the determination of the dynamic pressure-dependent solidification of polycarbonate (PC) during flow using high pressure capillary rheometer (HPC) measurements. In addition, the pressure-dependent solidification was determined by isothermal pressure-volume-temperature (pvT) measurements under static conditions without shear. Independent [...] Read more.
This study presents a method for the determination of the dynamic pressure-dependent solidification of polycarbonate (PC) during flow using high pressure capillary rheometer (HPC) measurements. In addition, the pressure-dependent solidification was determined by isothermal pressure-volume-temperature (pvT) measurements under static conditions without shear. Independent of the compression velocity, a linear increase of the solidification pressure with temperature could be determined. Furthermore, the results indicate that the relaxation time at a constant temperature and compression rate can increase to such an extent that the material can no longer follow within the time scale specified by the compression rate. Consequently, the flow through the capillary stops at a specific pressure, with higher compression rates resulting in lower solidification pressures. Consequently, in regard to HPC measurements, it could be shown that the evaluation of the pressure via a pressure hole can lead to measurement errors in the limit range. Since the filling process in injection molding usually takes place under such transient conditions, the results are likely to be relevant for modelling the flow processes of thin-walled and microstructures with high aspect ratios. Full article
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Open AccessArticle
Doubly Dynamic Hydrogel Formed by Combining Boronate Ester and Acylhydrazone Bonds
Polymers 2020, 12(2), 487; https://doi.org/10.3390/polym12020487 (registering DOI) - 21 Feb 2020
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Abstract
The incorporation of double dynamic bonds into hydrogels provides an effective strategy to engineer their performance on demand. Herein, novel hydrogels were PREPARED by combining two kinetically distinct dynamic covalent bonds, boronate ester and acylhydrazone bonds, and the synergistic properties of the hydrogels [...] Read more.
The incorporation of double dynamic bonds into hydrogels provides an effective strategy to engineer their performance on demand. Herein, novel hydrogels were PREPARED by combining two kinetically distinct dynamic covalent bonds, boronate ester and acylhydrazone bonds, and the synergistic properties of the hydrogels were studied comprehensively. The functional diblock copolymers P(N-isopropyl acrylamide-co-N-acryloyl-3-aminophenylboronic acid)-b-(N-isopropyl acrylamide-co-diacetone acrylamide) (PAD) were prepared via reversible addition−fragmentation chain transfer (RAFT) polymerization. The hydrogel was constructed by exploiting dynamic reaction of phenyboronic acid moieties with polyvinyl alcohol (PVA) and ketone moieties with adipic dihydrazide (ADH) without any catalyst. The active boronate ester linkage endows the hydrogel with fast gelation kinetics and self-healing ability, and the stable acylhydrazone linkage can enhance the mechanical property of the hydrogel. The difference in kinetics endows that the contribution of each linkage to mechanical strength of the hydrogel can be accurately estimated. Moreover, the mechanical property of the hydrogel can be readily engineered by changing the composition and solid content, as well as by controlling the formation or dissociation of the dynamic linkages. Thus, we provide a promising strategy to design and prepare multi-responsive hydrogels with tunable properties. Full article
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Temperature and pH-Dependent Response of Poly(Acrylic Acid) and Poly(Acrylic Acid-co-Methyl Acrylate) in Highly Concentrated Potassium Chloride Aqueous Solutions
Polymers 2020, 12(2), 486; https://doi.org/10.3390/polym12020486 (registering DOI) - 21 Feb 2020
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Abstract
In this study, the phase transition phenomena of linear poly(acrylic acid) (PAA) and linear or star-shaped poly(acrylic acid-co-methyl acrylate) (P(AA-co-MA)) in highly concentrated KCl solutions were investigated. The effects of polymer molecular weight, topology, and composition on their phase [...] Read more.
In this study, the phase transition phenomena of linear poly(acrylic acid) (PAA) and linear or star-shaped poly(acrylic acid-co-methyl acrylate) (P(AA-co-MA)) in highly concentrated KCl solutions were investigated. The effects of polymer molecular weight, topology, and composition on their phase transition behavior in solution were investigated. The cloud point temperature (TCP) of polymers drastically increased as the KCl concentration (CKCl) and solution pH increased. CKCl strongly influenced the temperature range at which the phase transition of PAA occurred: CKCl of 1.0–2.2 M allowed the phase transition to occur between 30 and 75 °C. Unfortunately, at CKCl above 2.6 M, the TCP of PAA was too high to theoretically trigger the crystallization of KCl. The addition of hydrophobic methyl acrylate moieties decreased the TCP into a temperature region where KCl crystallization could occur. Additionally, the hydrodynamic diameters (Dh) and zeta potentials of commercial PAA samples were examined at room temperature and at their TCP using dynamic light scattering. The salt concentration (from 1 to 3 M) did not impact the hydrodynamic diameter of the molecules. Dh values were 1500 and 15 nm at room temperature and at TCP, respectively. Full article
(This article belongs to the Section Polymer Processing and Performance)
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Open AccessArticle
Structural Changes of Oak Wood Main Components Caused by Thermal Modification
Polymers 2020, 12(2), 485; https://doi.org/10.3390/polym12020485 (registering DOI) - 21 Feb 2020
Viewed by 79
Abstract
Thermal modification of wood causes chemical changes that significantly affect the physical, mechanical and biological properties of wood; thus, it is essential to investigate these changes for better utilization of products. Fourier transform infrared spectroscopy and size exclusion chromatography were used for evaluation [...] Read more.
Thermal modification of wood causes chemical changes that significantly affect the physical, mechanical and biological properties of wood; thus, it is essential to investigate these changes for better utilization of products. Fourier transform infrared spectroscopy and size exclusion chromatography were used for evaluation of chemical changes at thermal treatment of oak wood. Thermal modification was applied according to Thermowood process at the temperatures of 160, 180 and 210 °C, respectively. The results showed that hemicelluloses are less thermally stable than cellulose. Chains of polysaccharides split to shorter ones leading to a decrease of the degree of polymerization and an increase of polydispersity. At the highest temperature of the treatment (210 °C), also crosslinking reactions take place. At lower temperatures degradation reactions of lignin predominate, higher temperatures cause mainly condensation reactions and a molecular weight increase. Chemical changes in main components of thermally modified wood mainly affect its mechanical properties, which should be considered into account especially when designing various timber constructions. Full article
(This article belongs to the Special Issue Degradation of Wood-Based Materials)
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Open AccessArticle
Drying of the Natural Fibers as A Solvent-Free Way to Improve the Cellulose-Filled Polymer Composite Performance
Polymers 2020, 12(2), 484; https://doi.org/10.3390/polym12020484 (registering DOI) - 21 Feb 2020
Viewed by 81
Abstract
When considering cellulose (UFC100) modification, most of the processes employ various solvents in the role of the reaction environment. The following article addresses a solvent-free method, thermal drying, which causes a moisture content decrease in cellulose fibers. Herein, the moisture content in UFC100 [...] Read more.
When considering cellulose (UFC100) modification, most of the processes employ various solvents in the role of the reaction environment. The following article addresses a solvent-free method, thermal drying, which causes a moisture content decrease in cellulose fibers. Herein, the moisture content in UFC100 was analyzed with spectroscopic methods, thermogravimetric analysis, and differential scanning calorimetry. During water desorption, a moisture content drop from approximately 6% to 1% was evidenced. Moreover, drying may bring about a specific variation in cellulose’s chemical structure. These changes affected the cellulose-filled polymer composite’s properties, e.g., an increase in tensile strength from 17 MPa for the not-dried UFC100 to approximately 30 MPa (dried cellulose; 24 h, 100 °C) was observed. Furthermore, the obtained tensile test results were in good correspondence with Payne effect values, which changed from 0.82 MPa (not-dried UFC100) to 1.21 MPa (dried fibers). This raise proves the reinforcing nature of dried UFC100, as the Payne effect is dependent on the filler structure’s development within a polymer matrix. This finding paves new opportunities for natural fiber applications in polymer composites by enabling a solvent-free and efficient cellulose modification approach that fulfils the sustainable development rules. Full article
(This article belongs to the Special Issue Cellulose and Renewable Materials)
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Open AccessArticle
Effect of PEW and CS on the Thermal, Mechanical, and Shape Memory Properties of UHMWPE
Polymers 2020, 12(2), 483; https://doi.org/10.3390/polym12020483 (registering DOI) - 21 Feb 2020
Viewed by 68
Abstract
Modified ultra-high-molecular-weight polyethylene (UHMWPE) with calcium stearate (CS) and polyethylene wax (PEW) is a feasible method to improve the fluidity of materials because of the tense entanglement network formed by the extremely long molecular chains of UHMWPE, and a modified UHMWPE sheet was [...] Read more.
Modified ultra-high-molecular-weight polyethylene (UHMWPE) with calcium stearate (CS) and polyethylene wax (PEW) is a feasible method to improve the fluidity of materials because of the tense entanglement network formed by the extremely long molecular chains of UHMWPE, and a modified UHMWPE sheet was fabricated by compression molding technology. A Fourier-transform infrared spectroscopy test found that a new chemical bond was generated at 1097 cm−1 in the materials. Besides, further tests on the thermal, thermomechanical, mechanical, and shape memory properties of the samples were also conducted, which indicates that all properties are affected by the dimension and distribution of crystal regions. Moreover, the experimental results indicate that the addition of PEW and CS can effectively improve the mechanical properties. Additionally, the best comprehensive performance of the samples was obtained at the PEW content of 5 wt % and the CS content of 1 wt %. In addition, the effect of temperature on the shape memory properties of the samples was investigated, and the results indicate that the shape fixity ratio (Rf) and the shape recovery ratio (Rr) can reach 100% at 115 °C and 79% at 100 °C, respectively, which can contribute to the development of UHMWPE-based shape memory polymers. Full article
(This article belongs to the Special Issue Functional Polymers in Additive Manufacturing)
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Open AccessArticle
Evaluation of Carbon Dioxide-Based Urethane Acrylate Composites for Sealers of Root Canal Obturation
Polymers 2020, 12(2), 482; https://doi.org/10.3390/polym12020482 (registering DOI) - 21 Feb 2020
Viewed by 84
Abstract
A new root canal sealer was developed based on urethane acrylates using polycarbonate polyol (PCPO), a macrodiol prepared in the consumption of carbon dioxide as feedstock. The superior mechanical properties and biostability nature of PCPO-based urethane acrylates were then co-crosslinked with a difunctional [...] Read more.
A new root canal sealer was developed based on urethane acrylates using polycarbonate polyol (PCPO), a macrodiol prepared in the consumption of carbon dioxide as feedstock. The superior mechanical properties and biostability nature of PCPO-based urethane acrylates were then co-crosslinked with a difunctional monomer of tripropylene glycol diarylate (TPGDA) as sealers for resin matrix. Moreover, nanoscale silicate platelets (NSPs) immobilized with silver nanoparticles (AgNPs) and/or zinc oxide nanoparticles (ZnONPs) were introduced to enhance the antibacterial effect for the sealers. The biocompatibility and the antibacterial effect were investigated by Alamar blue assay and LDH assay. In addition, the antibacterial efficiency was performed by using Enterococcus faecalis (E. faecalis) as microbial response evaluation. These results demonstrate that the PCPO-based urethane acrylates with 50 ppm of both AgNP and ZnONP immobilized on silicate platelets, i.e., Ag/[email protected], exhibited great potential as an antibacterial composite for the sealer of root canal obturation. Full article
(This article belongs to the Special Issue Advanced Polymer Nanocomposites)
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Open AccessArticle
Analysis of Thermal–Mechanical Properties of Silicon Dioxide/Polyvinylidene Fluoride Reinforced Non-Woven Fabric (Polypropylene) Composites
Polymers 2020, 12(2), 481; https://doi.org/10.3390/polym12020481 (registering DOI) - 21 Feb 2020
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Abstract
In this paper, solution casting method is used to prepare the PP (polypropylene) non-woven fabric based composite film filled with silicon dioxide/polyvinylidene fluoride (SiO2/PVDF). The mechanical and thermodynamic properties of PP/SiO2/PVDF composites were studied by a uniaxial tensile test [...] Read more.
In this paper, solution casting method is used to prepare the PP (polypropylene) non-woven fabric based composite film filled with silicon dioxide/polyvinylidene fluoride (SiO2/PVDF). The mechanical and thermodynamic properties of PP/SiO2/PVDF composites were studied by a uniaxial tensile test under different temperature and combustion experiment. It is found that the stress of PP/SiO2/PVDF composite film with 4 wt % SiO2 is the maximum value, reaching 18.314 MPa, 244.42% higher than that of pure PP non-woven. Meanwhile, the thermal–mechanical coupling tests indicate that with the increase of temperature, the ultimate stress and strain of the composite decrease. At the same time, the thermal shrinkage property of the composite during the heating process is studied. The modified composite has good thermal stability under 180 °C. Scanning electron microscope (SEM), X-ray diffraction (XRD) and thermogravimetric (TG) were used to characterize the pore shape, distribution and crystal phase change of the composite. The modified PP/SiO2/PVDF composite film structure shows high strength and good thermal stability, and can better meet the requirements of strength and thermal performance of lithium-ion battery during the charging and discharging process. Full article
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Open AccessArticle
Optical and Nonlinear Properties of Photonic Polymer Nanocomposites and Holographic Gratings Modified with Noble Metal Nanoparticles
Polymers 2020, 12(2), 480; https://doi.org/10.3390/polym12020480 (registering DOI) - 21 Feb 2020
Viewed by 131
Abstract
Nanocomposites based on transparent polymer matrices containing nanoparticles (NPs) of noble metals are modern-day materials that can be specially designed for photonics, linear and nonlinear optics, laser physics and sensing applications. We present the improved photosensitive nanocomposites doped with Au and Ag NPs [...] Read more.
Nanocomposites based on transparent polymer matrices containing nanoparticles (NPs) of noble metals are modern-day materials that can be specially designed for photonics, linear and nonlinear optics, laser physics and sensing applications. We present the improved photosensitive nanocomposites doped with Au and Ag NPs allowing fabrication of high effective submicrometer dimensional diffraction structures using holographic method. A general approach for the fabrication of holographic structures using a two-component mixture of the monomers of different reactivity was developed. Two different methods, ex situ and in situ, were studied to introduce Au and Ag NPs in the polymer matrix. The diffusion model of the grating formation upon holographic exposure as well as the process of Ag NP synthesis in a polymer matrix is considered. The influence of the NP size on the polymerization process, material dynamic range and nonlinear properties were investigated. The mechanisms and characteristics of the nanocomposite nonlinear optical response are discussed. Full article
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Open AccessArticle
CD133 Targeted PVP/PMMA Microparticle Incorporating Levamisole for the Treatment of Ovarian Cancer
Polymers 2020, 12(2), 479; https://doi.org/10.3390/polym12020479 (registering DOI) - 20 Feb 2020
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Abstract
Levamisole (LEVA) is used to treat worm infections, but it can also inhibit cancer cell growth by inhibiting the aldehyde dehydrogenase pathway. Therefore, here, we developed a drug carrier targeting CD133, a biomarker overexpressed in ovarian cancer cells. The particle structure and cytotoxicity [...] Read more.
Levamisole (LEVA) is used to treat worm infections, but it can also inhibit cancer cell growth by inhibiting the aldehyde dehydrogenase pathway. Therefore, here, we developed a drug carrier targeting CD133, a biomarker overexpressed in ovarian cancer cells. The particle structure and cytotoxicity of the prepared LEVA-containing particles—called LEVA/PVP/PMMA microparticles (MPs) (because it used matrix material polyvinylpyrrolidone (PVP) and poly(methylmethacrylate) (PMMA))—were investigated in the ovarian cancer cell lines SKOV-3 and CP70. The particle size of the MPs was determined to be 1.0–1.5 µm and to be monodispersed. The hydrophilic property of PVP created a porous MP surface after the MPs were soaked in water for 20 min, which aided the leaching of the hydrophilic LEVA out of the MPs. The encapsulation efficiency of LEVA/PVP/PMMA MPs could reach up to 20%. Free-form LEVA released 50% of drugs in <1 h and 90% of drugs in 1 day, whereas the drug release rate of LEVA/PVP/PMMA MPs was much slower; 50% released in 4 h and only 70% of drugs released in 1 day. In the in vitro cell model test, 5 mM free-form LEVA and 0.1 g/mL CD133 targeted LEVA/PVP/PMMA MPs reduced SKOV-3 cell viability by 60%; 0.1 g/mL LEVA/PVP/PMMA MPs was equivalent to a similar dosage of the free drug. In addition, the cytotoxicity of CD133-conjugated LEVA/PVP/PMMA MPs shows a different cytotoxicity response toward cell lines. For SKOV-3 cells, treatment with free-form LEVA or CD133-conjugated LEVA/PVP/PMMA MPs exerted dose-dependent cytotoxic effects on SKOV-3 cell viability. However, CD133-conjugated LEVA/PVP/PMMA MPs demonstrated no significant dose-dependent cytotoxic efficacy toward CP70 cells. Full article
(This article belongs to the Special Issue Polymeric Colloidal Materials for Biomedical Applications)
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Open AccessArticle
Study of POSS on the Properties of Novel Inorganic Dental Composite Resin
Polymers 2020, 12(2), 478; https://doi.org/10.3390/polym12020478 (registering DOI) - 20 Feb 2020
Viewed by 122
Abstract
: Various amounts of methacryl polyhedral oligomeric silsesquioxane (POSS) were explored to be incorporated into novel nano SiO2 dental resin composites using light curing method. The scanning electron microscopy (SEM), optical microscopy, fourier transform infrared spectroscopy (FTIR), nanoindentation, nanoscratch and three-point flexure [...] Read more.
: Various amounts of methacryl polyhedral oligomeric silsesquioxane (POSS) were explored to be incorporated into novel nano SiO2 dental resin composites using light curing method. The scanning electron microscopy (SEM), optical microscopy, fourier transform infrared spectroscopy (FTIR), nanoindentation, nanoscratch and three-point flexure tests were performed. The volumetric shrinkage and mechanical properties such as hardness, elastic modulus, resistance, flexural strength and fracture energy were analyzed. With the additions of POSS, the volume shrinkage decreased and the mechanical properties initially increased. The effects of POSS on these properties were studied to provide a reference for clinically selecting a composite resin with excellent properties. Full article
(This article belongs to the Special Issue Silsesquioxane (POSS) Polymers, Copolymers and Nanoparticles)
Open AccessArticle
Quantitative Structural Analysis of Polystyrene Nanoparticles Using Synchrotron X-Ray Scattering and Dynamic Light Scattering
Polymers 2020, 12(2), 477; https://doi.org/10.3390/polym12020477 (registering DOI) - 19 Feb 2020
Viewed by 152
Abstract
A series of polystyrene nanoparticles (PS-1, PS-2, PS-3, and PS-4) in aqueous solutions were investigated in terms of morphological structure, size, and size distribution. Synchrotron small-angle X-ray scattering analysis (SAXS) was carried out, providing morphology details, size and size distribution on the particles. [...] Read more.
A series of polystyrene nanoparticles (PS-1, PS-2, PS-3, and PS-4) in aqueous solutions were investigated in terms of morphological structure, size, and size distribution. Synchrotron small-angle X-ray scattering analysis (SAXS) was carried out, providing morphology details, size and size distribution on the particles. PS-1, PS-2, and PS-3 were confirmed to behave two-phase (core and shell) spherical shapes, whereas PS-4 exhibited a single-phase spherical shape. They all revealed very narrow unimodal size distributions. The structural parameter details including radial density profile were determined. In addition, the presence of surfactant molecules and their assemblies were detected for all particle solutions, which could originate from their surfactant-assisted emulsion polymerizations. In addition, dynamic light scattering (DLS) analysis was performed, finding only meaningful hydrodynamic size and intensity-weighted mean size information on the individual PS solutions because of the particles’ spherical nature. In contrast, the size distributions were extracted unrealistically too broad, and the volume- and number-weighted mean sizes were too small, therefore inappropriate to describe the particle systems. Furthermore, the DLS analysis could not detect completely the surfactant and their assemblies present in the particle solutions. Overall, the quantitative SAXS analysis confirmed that the individual PS particle systems were successfully prepared with spherical shape in a very narrow unimodal size distribution. Full article
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Open AccessArticle
Experimental Cold-Cured Nanostructured Epoxy-Based Hybrid Formulations: Properties and Durability Performance
Polymers 2020, 12(2), 476; https://doi.org/10.3390/polym12020476 (registering DOI) - 19 Feb 2020
Viewed by 123
Abstract
Different hybrid epoxy formulations were produced and cold-cured, monitoring the properties development during low temperature curing and aging. All systems were based on silane functionalized bis-phenol A (DGEBA) resins (Part A), cured at ambient temperature with two amine hardeners (Part B). The different [...] Read more.
Different hybrid epoxy formulations were produced and cold-cured, monitoring the properties development during low temperature curing and aging. All systems were based on silane functionalized bis-phenol A (DGEBA) resins (Part A), cured at ambient temperature with two amine hardeners (Part B). The different components of the formulations were selected on their potential capability to bring about enhancements in the glass transition temperature. The durability of the produced hybrids was probed in comparison to the corresponding neat epoxies by monitoring changes in glass transition temperature (Tg) and flexural mechanical properties after exposure to different levels of humidity and immersion in water and at temperatures slightly higher than the local ambient temperature, in order to simulate the conditions encountered during summer seasons in very humid environments. The thermal degradation resistance of the hybrid systems was also evaluated by thermogravimetric analysis. Full article
(This article belongs to the Special Issue State-of-the-Art Polymer Science and Technology in Italy)
Open AccessArticle
Fabrication of Porous Recycled HDPE Biocomposites Foam: Effect of Rice Husk Filler Contents and Surface Treatments on the Mechanical Properties
Polymers 2020, 12(2), 475; https://doi.org/10.3390/polym12020475 (registering DOI) - 19 Feb 2020
Viewed by 153
Abstract
In this study, a biodegradable, cheap and durable recycled high-density polyethylene (rHDPE) polymer reinforced with rice husk (RH) fibre was fabricated into a foam structure through several processes, including extrusion, internal mixing and hot pressing. The effect of filler loading on the properties [...] Read more.
In this study, a biodegradable, cheap and durable recycled high-density polyethylene (rHDPE) polymer reinforced with rice husk (RH) fibre was fabricated into a foam structure through several processes, including extrusion, internal mixing and hot pressing. The effect of filler loading on the properties of the foam and the influence of RH surface treatments on the filler–matrix adhesion and mechanical properties of the composite foam were investigated. The morphological examination shows that 50 wt.% filler content resulted in an effective dispersion of cells with the smallest cell size (58.3 µm) and the highest density (7.62 × 1011 sel/cm3). This small cell size benefits the mechanical properties. Results indicate that the tensile strength and the Young’s modulus of the alkali-treated RH/rHDPE composite foam are the highest amongst the treatments (10.83 MPa and 858 MPa, respectively), followed by UV/O3, which has shown considerable increments compared with the untreated composite. The flexural and impact tests also show the increment in strength for the composite foam after chemical treatment. Although the UV/O3 surface treatment has minor influence on the mechanical enhancement of the composite foam, this method may be a reliable surface treatment of the fibre-reinforced composite. Full article
(This article belongs to the Special Issue Durability of Natural Fibers and Plastics)
Open AccessArticle
Improvement of Peptide Affinity and Stability by Complexing to Cyclodextrin-Grafted Ammonium Chitosan
Polymers 2020, 12(2), 474; https://doi.org/10.3390/polym12020474 (registering DOI) - 19 Feb 2020
Viewed by 133
Abstract
Cyclodextrin-grafted polymers are attractive biomaterials that could bring together the host–guest complexing capability of pristine cyclodextrin and the pharmaceutical features of the polymeric backbone. The present paper is aimed at characterizing the potential application of ammonium–chitosan grafted with 2-methyl-β-cyclodextrin (N+-rCh-MCD) as [...] Read more.
Cyclodextrin-grafted polymers are attractive biomaterials that could bring together the host–guest complexing capability of pristine cyclodextrin and the pharmaceutical features of the polymeric backbone. The present paper is aimed at characterizing the potential application of ammonium–chitosan grafted with 2-methyl-β-cyclodextrin (N+-rCh-MCD) as the functional macromolecular complexing agent for the oral administration of the neuropeptide dalargin (DAL). Specific NMR characterization procedures, along with UV and fluorescence techniques, as well as biological in vitro assessments have been performed. The results indicate that N+-rCh-MCD forms water-soluble complexes with DAL, with a prevalent involvement of Tyr or Phe over Leu and Ala residues. The association constant of DAL with the polymeric derivative is one order of magnitude higher than that with the pristine cyclodextrin (Ka: 2600 M−1 and 120 M−1, respectively). Additionally, N+-rCh-MCD shields DAL from enzymatic degradation in gastrointestinal in vitro models with a three-fold time delay, suggesting a future pharmaceutical exploitation of the polymeric derivative. Therefore, the greater affinity of N+-rCh-MCD for DAL and its protective effect against enzymatic hydrolysis can be attributed to the synergistic cooperation between cyclodextrin and the polymer, which is realized only when the former is covalently linked to the latter. Full article
(This article belongs to the Special Issue State-of-the-Art Polymer Science and Technology in Italy)
Open AccessArticle
Development of Interfacial Adhesive Property by Novel Anti-Stripping Composite between Acidic Aggregate and Asphalt
Polymers 2020, 12(2), 473; https://doi.org/10.3390/polym12020473 (registering DOI) - 19 Feb 2020
Viewed by 128
Abstract
Studies on control of and preventive measures against asphalt pavement moisture damage have important economic and social significance due to the multiple damage and repair of pavements, the reasons for which include the poor interfacial adhesive ability between acidic aggregates and asphalts. Anti-stripping [...] Read more.
Studies on control of and preventive measures against asphalt pavement moisture damage have important economic and social significance due to the multiple damage and repair of pavements, the reasons for which include the poor interfacial adhesive ability between acidic aggregates and asphalts. Anti-stripping agent is used in order to improve the poor adhesion, and decomposition temperature is regarded as being important for lots of anti-stripping products, because they always decompose and lose their abilities under the high temperature in the mixing plant before application to the pavement. A novel anti-stripping composite, montmorillonoid/Polyamide (OMMT/PAR), which possesses excellent thermal stability performance and is effective in preventing moisture damage, especially for acidic aggregates, was prepared. Moreover, the modification mechanisms and pavement properties were also investigated with reference to the composites. The results show that OMMT/PAR was prepared successfully, improving the interfacial adhesion between the acidic aggregate and the modified asphalt. Due to the nanostructure of OMMT/PAR, the thermal stability was enhanced dramatically and the interfacial adhesion properties were also improved. Furthermore, asphalts modified with OMMT/PAR and their mixtures showed excellent properties. Finally, the moisture damage process and the mechanisms by which OMMT/PAR improves the interfacial adhesion properties are explained through adhesion mechanism analyses. Full article
(This article belongs to the Special Issue Processing and Molding of Polymers)
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Comparison and Impact of Different Fiber Debond Techniques on Fiber Reinforced Flexible Composites
Polymers 2020, 12(2), 472; https://doi.org/10.3390/polym12020472 (registering DOI) - 18 Feb 2020
Viewed by 131
Abstract
The focus of this paper is the realization and verification of a modified fiber bundle pull-out test setup to estimate the adhesion properties between threads and elastic matrix materials with a more realistic failure mode than single fiber debond techniques. This testing device [...] Read more.
The focus of this paper is the realization and verification of a modified fiber bundle pull-out test setup to estimate the adhesion properties between threads and elastic matrix materials with a more realistic failure mode than single fiber debond techniques. This testing device including a modified specimen holder provides the basis for an adequate estimation of the interlaminar adhesion of fiber bundles including the opportunity of a faster, easier, and more economic handling compared to single fiber tests. The verification was done with the single-fiber and microbond test. Overall, the modified test setup showed the typical pull-out behavior, and the relative comparability between different test scales is given. Full article
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The Performance Changes and Migration Behavior of PLA/Nano-TiO2 Composite Film by High-Pressure Treatment in Ethanol Solution
Polymers 2020, 12(2), 471; https://doi.org/10.3390/polym12020471 (registering DOI) - 18 Feb 2020
Viewed by 141
Abstract
To study the relationship between performance changes and nanoparticles migration of the composite film at different migration stages, the poly (lactic acid) (PLA)/nano-TiO2 composite film treated by high pressure was immersed in 50% (v/v) ethanol solution for 45 [...] Read more.
To study the relationship between performance changes and nanoparticles migration of the composite film at different migration stages, the poly (lactic acid) (PLA)/nano-TiO2 composite film treated by high pressure was immersed in 50% (v/v) ethanol solution for 45 days at 40 °C, and the film characteristics and migration behavior were analyzed. The results showed that the migration of the composite film with the highest loading of nano-TiO2 (20 wt. %) in alcoholic food simulated solution was far less than 10 mg/kg during the 45-day migration process. Although with the increase of migration time, the micro-morphology of composite film became rougher, the crystallinity decreased and the gas permeability increased, but the internal crystal structure of the composite film remained basically unchanged. The PLA/nano-TiO2 composite films treated by high pressure treatment were relatively stable, and had good performance and migration behavior in alcoholic food simulated solution, the nanocomposite film after high pressure treatment could be used to reduce nano-TiO2 particle migration and subsequently reduce human exposure as the packaging film for the packaging of alcoholic food, which provide a theoretical basis for the applications of high pressure treatment of PLA/nano-TiO2 composite films in food packaging material and broaden its application prospects. Full article
(This article belongs to the Special Issue Advanced biodegradable Polymers and composites for Food Packaging)
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Open AccessCommunication
Role of Nanoparticle–Polymer Interactions on the Development of Double-Network Hydrogel Nanocomposites with High Mechanical Strength
Polymers 2020, 12(2), 470; https://doi.org/10.3390/polym12020470 (registering DOI) - 18 Feb 2020
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Abstract
Extensive experimental and theoretical research over the past several decades has pursued strategies to develop hydrogels with high mechanical strength. Our study investigated the effect of combining two approaches, addition of nanoparticles and crosslinking two different polymers (to create double-network hydrogels), on the [...] Read more.
Extensive experimental and theoretical research over the past several decades has pursued strategies to develop hydrogels with high mechanical strength. Our study investigated the effect of combining two approaches, addition of nanoparticles and crosslinking two different polymers (to create double-network hydrogels), on the mechanical properties of hydrogels. Our studies revealed that these orthogonal approaches may be combined to synthesize hydrogel composites with enhanced mechanical properties. However, the enhancement in double network hydrogel elastic modulus due to incorporation of nanoparticles is limited by the ability of the nanoparticles to strongly interact with the polymers in the network. Moreover, double-network hydrogel nanocomposites prepared using lower monomer concentrations showed higher enhancements in elastic moduli compared to those prepared using high monomer concentrations, thus indicating that the concentration of hydrogel monomers used for the preparation of the nanocomposites had a significant effect on the extent of nanoparticle-mediated enhancements. Collectively, these results demonstrate that the hypotheses previously developed to understand the role of nanoparticles on the mechanical properties of hydrogel nanocomposites may be extended to double-network hydrogel systems and guide the development of next-generation hydrogels with extraordinary mechanical properties through a combination of different approaches. Full article
(This article belongs to the Special Issue Reinforced Polymer Composites)
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Open AccessArticle
Influence of the Chitosan and Rosemary Extract on Fungal Biodegradation of Some Plasticized PLA-Based Materials
Polymers 2020, 12(2), 469; https://doi.org/10.3390/polym12020469 (registering DOI) - 18 Feb 2020
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Abstract
The fungal degradation of the complex polymeric systems based on poly(lactic acid) (PLA) and natural bioactive compounds (chitosan and powdered rosemary alcoholic extract) was studied. Two fungal strains, Chaetomium globosum and Phanerochaete chrysosporium were tested. Both fungi characteristics and changes in morphology, [...] Read more.
The fungal degradation of the complex polymeric systems based on poly(lactic acid) (PLA) and natural bioactive compounds (chitosan and powdered rosemary alcoholic extract) was studied. Two fungal strains, Chaetomium globosum and Phanerochaete chrysosporium were tested. Both fungi characteristics and changes in morphology, structure and thermal properties were monitored. Biochemical parameters as superoxide dismutase, catalase, soluble protein and malondialdehyde have been determined at different time periods of fungal degradation. The fungi extracellular enzyme activities are slightly decreased in the case of composites containing bioactive compounds. The presence of natural compounds in the PLA-based polymeric system determines an acceleration of fungal degradation and probably the chemical hydrolysis, which further helps the attachment of fungi on the surface of polymeric samples. Significant decreases in average molecular mass of the polymeric samples were observed by fungi action; accompanied by structural changes, increase in crystallinity and decrease of thermal properties and the loss of the physical integrity and finally to degradation and integration of fungal degradation products into environmental medium. It was found that both fungi tested are efficient for PLA-based materials degradation, the most active from them being Chaetomium globosum fungus. Full article
Open AccessArticle
Supramolecular Triblock Copolymers Through the Formation of Hydrogen Bonds: Synthesis, Characterization, Association Effects in Solvents of Different Polarity
Polymers 2020, 12(2), 468; https://doi.org/10.3390/polym12020468 (registering DOI) - 18 Feb 2020
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Abstract
Anionic polymerization techniques were employed for the synthesis of linear polystyrene (PS) and block copolymer of PS and polyisoprene (PI) PS-b-PI bearing end hydroxyl groups. Following suitable organic chemistry transformation, the –OH end groups were converted to moieties able to form [...] Read more.
Anionic polymerization techniques were employed for the synthesis of linear polystyrene (PS) and block copolymer of PS and polyisoprene (PI) PS-b-PI bearing end hydroxyl groups. Following suitable organic chemistry transformation, the –OH end groups were converted to moieties able to form complementary hydrogen bonds including 2,6-diaminopurine, Dap, thymine, Thy, and the so-called Hamilton receptor, Ham. The formation of hydrogen bonds was examined between the polymers PS-Dap and PS-b-PI-Thy, along with the polymers PS-Ham and PS-b-PI-Thy. The conditions under which supramolecular triblock copolymers are formed and the possibility to form aggregates were examined both in solution and in the solid state using a variety of techniques such as 1H-NMR spectroscopy, size exclusion chromatography (SEC), dilute solution viscometry, dynamic light scattering (DLS), thermogravimetric analysis (TGA), differential thermogravimetry (DTG), and differential scanning calorimetry (DSC). Full article
(This article belongs to the Section Polymer Synthesis)
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Open AccessArticle
Methods for Determining the Thermal Transfer in Phase-Changing Materials (PCMs)
Polymers 2020, 12(2), 467; https://doi.org/10.3390/polym12020467 (registering DOI) - 18 Feb 2020
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Abstract
A very important issue that needs to be solved as simply and correctly as possible is how to establish the thermal performance of phase-changing materials (PCM). The undertaken researches have analyzed the values of the thermal performances of the PCM taking into account [...] Read more.
A very important issue that needs to be solved as simply and correctly as possible is how to establish the thermal performance of phase-changing materials (PCM). The undertaken researches have analyzed the values of the thermal performances of the PCM taking into account the method of finite elements and the experimental research, respectively, based on a modern measurement system that was designed and implemented. Butyl stearate which has been encapsulated through complex coacervation in polymethyl methacrylate has been used as a PCM. Samples were made containing 10%, 20%, 30% and 40% PCM, respectively, within their structure. The research has established that at both the hot plate and the cold plate interface, the evolution of the temperature over time, established by both the finite element method (FEM) and experimental research, are quite close, and the best results have been obtained for the P30 sample. A very important thing observed during the finite element method (FEM) is that the simulated thermal flow variation extends between 2700-3110W/m2 being small enough not to influence the temperature measurement at the interface of hot or cold plates. Thus, the use of the FEM or the experimental research method can be applied with good results, provided that the correct initial conditions are used in the finite element method and that the experimental research is performed using the best possible apparatus. Full article
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Open AccessArticle
On the Nature of Epoxy Resin Post-Curing
Polymers 2020, 12(2), 466; https://doi.org/10.3390/polym12020466 (registering DOI) - 18 Feb 2020
Viewed by 167
Abstract
Post-curing is intended to improve strength, elevate glass transition, and reduce residual stress and outgassing in thermosets. Also, experiments indicate post-curing temperatures lead to ether crosslinks and backbone dehydration. These results informed molecular dynamics methods to represent them and compare the resulting thermomechanical [...] Read more.
Post-curing is intended to improve strength, elevate glass transition, and reduce residual stress and outgassing in thermosets. Also, experiments indicate post-curing temperatures lead to ether crosslinks and backbone dehydration. These results informed molecular dynamics methods to represent them and compare the resulting thermomechanical effects. Diglycidyl ether of bisphenol A (DGEBA)-diamino diphenyl sulfone (DDS) systems were examined. Independent variables were resin length, stoichiometry, and reaction type (i.e., amine addition, etherification, and dehydration). Etherification affected excess epoxide systems most. These were strengthened and became strain hardening. Systems which were both etherified and dehydrated were most consistent with results of post-curing experiments. Dehydration stiffened and strengthened systems with the longer resin molecules due to their intermediate hydroxyl groups for crosslinking. Changes in the concavity of functions fit to the specific volume versus temperature were used to detect thermal transitions. Etherification generally increased transition temperatures. Dehydration resulted in more transitions. Full article
(This article belongs to the Special Issue Thermosets II)
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Open AccessArticle
Main Chain–Type Block Copolymers through Atom Transfer Radical Polymerization from Double-Decker–Shaped Polyhedral Oligomeric Silsesquioxane Hybrids
Polymers 2020, 12(2), 465; https://doi.org/10.3390/polym12020465 (registering DOI) - 17 Feb 2020
Viewed by 203
Abstract
In this study, we synthesized two main chain–type block copolymers featuring hydrogen bond donor and acceptor segments through atom transfer radical polymerization (ATRP) using a bifunctionalized polyhedral oligomeric silsesquioxane (POSS) nanoparticle as the initiator. Hydrosilylation of vinylbenzyl chloride at the two corners of [...] Read more.
In this study, we synthesized two main chain–type block copolymers featuring hydrogen bond donor and acceptor segments through atom transfer radical polymerization (ATRP) using a bifunctionalized polyhedral oligomeric silsesquioxane (POSS) nanoparticle as the initiator. Hydrosilylation of vinylbenzyl chloride at the two corners of a double-decker silsesquioxane (DDSQ) provided the bifunctionalized benzyl chloride initiator VBC-DDSQ-VBC, which we applied as a platform to prepare a main chain–type polystyrene homopolymer (PS-DDSQ-PS), the diblock copolymer poly(styrene–b–4-vinylpyridine) (P4VP-b-PS-DDSQ-PS-b-P4VP), and the diblock copolymer poly(styrene–btert-butoxystyrene) (PtBuOS-b-PS-DDSQ-PS-b-PtBuOS) through sequential ATRP. Selective hydrolysis of the tert-butoxyl units of PtBuOS-b-PS-DDSQ-PS-b-PtBuOS yielded the strongly hydrogen bonding diblock copolymer poly (styrene-b-vinylphenol) (PVPh-b-PS-DDSQ-PS-b-PVPh). We used Fourier transfer infrared spectroscopy, nuclear magnetic resonance spectroscopy, size exclusion chromatography, differential scanning calorimetry, mass-analyzed laser desorption ionization mass spectrometry, and transmission electron microscopy to investigate the chemical structures, thermal behavior, and self-assembled nanostructures formed by these main chain–type block copolymers based on DDSQ. Full article
(This article belongs to the Special Issue Silsesquioxane (POSS) Polymers, Copolymers and Nanoparticles)
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Open AccessReview
Protein–Polysaccharide Composite Materials: Fabrication and Applications
Polymers 2020, 12(2), 464; https://doi.org/10.3390/polym12020464 (registering DOI) - 17 Feb 2020
Viewed by 253
Abstract
Protein–polysaccharide composites have been known to show a wide range of applications in biomedical and green chemical fields. These composites have been fabricated into a variety of forms, such as films, fibers, particles, and gels, dependent upon their specific applications. Post treatments of [...] Read more.
Protein–polysaccharide composites have been known to show a wide range of applications in biomedical and green chemical fields. These composites have been fabricated into a variety of forms, such as films, fibers, particles, and gels, dependent upon their specific applications. Post treatments of these composites, such as enhancing chemical and physical changes, have been shown to favorably alter their structure and properties, allowing for specificity of medical treatments. Protein–polysaccharide composite materials introduce many opportunities to improve biological functions and contemporary technological functions. Current applications involving the replication of artificial tissues in tissue regeneration, wound therapy, effective drug delivery systems, and food colloids have benefited from protein–polysaccharide composite materials. Although there is limited research on the development of protein–polysaccharide composites, studies have proven their effectiveness and advantages amongst multiple fields. This review aims to provide insight on the elements of protein–polysaccharide complexes, how they are formed, and how they can be applied in modern material science and engineering. Full article
(This article belongs to the Special Issue Protein Biopolymer II)
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Open AccessArticle
Development of Poly (Lactide Acid) Foams with Thermally Expandable Microspheres
Polymers 2020, 12(2), 463; https://doi.org/10.3390/polym12020463 (registering DOI) - 17 Feb 2020
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Abstract
This study presents the investigation of different content of thermally expandable microsphere (EMS) type of a physical blowing agent added to polylactic acid (PLA). The effects of the different doses of EMS, processing temperatures, and d-lactide content of the polylactic acid were analyzed [...] Read more.
This study presents the investigation of different content of thermally expandable microsphere (EMS) type of a physical blowing agent added to polylactic acid (PLA). The effects of the different doses of EMS, processing temperatures, and d-lactide content of the polylactic acid were analyzed for foam properties and structures. We characterized the different PLAs and the physical blowing agent with different testing methods (gel permeation chromatography, rotational rheometry, isothermal thermogravimetric analysis, and thermomechanical analysis). The amounts of the foaming agent were 0.5, 1, 2, 4, 8 wt%, and processing temperatures were 190 °C, 210 °C, and 230 °C. The foam structures were produced by twin-screw extrusion. We used scanning electron microscopy to examine the cell structure of the foams produced, and carried out morphological and mechanical tests as well. The result of extrusion foaming of PLA using different amounts of EMS shows that an exponentially decreasing tendency of density reduction can be achieved, described by the following equation, ρ(x)=1.062∙e-x7.038+0.03 (R2 = 0.947) at 190 °C. With increasing processing temperature, density decreases at a lower rate, due to the effect that the microspheres are unable to hold the pentane gas within the polymer shell structure. The d-lactide content of the PLAs does not have a significant effect on the density of the produced foam structures. Full article
(This article belongs to the Section Polymer Applications)
Open AccessArticle
Salt-Free Dyeing of Modified Cotton through Graft Polymerization with Highly Enhanced Dye Fixation and Good Strength Properties
Polymers 2020, 12(2), 462; https://doi.org/10.3390/polym12020462 (registering DOI) - 17 Feb 2020
Viewed by 153
Abstract
Modification of cotton fabric with 2-methacryloyloxyethyltrimethyl ammonium chloride (DMC) was achieved through free-radical initiated graft polymerization with K2S2O8/NaHSO3 as the initiator. Grafting of DMC was confirmed by ATR-IR of the modified cotton. The optimal grafting reaction [...] Read more.
Modification of cotton fabric with 2-methacryloyloxyethyltrimethyl ammonium chloride (DMC) was achieved through free-radical initiated graft polymerization with K2S2O8/NaHSO3 as the initiator. Grafting of DMC was confirmed by ATR-IR of the modified cotton. The optimal grafting reaction conditions, including DMC dosage, mole ratio of initiator to DMC, temperature, and time, were determined by cation content and dye fixation results of the modified cotton. The modified fibers were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and whiteness measurement. Salt-free dyeing of the modified cotton with commonly used C. I. Reactive Blue 19, C. I. Reactive Yellow 145, and C. I. Reactive Red 195 presented high fixation of 96.8%, 98.7%, and 97.3%, respectively. These results indicated that the modification is effective for changing the surface charge of the fiber and increasing the dye-fiber reactivity. The color fastness and strength property were still very satisfactory. With excellent properties, this dyeing method shows promise in real application for eliminating the usage of salt and reducing environmental pollution. Full article
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Open AccessArticle
Dentin Bonding and SEM Analysis of a New Experimental Universal Adhesive System Containing a Dendrimer
Polymers 2020, 12(2), 461; https://doi.org/10.3390/polym12020461 (registering DOI) - 17 Feb 2020
Viewed by 157
Abstract
Due to their polymerization characteristics, hyper-branched dendrimers have lately shown to be promising candidates for use in dental materials. In this study, a new dental adhesive system was prepared, using a dendrimer derived from 2-isocyanatoethyl methacrylate (G-IEMA), and its adhesive properties were investigated. [...] Read more.
Due to their polymerization characteristics, hyper-branched dendrimers have lately shown to be promising candidates for use in dental materials. In this study, a new dental adhesive system was prepared, using a dendrimer derived from 2-isocyanatoethyl methacrylate (G-IEMA), and its adhesive properties were investigated. The exposed dentin was treated with four universal adhesives (UAs): SBU (Scotchbond Universal), FUT (Futurabond M+), AE1 (experimental adhesive with Bis-GMA) and AE2 (experimental adhesive with G-IEMA), using Etch & Rinse (ER) or Self Etch (SE) protocols. Composite build-ups were prepared and stored for 24 h at 37 °C in distilled water. Composite/dentin beams were prepared with cross-sectional areas of 1 ± 0.3 mm2 and µTBS (Micro-tensile bond strength) test was performed at 0.5 mm/min. Failures modes were evaluated by stereomicroscopy, and bonding interfaces were observed by scanning electron microscopy (SEM). Statistical analysis of µTBS data was performed using General Linear (GLM) and Linear Mixed Models (LMM). The effect of adhesive type on µTBS was significant (p = 0.010), with AE1 presenting significantly higher µTBS than SBU (p = 0.019). No other differences between adhesives were observed. ER showed significantly better results than SE (p = 0.019), and no significant interactions between the adhesives and protocols were determined. Results obtained so far pinpoint the emergence of a new paradigm in the dental materials field, as G-IEMA can be used successfully as an alternative to Bis-GMA. Full article
(This article belongs to the Section Polymer Applications)
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Open AccessArticle
Fabrication and Actuation of Cu-Ionic Polymer Metal Composite
Polymers 2020, 12(2), 460; https://doi.org/10.3390/polym12020460 (registering DOI) - 17 Feb 2020
Viewed by 188
Abstract
In this study, Cu-Ionic polymer metal composites (Cu-IPMC) were fabricated using the electroless plating method. The properties of Cu-IPMC in terms of morphology, water loss rate, adhesive force, surface resistance, displacements, and tip forces were evaluated under direct current voltage. In order to [...] Read more.
In this study, Cu-Ionic polymer metal composites (Cu-IPMC) were fabricated using the electroless plating method. The properties of Cu-IPMC in terms of morphology, water loss rate, adhesive force, surface resistance, displacements, and tip forces were evaluated under direct current voltage. In order to understand the relationship between lengths and actuation properties, we developed two static models of displacements and tip forces. The deposited Cu layer is uniform and smooth and contains about 90% by weight of copper, according to the energy-dispersive X-ray spectroscopy (EDS) analysis data obtained. The electrodes adhere well (level of 5B) on the membrane, to ensure a better conductivity and improve the actuation performance. The penetration depth of needle-like electrodes can reach up to around 70 μm, and the structure shows concise without complex branches, to speed up the actuation. Overall the maximum displacement increased as the voltage increased. The applied voltage for the maximum force output is 8–9 V. The root mean square error (RMSE) and determination coefficient (DC) of the displacement and force models are 1.66 and 1.23, 0.96 and 0.86, respectively. Full article
(This article belongs to the Section Polymer Processing and Performance)
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Open AccessArticle
Extrusion of Porous Protein-Based Polymers and Their Liquid Absorption Characteristics
Polymers 2020, 12(2), 459; https://doi.org/10.3390/polym12020459 (registering DOI) - 16 Feb 2020
Viewed by 262
Abstract
The production of porous wheat gluten (WG) absorbent materials by means of extrusion processing is presented for the future development of sustainable superabsorbent polymers (SAPs). Different temperatures, formulations, and WG compositions were used to determine a useful protocol that provides the best combination [...] Read more.
The production of porous wheat gluten (WG) absorbent materials by means of extrusion processing is presented for the future development of sustainable superabsorbent polymers (SAPs). Different temperatures, formulations, and WG compositions were used to determine a useful protocol that provides the best combination of porosity and water swelling properties. The most optimal formulation was based on 50 wt.% WG in water that was processed at 80 °C as a mixture, which provided a porous core structure with a denser outer shell. As a green foaming agent, food-grade sodium bicarbonate was added during the processing, which allowed the formation of a more open porous material. This extruded WG material was able to swell 280% in water and, due to the open-cell structure, 28% with non-polar limonene. The results are paving the way towards production of porous bio macromolecular structures with high polar/non-polar liquid uptake, using extrusion as a solvent free and energy efficient production technique without toxic reagents. Full article
(This article belongs to the Special Issue Nordic Polymer Days)
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