Twin-screw Extruder Research Articles

Impact of added enzyme-treated bran on the techno-functional properties of puffed-extruded sorghum snack

Dietary fibre intake is crucial for improving human health and reducing the prevalence of diet-related non-communicable diseases. This study determines the effect of the enzyme (Viscozyme®L: a cocktail of cell wall degrading enzymes including arabanase, cellulase, β-glucanase, hemicellulase and xylanase) hydrolyzed fibre on the techno-functional properties of puffed-extruded sorghum snacks made from sorghum flour. Sorghum flour and sorghum flour mixed with untreated bran, water-incubated bran, and enzyme-treated bran were extruded using a twin-screw extruder. The puffed-extruded snacks from sorghum flour with 2-hour enzyme-treated bran showed similar expansion ratios to snacks from sorghum flour without bran. The expansion ratios of the without-bran snacks (2.80) and enzyme-treated bran-added snacks (2.77) were significantly (P<0.05) higher than those made with untreated sorghum bran (1.87). A higher expansion ratio usually results in a lighter, crispier texture and a more attractive appearance of puffed-extruded snacks, which consumers often prefer. The enzyme treatment also increased the water solubility index and decreased the water absorption index compared to snacks with untreated bran. This study explores the potential of using an enzyme-treated sorghum bran to manufacture puffed-extruded snacks comparable to those made with sorghum flour.

Analysis of the Dispersive and Distributive Mixing Effect of Screw Elements on the Co-Rotating Twin-Screw Extruder with Particle Tracking

Compounding is an important step in processing base polymers and is used to incorporate various additives into a polymer. For this purpose, different screw elements are used for dispersive and distributive mixing on a co-rotating twin-screw extruder. Optimising the screw configuration requires precise knowledge of the screw elements’ mixing properties, which have not been thoroughly investigated. This study analyses the mixing behaviour of individual screw elements regarding dispersive and distributive mixing using 3D CFD flow simulations with subsequent particle tracking. For distributive mixing, the particle distribution behind the screw elements in the XY plane is analysed and the mixing index MQ, which relates the standard deviation and the mean value of the triangular areas between the particles, is calculated. For dispersive mixing, the maximum shear stress on the particle path and the integral of the shear stress over the residence time of each individual particle are determined. The results show that screw element geometry and rotation speed have a significant influence on dispersive and distributive mixing. In addition, better dispersive mixing is achievable with highly viscous materials. These findings enable the optimisation of the mixing zone of a co-rotating twin-screw extruder for the efficient mixing of mineral fillers.

Upcycling of Chitin to Cross-Coupling Catalysts: Tailored Supports and Opportunities in Mechanochemistry.

In this study chitin derived from shrimp shells was used in the design of heterogeneous Pd-based catalysts for Heck and Suzuki-Miyaura cross-coupling reactions. The synthesis of Pd nanoparticles supported on N-doped carbons was performed through different approaches, including a sustainable mechanochemical approach, by using a twin-screw extruder. All catalytic systems were characterized by a multitechnique approach and the effect of nanoparticles size, N-doping on the support, and their synergistic interactions were elucidated. Specifically, Kelvin Probe Atomic Force Microscopy provided valuable insights on charge transfer and metal-support interactions. The catalytic behaviour of the samples was investigated in cross-coupling reactions under batch conditions and under semi-continuous flow solvent-free conditions, respectively obtaining a quantitative yield and a noteworthy productivity of 8.7 mol/(gPdh).

Highly Filled Waste Polyester Fiber/Low-Density Polyethylene Composites with a Better Fiber Length Retention Fabricated by a Two-Rotor Continuous Mixer

A key challenge in the utilization of waste polyester fibers (PET fibers) is the development of fiber-reinforced composites with high filler content and the improvement of fiber length retention. Herein, the effects of a two-rotor continuous mixer and a twin-screw extruder on the structure and properties of waste polyester fiber composites were evaluated. The results revealed that the mechanical properties of the composites were improved significantly with increasing fiber content, especially when processed using the twin-rotor continuous mixer. This mixer facilitated the formation of a robust fiber network structure, leading to substantial enhancements in tensile strength, flexural strength, and heat resistance. Specifically, compared to those processed by the twin-screw extruder, with 60 wt% fibers content, the tensile and flexural strengths of specimens processed by the twin-rotor continuous mixer increase by 21% and 13%, respectively. The average fiber length in specimens processed by the twin-rotor continuous mixer was 32% longer than that in specimens processed by the twin-screw extruder, attributable to the lower shear frequency and the higher tensile ratio of the former. This blending technique emerges as an effective strategy, contributing significantly to promoting the development and practical application of waste textile fiber-reinforced polymer composites.

Sugar inclusion influences the expansion characteristics of corn starch extrudates.

Corn starch-based direct expanded products incorporated with 2% and 10% (w/w) sugar (fructose, glucose, sucrose, and xylose) were produced using a 20mm co-rotating twin-screw extruder. The pasting and thermal properties of raw corn starch-sugar mixes were analyzed before extrusion processing. The independent variables for extrusion processing included two sugar inclusion levels (2% and 10% w/w) and two screw speeds (150 and 250rpm). The extrudates were characterized by their initial expansion ratio (IER), expansion ratio (ER), and shrinkage. ER values were high for fructose at 2% and 150rpm and 10% glucose and sucrose extrudates at 250rpm. The extrudates with 2% sucrose inclusion shrunk significantly higher than the control. Fourier transform infrared (FTIR) spectroscopy of the extruded blends did not indicate the presence of any new covalent bond formed between starch and sugar post-extrusion. The interactions between sugar concentration and screw speed significantly influenced extrudate expansion characteristics. Due to their thermal and plasticizing properties, sugar inclusion (glucose, fructose, sucrose, and xylose) enhanced the extrudate expansion by altering their melt viscosity. PRACTICAL APPLICATION: The findings of this study can improve the expansion characteristics of high-fiber-based extruded snacks. Ingredients high in fiber generally hinder the starch transformation during extrusion and negatively impact the expansion properties. The presence of sugar at low concentrations can improve melt properties during extrusion processing and, in turn, significantly improve the textural properties of snacks.

Conversion of kraft lignin to hydrocarbons using an integrated molten salt pyrolysis/catalytic hydrotreatment approach

Thermochemical conversion of underutilized lignocellulosic streams such as kraft lignin from the pulp and paper industry has the potential to produce sustainable chemicals and biofuels. We here report a process to continuously convert softwood-based lignoboost lignin to hydrocarbons using a three-step approach: i) liquefaction/dispersion of the lignin in a suitable molten salt, ii) pyrolysis of the liquefied/dispersed lignin in a molten salt mixture (ZnCl2, KCl, and NaCl), to obtain a crude lignin oil and iii) upgrading of the lignin oil using a catalytic hydrotreatment to yield hydrocarbons. Step 1 and 2 were integrated using a twin screw extruder with different heating sections at a scale of 20 g/h lignin input. Besides char, a lignin oil, mainly composed of monomeric phenolics, and propylene were the major products. The highest yield of the latter two products was around 32 wt% (23 wt% crude lignin oil and 9 wt% propylene). The lignin oil was subsequently converted to hydrocarbons using a two-step catalytic hydrotreatment approach (stabilization step using CoMo/Al2O3 catalyst and a further deep hydrotreatment over a NiMo/Al2O3 catalyst). The final liquid product contained less than 0.5 wt% of oxygen and was shown to be rich in (cyclo)alkanes and aromatic hydrocarbons. The carbon yield for the overall conversion of lignin to hydrocarbons was 23 %.

Development and in vitro Evaluation of Cannabidiol Mucoadhesive Buccal Film Formulations Using Hot-Melt Extrusion Technology

Introduction: Cannabidiol (CBD) has sparked considerable interest because of its wide range of pharmacological uses and the fact that it does not induce psychoactive effects. CBD formulation development presents significant challenges due to its limited water solubility and susceptibility to first-pass metabolism, both of which restrict its overall bioavailability. The current research aimed to use hot-melt extrusion (HME) technology to develop mucoadhesive buccal films to improve CBD solubility and reduce first-pass metabolism. Methods: Five formulations containing 10% w/w CBD were extruded using a counter-rotating twin-screw extruder (Haake Minilab II, Thermo Fisher Scientific). Different characterization studies were conducted on the developed formulations. Results: Differential scanning calorimetry (DSC) revealed that the CBD endothermic peak disappeared in some of the developed films, indicating that CBD was converted from crystalline to amorphous form. A bio-adhesion study showed that the formulations containing Carbopol® (BF2, BF3, BF4, and BF5) had higher adhesiveness properties. In vitro release and solubility studies showed an increase in CBD release and water solubility in the developed formulations when compared to pure CBD. Stability studies revealed that CBD content and release in the lead formulation (BF2) was stable over 15 months. Conclusion: The current study demonstrates that HME was successfully used as an approach to develop CBD mucoadhesive buccal films and CBD solubility was enhanced.

Exploring interfacial tension role in the laminar morphology development in reactive compatibilized PP/EVOH

AbstractLaminar-like structures in PP/EVOH (80/20 wt%) blends were developed by in situ reactive compatibilization using a co-rotating intermeshing twin-screw extrusion without the imposition of post-die-forming elongation flows, i.e., draw ratio (DR) = 0. For that, a maleic anhydride-grafted homopolymer polypropylene (PP-g-MA) was added at 1, 1.5, and 3 wt% using a simple mixing protocol. The correlation between the laminar morphology observed via SEM with interfacial parameters was conducted by nonlinear regression of PP/EVOH viscoelastic response (Gʹ and Gʹʹ) applying the Monomodal Palierne Model to estimate interfacial tension. Uncompatibilized PP/EVOH formed a droplet-matrix morphology with high interfacial tension, indicating incompatibility. As PP-g-MA is added, a laminar-like structure is developed. The remaining droplets become smaller at higher content, with lower interfacial tension between the phases. This scenario hampers the stratification of the dispersed phase. At 3 wt% of PP-g-MA, the morphology returns to being a droplet-matrix, although with high adhesion between the phases. Graphical abstract

Physical properties, nutritional profile, and consumer acceptability of gluten-free breakfast flakes from cassava flour

Driven by the increasing demand for gluten-free and affordable breakfast options, this study investigated the potential of cassava flour, as a primary ingredient and gluten-free alternative, for producing extruded breakfast flakes. Cassava flakes were prepared using a twin-screw extruder at a constant screw speed of 35 rpm, constant cutter speed of 21.2 rpm and barrel temperatures of 81 °C, 93 °C, and 89 °C in the first, second, and third zones, respectively. The physical properties, nutritional profile, and consumer acceptability of the cassava flakes were compared to a commercially available breakfast cereal. Cassava flakes exhibited significantly different (p < 0.05) physical properties. They had a higher WSI (57.6 %) but lower values of bulk density (0.3 g/cm3), WAI (2.3 g g-1), and color value (yellow orange ±1.73). Cassava flakes had lower fat (0.3 %), protein (6.6 %), and dietary fiber (1.8 %) compared to the commercial product, except for ash (2.3 %), moisture (6.0 %), carbohydrates (89.0 %), and energy (384.7 Kcal/100 g). Despite these differences, cassava flakes met the UNBS requirements for breakfast cereals. Additionally, the cassava flakes’ nutritional adequacy for school going children and adolescents was assessed by determining their %contribution to RDA per serving (30 g cassava flakes + 100 g milk). Their contribution to the RDAs of school going children was minimal with only the contribution of carbohydrates for all age groups and the contribution of protein for 4–8 years aged children meeting recommendations due to the low protein, fat and fiber content. It is, therefore, important to consider reformulation of the cassava flakes and incorporation of other ingredients to improve their protein, fiber, and energy content. Overall, cassava flakes were acceptable with good functionality, but the acceptability can further be enhanced through optimization of the sensory and nutritional qualities.

Antibacterial performance of biodegradable polymer and hazelnut husk flour antibacterial biofilm with silver nanoparticles

The antibacterial performance of biocomposite films prepared from lignocellulosic waste (hazelnut husk or hazelnut leafy green cover) modified with silver nanoparticles and polylactic acid (PLA) was determined. The amount of hazelnut husk in the PLA matrix ranged from 10 to 40% by weight in 10% increments. The composite pellets were produced using a twin-screw extruder. Biocomposite films of 0.6 mm x 40 mm x 200 mm were produced from the pellets in a laboratory hydraulic hot press. The surfaces of the modified hazelnut husk and biocomposite specimens were analyzed by scanning electron microscopy (SEM) and inductively coupled plasma optical emission spectrometry (ICP-OES). The antibacterial activity of the biocomposite films against Staphylococcus aureus bacteria was determined using the ASTM E 2149 (2020) method. The antibacterial activity of the biocomposite films increased noticeably with the addition of hazelnut husk modified with the silver nanoparticles. Compared to the pure PLA film, the biocomposite films with 10 wt% modified husk flour showed the lowest antibacterial activity (31.3%) against S. aureus over 24-h while the films with 40 wt% showed the highest antibacterial activity (99.9%). The biocomposite films made of hazelnut husk flour with silver nanoparticles and PLA matrix could be considered for food packaging applications.

Recycled Low Density Polyethylene Reinforced with Deverra tortuosa Vegetable Fibers

In this work, natural fibers extracted from the medicinal aromatic plant Deverra tortuosa, with different sizes (S1 = 2 mm and S2 = 500 μm), were incorporated into recycled low density polyethylene (rLDPE) to produce sustainable biocomposites. Compounding was performed with different fiber concentrations (0 to 30% wt.) via twin-screw extrusion followed by injection molding. Based on the samples obtained, a comprehensive series of characterization was conducted, encompassing morphological and mechanical (flexural, tensile, hardness, and impact) properties. Additionally, thermal properties were assessed via differential scanning calorimetry (DSC), while Fourier transform infrared spectroscopy (FTIR) was used to elucidate potential chemical interactions and changes with processing. Across the range of conditions investigated, substantial improvements were observed in the rLDPE properties, in particular for the tensile modulus (23% for S1 and 104% for S2), flexural modulus (47% for S1 and 61% for S2), and flexural strength (31% for S1 and 65% for S2). Nevertheless, the tensile strength decreased (15% for S1 and 46% for S2) due to poor fiber–matrix interfacial adhesion. These preliminary results can be used for further development in sustainable packaging materials.

Modifying Cassava Starch via Extrusion with Phosphate, Erythorbate and Nitrite: Phosphorylation, Hydrolysis and Plasticization.

Extrusion processing of plasticized cassava starch, a prominent industrial crop, with chemical additives offers a thermo-mechanical approach to modify starch structures through physical and chemical interactions. This research investigates the interaction and morphology of thermoplastic cassava starch (TPS) blended with tetrasodium pyrophosphate (Na4P2O7), sodium tripolyphosphate (Na5P3O10), sodium hexametaphosphate (Na6(PO3)6), sodium erythorbate (C6H7O6Na), and sodium nitrite (NaNO2) via twin-screw extrusion. The effects of these additives on the chemical structure, thermal profile, water absorption, and solubility of the TPS were examined. The high temperature and shearing forces within the extruder disrupted hydrogen bonding at α-(1-4) and α-(1-6) glycosidic linkages within anhydroglucose units. Na4P2O7, Na5P3O10 and Na6(PO3)6 induced starch phosphorylation, while 1H NMR and ATR-FTIR analyses revealed that C6H7O6Na and NaNO2 caused starch hydrolysis. These additives hindered starch recrystallization, resulting in higher amorphous fractions that subsequently influenced the thermal properties and stability of the extruded TPS. Furthermore, the type and content of the added modifier influenced the water absorption and solubility of the TPS due to varying levels of interaction. These modified starch materials exhibited enhanced antimicrobial properties against Escherichia coli and Staphylococcus aureus in polyester blends fabricated via extrusion, with nitrite demonstrating the most potent antimicrobial efficacy. These findings suggest that starch modification via either phosphorylation or acid hydrolysis impacts the thermal properties, morphology, and hydrophilicity of extruded cassava TPS.

Mechanochemical preparation and performance regulation mechanism of highly durable and multifunctional iron red nanocomposite pigments derived from natural mixed-dimensional palygorskite clay

Iron oxide red pigments are one of the most widely used inorganic red pigments around the world. It is always pursed to improve their physicochemical properties. Herein, a continuous mechanochemical method was employed to fabricate high-performance iron red nanocomposite pigments via anchoring α-Fe2O3 nanoparticles on the surface of natural mixed-dimensional palygorskite clay (MDPal). The mechanical force of twin-screw extrusion promoted the Si-OH groups of MDPal to coordinate with Fe3+ to form the precursor, while MDPal was activated with the residual H+ of the involved nitrate to accelerate the thermal diffusion of Al3+ into α-Fe2O3 crystal lattice, thus the nanocomposite pigments presented a bright yellowish-red color (L∗ ​= ​35.61, a∗ ​= ​33.10, b∗ ​= ​35.86, C∗ ​= ​48.80). Furthermore, the mixed-dimensional nanostructure of MDPal served as a good substrate for chemical bonding of α-Fe2O3 nanoparticles to improve the dispersion and environmental stability of iron red pigments. Due to the synergistic effect of each component and the excellent thermal and chemical stability, the obtained nanocomposite pigments exhibited excellent application prospect as functional inorganic pigments for anti-corrosion coating, overglaze ceramic and coloring and reinforcing of polypropylene, respectively. It provided a facile strategy for preparation of high-performance multifunctional iron red pigments based on MDPal.

DETERMINATION THERMAL AND MECHANICAL PROPERTIES OF NANO CARBON, GRAPHITE AND GRAPHENE REINFORCED RECYCLING POLYPROPYLENE COMPOSITE SAMPLES

Polymer-based plastic materials occupy a major place in daily life. However, due to the nature of polymer materials, low thermal resistance and mechanical properties of these products, the need for new and sustainable materials in the industry has increased. With the rapid technological developments in advanced manufacturing industries such as aviation, marine, motor sports and defence industry, lightweight and high-strength composite products have become even more important. In this context, in this study, 1% carbon, graphene and graphite particle reinforced Polypropylene (PP) composite material mixed in a twin-screw extruder and MA/G series injection moulding machine standard tensile test sample produced. Melt Flow Index (MFI), Heat Deformation Test (HDT), tensile test, Shore-D hardness measurement and density tests performed on these test samples. According to the results obtained from these tests, the mechanical and thermal properties of the test samples produced from different composite materials were determined. The best mechanical and thermal properties occurred in the graphene particle. It formed in graphite and carbon, respectively.

Physical, mechanical and thermal properties of novel bamboo/kenaf fiber-reinforced polylactic acid (PLA) hybrid composites

This study investigates the physical, mechanical, and thermal properties of bamboo (BF) and kenaf (KF) fiber-reinforced polylactic acid (PLA) hybrid composites. Three hybrid (30BF-70KF, 50BF-50KF, and 70BF-30KF) and two non-hybrid (BF-PLA and KF-PLA) composites were developed through twin screw extrusion and compression molding techniques. The physical properties (density, void content, crystallinity via XRD, and chemical interactions via FTIR), mechanical properties (tensile, flexural, compressive, impact, and hardness), and thermal properties (Thermogravimetric analysis-TGA and Differential scanning calorimetry-DSC) were thoroughly analyzed. BF reinforcement reduced the composites’ density to 1.1826 g/cm³, while the inclusion of KF increased it to 1.2479 g/cm³. 50:50 blend of bamboo-kenaf reinforcement achieved the lowest void content of 0.27 %. The XRD patterns revealed heightened crystallinity in the BF-PLA composite. FTIR analysis showed stable functional groups, with O–H absorption bands indicative of cellulosic fibers. The BF-PLA non-hybrid composite exhibited the highest tensile strength at 25.95 MPa and compressive strength at 173.15 MPa, with the 30BF-70KF hybrid composite showing notable impact strength. Fractured morphology by FESEM revealed superior fiber-matrix adhesion for BF-PLA composite. TGA demonstrated a variation in thermal degradation temperatures, with the BF30-KF70 composite showing the highest onset of degradation at 484 °C. DSC analysis indicated a reduction in the glass transition temperature (Tg) across all fiber-reinforced samples and revealed significant adjustments in melting and crystallization temperatures. This research highlights the potential of BF-KF/PLA hybrid composites in the development of eco-friendly plastic furniture and consumer products.

Studies on mechanical, thermal, rheological and impact properties of polyamide 6 and thermoplastic copoly(ether-ester) elastomer blends

A series of blends of polyamide 6 (PA-6) (nylon-6) and a copoly(ether-ester) (HYTREL) were prepared by the melt-mixing method using a twin-screw extruder. The HYTREL content was varied from 0% to 25% by weight of the blends. Thermal and rheological studies on the blends using differential scanning calorimetry, dynamic mechanical analysis (DMA) and capillary rheometer showed that the blends are semi-compatible in nature. A two-phase globular morphology of the blends was established by scanning electron microscope (SEM) analysis. The matrix ligament thickness (interparticle distance) in each blend composition was measured from SEM images and compared with those calculated using Wu’s equation. The impact strength of the blends as measured by the Izod impact test was found to be substantially improved as a result of the incorporation of HYTREL. The toughness determined by loss area calculation from the DMA spectrum showed similar trends. The toughness was found to be optimal in a blend having 15 wt.% HYTREL with an average dispersed particle size of around 450 nm. The yield stress of the blend decreased in comparison to PA-6 on addition of HYTREL, while the thermal stability of PA-6 remained unaffected.

Scaling-Up for the Counter-Rotating Twin Screw Extrusion of Polymers.

A novel and original computer scaling-up system for the counter-rotating twin screw extrusion of polymers was developed. In the system, each scaling parameter (scaling criterion) may be considered as an objective function to be minimized for the single parameters or the functional relationships along the length of the screw. Scaling was based on the process simulation, which was performed using the comprehensive (or global) counter-rotating twin screw extrusion program called TSEM (Twin Screw Extrusion Model). The extrusion process was scaled by applying GASESTWIN (Genetic Algorithms Screw Extrusion Scaling) software developed for this purpose using genetic algorithms. Scaling up the extrusion process was carried out to enhance extrusion process throughput according to the scaling criteria specified by the single quantities of polymer melt temperature at the die exit and relative melting length, and by distributions along the screw length of the extrusion parameters of the polymer melt temperature and polymer plasticating. The global objective function had the lowest value for the selected extrusion parameters, which means the minimal differences between the values of the scaled-up processes and extrusion throughput was significantly increased. The solution to the problem of scaling the counter-rotating process presented in this paper complements the existing solutions for optimizing and scaling basic variants of the extrusion process, i.e., flood-fed and starve (metered)-fed single-screw extrusion, as well as co-rotating and counter-rotating twin-screw extrusion.

Influence of Twin Screw Extrusion Conditions on MWCNT Length and Dispersion and Resulting Electrical and Mechanical Properties of Polycarbonate Composites

The processing conditions were varied during the production of polycarbonate-based composites with the multiwalled carbon nanotubes (MWCNTs) Baytubes® C150 P (Bayer MaterialScience AG, Leverkusen, Germany), by melt mixing with an extruder on a laboratory scale. These included the screw design, rotation speed, throughput, feeding position and MWCNT content. Particular attention was paid to the shortening of the MWCNT length as a function of the conditions mentioned. It was found that there is a correlation between the applied specific mechanical energy (SME) during the melt mixing process and MWCNT dispersion, which was quantified by the agglomerate area ratio of the non-dispersed nanotubes based on optical microscopic analysis. The higher the SME value, the lower this ratio, which indicates better dispersion. Above an SME value of about 0.4 kWh/kg, no further improvement in dispersion was achieved. The MWCNT length, as measured by the quantitative analysis of TEM images of the MWCNTs dissolved from the composites, decreased with the SME value down to values of 44% of the original MWCNT length. At a constant loading of 3 wt.%, the tensile strength and tensile modulus were almost independent of the SME, while the elongation at break and notched impact strength showed an increasing trend. The variation in the feeding position showed that feeding the MWCNTs into a side feeder led to slightly better electrical and mechanical properties for both types of MWCNTs studied (Baytubes® C150 P and Nanocyl™ NC7000 (Nanocyl S.A., Sambreville, Belgium)). However, feeding into the hopper led to better CNT dispersion with Baytubes® C150 P, while this was the case with Nanocyl™ NC7000 when feeding into the side feeder. The screw profile had an influence on the dispersion, the MWCNT length and the electrical resistance, but only to a small extent. Distributive screws led to a greater shortening of the MWCNT length than dispersive screws. By varying the MWCNT content, it was shown that a greater MWCNT shortening occurred at higher loadings. Two-stage masterbatch dilution leads to stronger shortening than composite production with direct MWCNT incorporation.

Recycling of EPDM rubber via thermomechanical devulcanization: Batch and continuous operations

Thermomechanical devulcanization is a possible solution for the circular economy of EPDM rubber, as it removes covalent crosslinks from vulcanizates, resulting in a material similar to uncured rubber mixes. In this paper, sulfur-cured EPDM rubber was treated with thermomechanical stimuli: a) processing on a two-roll mill and in an internal mixer, and b) twin-screw extrusion. Horikx's analysis indicated a 75 % decrease in crosslink density with little polymer chain degradation. The resulting devulcanizates and non-devulcanized rubber crumb were added to the original rubber mix, yielding samples with 0, 25, 50, 75 and 100 wt% recycled rubber contents. Revulcanizates with up to 50 wt% devulcanizate content retained the tensile strength of the original rubber with a slight increase in modulus. Ultimately, batch devulcanization had the most promising results, and extrusion devulcanization was also more beneficial than using non-devulcanized rubber crumb. Crosslink density and morphological tests also support these findings.

Use of graphene (go and rGO) as a reinforcement filler to increase the beta phase in fluorinated copolymer nanocomposites

The present study aims to evaluate the influence of different types of graphene, graphene oxide (GO, synthesized by the Hummers method) and reduced graphene oxide (rGO, obtained by thermal reduction of GO) on the piezoelectric properties of composites based on PVDF copolymer. Hydrogen-fluorine interaction is expected to occur between GO or rGO and the fluorinated copolymer, increasing the β-conformation content in the polymer. The samples were prepared in the molten state at two concentrations of each charge inside a twin-screw extruder with interpenetrating screws. The characterizations of the nanocomposites were made according to their thermal and electrical properties. The effect of graphene incorporation into the P(VDF-TrFE) matrix was observed from thermogravimetric analysis (TGA), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The results obtained indicated that the incorporation of graphene contributed to the increase in the β phase content of P(VDF-TrFE), which is indicative of the increase in its piezoelectricity.