Characterization of Cellulosic Pulps Isolated from Two Widespread Agricultural Wastes: Cotton and Sunflower Stalks.

Globally, huge amounts of cotton and sunflower stalks are generated annually. These wastes are being underutilized since they are mostly burned in the fields. So, in this work, we proposed a three-step method consisting of acid pre-treatment, alkaline hydrolysis, and bleaching for the extraction of cellulose pulps. These pulps were characterized to assess their morpho-structural and thermal properties. The design of experiments and response surface methodology were used for the optimization of the acid pre-treatment in order to achieve maximum removal of non-cellulosic compounds and obtain pulps enriched in cellulose. For cotton stalks, optimal conditions were identified as a reaction time of 190 min, a reaction temperature of 96.2 °C, and an acid (nitric acid) concentration of 6.3%. For sunflower stalks, the optimized time, temperature, and acid concentration were 130 min, 73.8 °C, and 8.7%, respectively. The pulps obtained after bleaching contained more than 90% cellulose. However, special care must be taken during the process, especially in the acid pre-treatment, as it causes the solubilization of a great amount of material. The characterization revealed that the extraction process led to cellulose pulps with around 69-70% crystallinity and thermal stability in the range of 340-350 °C, ready to be used for their conversion into derivatives for industrial applications.

Obtaining Cellulose Nanocrystals from Olive Tree Pruning Waste and Evaluation of Their Influence as a Reinforcement on Biocomposites.

The objective of this work is to improve the mechanical properties of polylactic acid (PLA) by incorporating cellulose nanocrystals (CNC) previously obtained from a cellulose pulp extracted from olive tree pruning (OTP) waste. Composites were manufactured by melt processing and injection moulding to evaluate the effect of the introduction of CNC with conventional manufacturing methods. This OTP-cellulose pulp was subjected to a further purification process by bleaching, thus bringing the cellulose content up to 86.1%wt. This highly purified cellulose was hydrolysed with sulfuric acid to obtain CNCs with an average length of 267 nm and a degradation temperature of 300 °C. The CNCs obtained were used in different percentages (1, 3, and 5%wt.) as reinforcement in the manufacture of PLA-based composites. The effect of incorporating CNC into PLA matrix on the mechanical, water absorption, thermal, structural, and morphological properties was studied. Maximum tensile stress and Young's modulus improved by 87 and 58%, respectively, by incorporating 3 and 5%wt. CNC. Charpy impact strength increased by 21% with 3%wt. These results were attributed to the good dispersion of CNCs in the matrix, which was corroborated by SEM images. Crystallinity index, glass transition, and melting temperatures were maintained.

Effect of Olive Pit Reinforcement in Polylactic Acid Biocomposites on Environmental Degradation.

Polylactic acid (PLA) is a biomaterial widely used as an alternative to petroleum-based polymeric matrices in plastic components. PLA-based biocomposites reinforced with lignocellulosic waste are currently receiving special attention owing to their mechanical properties, low toxicity, recyclability, and biodegradability. The influence of the percentage of waste on their properties and resistance to degradation are some of the points of great relevance. Therefore, a series of PLA-based biocomposites containing different percentages of olive pits (5, 15, 25 and 40% wt.) were manufactured and characterized both (a) immediately after manufacture and (b) after one year of storage under environmental conditions. The results obtained were analyzed to evaluate the influence of the incorporation of olive pits on the resistance to degradation (measured through Carbonyl Indices, CI), mechanical properties (tensile, flexural and impact strength), structure (Fourier Transform Infrared Spectroscopy, FT-IR; and, X-ray Diffraction, XRD), morphology (Scanning Electron Microscopy, SEM) and water absorption capacity of the manufactured materials. PLA degradation, corroborated by Differential Scanning Calorimetry (DSC), FT-IR, and XRD, resulted in a decrease in tensile and flexural strengths and an increase in the tensile and flexural moduli. This trend was maintained for the biocomposites, confirming that reinforcement promoted the PLA degradation.

Preliminary Study of the Bactericide Properties of Biodegradable Polymers (PLA) with Metal Additives for 3D Printing Applications.

Plastic is a highly used material in various sectors. Due to its plentiful availability in the environment, microorganism surface contamination is a risk. The aim of this work is to achieve bactericidal capacity in plastics that reduces the microorganism's colonization risk and, consequently, reduces the chances of having an infection with E. coli and Listeria monocytogenes bacteria. Using polylactic acid (PLA) as the polymeric matrix, mixtures in concentrations of metal additive of ions of silver (Ag) R148 and S254 in 1% and 2% have been studied and manufactured. The materials are developed on an industrial scale through a process that proceeds as follows: (I) a mixture of polymer and additive in a double-screw compounder to obtain the compound in different concentrations, (II) the manufacture of filaments with a single-screw extruder, (III) 3D printing parts. Therefore, materials are evaluated in the form of powder, pellets and printed pieces to ensure their antibacterial effectiveness throughout the manufacturing process. The results of the research show antibacterial effectiveness for E. coli and Listeria monocytogenes of metal additives and polymeric compounds for all manufacturing phases on an industrial scale, with the effectiveness for additive R148 predominating at a concentration of 2%, demonstrating its microbial efficacy on surfaces with potential application in medicine.

Manufacture and Characterization of Recycled Polypropylene and Olive Pits Biocomposites.

The present work studies the use of olive pit (OP) as a reinforcement in the manufacture of composites based on a post-consumer recycled polypropylene (rPP). In this way, it is feasible to provide added value from olive pits, a by-product resulting from the olive industry operations, while promoting the circular economy and reducing the use of fossil-based polymers. For this purpose, suitable samples were manufactured using 25 wt% and 40 wt% of OP. Additionally, the effect of incorporating additives was studied: (a) a process control additive (PA), and (b) a coupling agent of maleic anhydride grafted polypropylene (MAPP). The results showed an improvement in Young's and flexural modulus with the OP addition. The incorporation of PA did not present any significant improvement in the properties of the materials, nevertheless it facilitated the biocomposite manufacturing process. As for the coupling agent, it significantly improved the mechanical properties, achieving the best results with the addition of the two types of additives and 40 wt% of OP. Moreover, the thermal properties were maintained, and there was an increase in crystallinity in all composites compared to rPP. According to the results of the fracture surface analysis, the coupling agent improves reinforcement-polymer matrix cohesion.

Experimental and Numerical Analysis for the Mechanical Characterization of PETG Polymers Manufactured with FDM Technology under Pure Uniaxial Compression Stress States for Architectural Applications.

This paper presents the numerical and experimental analysis performed on the polymeric material Polyethylene Terephthalate Glycol (PETG) manufactured with Fused Deposition Modeling Technology (FDM) technology, aiming at obtaining its mechanical characterization under uniaxial compression loads. Firstly, with the objective of evaluating the printing direction that poses a greater mechanical strength, eighteen test specimens were manufactured and analyzed according to the requirements of the ISO-604 standards. After that, a second experimental test analyzed the mechanical behavior of an innovative structural design manufactured in Z and X-Y directions under uniaxial compression loads according to the requirements of the Spanish CTE standard. The experimental results point to a mechanical linear behavior of PETG in X, Y and Z manufacturing directions up to strain levels close to the yield strength point. SEM micrographs show different structural failures linked to the specimen manufacturing directions. Test specimens manufactured along X present a brittle fracture caused by a delamination process. On the contrary, test specimens manufactured along X and Y directions show permanent plastic deformations, great flexibility and less strength under compression loads. Two numerical analyses were performed on the structural part using Young's compression modulus obtained from the experimental tests and the load specifications required for the Spanish CTE standards. The comparison between numerical and experimental results presents a percentage of relative error of 2.80% (Z-axis), 3.98% (X-axis) and 3.46% (Y-axis), which allows characterizing PETG plastic material manufactured with FDM as an isotropic material in the numerical simulation software without modifying the material modeling equations in the data software. The research presented here is of great help to researchers working with polymers and FDM technology for companies that might need to numerically simulate new designs with the PETG polymer and FDM technology.

Study of the influence of storage conditions on the quality and migration levels of antimony in polyethylene terephthalate-bottled water.

The main objectives of this study are to determine the presence of antimony in water stored in polyethylene terephthalate bottles and the influence of temperature and time over the migration levels. For this purpose, Sb determination was carried out in water at different experimental conditions: storage for one to three weeks at 25 to 80 ℃; long-term (six months) storage at room temperature between 16 and 24 ℃ and storage in car during summer which is a common consumer's habit. In addition, water quality analysis was developed after different time-temperature storage conditions. All the samples at the end of their storage conditions were analyzed by inductively coupled plasma mass spectrometry. The limit of detection and quantification were 0.50 and 0.80 µg/L, respectively. The results for the bottled water stored during six months indicated that the average Sb concentration was 0.332 ± 0.015 µg/L. This value is below the European maximum permissible migration level of 5 µg/L. With regard to the newly bottled water, no Sb was detected at the initial time for all temperatures studied. However, the Sb concentration in water increased with both time and temperature. The levels of Sb started exceeding the European limits when the samples were stored at 60 ℃ for two weeks.

Influence of Extreme Storage Conditions on Extra Virgin Olive Oil Parameters: Traceability Study.

This study reflects the effect of extreme storage conditions on several extra virgin olive oil (EVOO) varieties (arbequina, hojiblanca, and picual). The conditions were simulated in the laboratory, by means of heating treatments in stove at different temperatures (40 and 60°C) and times (two and three weeks). The aim is the evaluation of the deterioration of the quality parameters and minority components, which are responsible for the nutritional and therapeutic properties (fatty acids, polyphenols, pigments, and tocopherols), and organoleptic qualities. The quality criteria and limits used in this work are according to International Olive Council. The results contribute to the control of the traSceability for the commercialization of the EVOO.