Estudo da flamabilidade e resistência à chama de compósito de poliéster insaturado e fibra da folha do abacaxizeiro (PALF)

In the present research work, composites were prepared using pine apple leaf fibres (PALF) as reinforcement with unsaturated polyester resin as matrix, incorporating with fire retardant at different compositions. The PALF was obtained from the decortication of pine apple leaves obtained from Ramada 4 from Ielmo Marinho in the State of Rio Grande do Norte. The unsaturated polyester resin and the catalyzer were bought from the local establishment. The fire retardant, aluminium tri-hydroxide - Al(OH)3 was donated by Alcoa Alumínio S.A and was used in the proportions of 20%, 40% and 60% w/w. Initially the fibres were treated with 2% NaOH for 1 hour, to remove any impurities present on the fibre surface, such as wax, fat, pectin and pectate, in order to have a better adsorption of the fibres with the matrix as well as the flame retardant. The fibre mat was prepared in a mat preparator by immersion, developed in the Textile Engineering Laboratory, at the UFRN. The composites (300x300x3 mm) were prepared by compression molding and the samples (150x25x3 mm) for analysis of the properties were cut randomly using a laser cutter. Some of the cut samples were used to measure the smoke emission and fire resistance using UL94 standard. Mechanical tension-extension and flexural properties were carried in CTGás RN and the Laboratório de Metais e Ensaios Mecânicos Engenharia de Materiais UFRN , as well as SEM studies were carried out at Núcleo de Estudos em Petróleo e Gás Natural - UFRN . From the observed results, it was noted that, there was no marked influence of the fire retardant on the mechanical properties. Also in the water absorption test, the quantity of water absorbed was less in the sample with higher concentration of fire retardant. It was also observed that the increase in the proportion of the fire retardant increased the time of burning, may be due to the compactness of the composite due to the presence of fire retardant as a filling material even though it was meant to reduce the rate of inflammability of the composite

Produção de enzimas por fungos em fermentação semi-sólida utilizando bagaço de coco e pedúnculo de caju como substratos

The production of enzymes by microorganisms using organic residues is important and it can be associated with several applications such as food and chemical industries and so on. The objective of this work is the production of CMCase, Xylanase, Avicelase and FPase enzymes by solid state fermentation (SSF) using as substrates: bagasse of coconut and dried cashew stem. The microorganisms employed are Penicillium chrysogenum and an isolated fungus from the coconut bark (Aspergillus fumigatus). Through the factorial design methodology and response surface analysis it was possible to study the influence of the humidity and pH. For Penicillium chrysogenum and the isolated fungus, the coconut bagasse was used as culture medium. In another fermentation, it was used the mixture of coconut bagasse and cashew stem. Fermentations were conducted using only the coconut bagasse as substrate in cultures with Penicillium chrysogenum fungus and the isolated one. A mixture with 50% of coconut and 50% of cashew stem was employed only for Penicillium chrysogenum fungus, the cultivation conditions were: 120 hours at 30 °C in BOD, changing humidity and pH values. In order to check the influence of the variables: humidity and pH, a 2 2 factorial experimental design was developed, and then two factors with two levels for each factor and three repetitions at the central point. The levels of the independent variables used in ascending order (-1, 0, +1), to humidity, 66%, 70.5% and 75% and pH 3, 5 and 7, respectively. The software STATISTICA TM (version 7.0, StatSoft, Inc.) was used to calculate the main effects of the variables and their interactions. The response surface methodology was used to optimize the conditions of the SSF. A chemical and a physic-chemical characterization of the coconut bagasse have determined the composition of cellulose (%) = 39.09; Hemicellulose (%) = 23.80, Total Lignin (%) = 36.22 and Pectin (%) = 1.64. To the characterization of cashew stem, the values were cellulose (g) = 15.91 Hemicellulose (%) = 16.77, Total Lignin (%) = 30.04 and Pectin (%) = 15.24. The results indicate the potential of the materials as substrate for semisolid fermentation enzyme production. The two microorganisms used are presented as good producers of cellulases. The results showed the potential of the fungus in the production of CMCase enzyme, with a maximum of 0.282 UI/mL and the Avicelase enzyme the maximum value ranged from 0.018 to 0.020 UI/ mL, using only coconut bagasse as substrate. The Penicillium chrysogenum fungus has showed the best results for CMCase = 0.294 UI/mL, FPase = 0.058 UI/mL, Avicelase = 0.010 UI/mL and Xylanase = 0.644 UI/ mL enzyme, using coconut bagasse and cashew stem as substrates. The Penicllium chrysogenum fungus showed enzymatic activities using only the coconut as substrate for CMCase = 0.233 UI/mL, FPase = 0.031 to 0.032 UI/ mL, Avicelase = 0.018 to 0.020 UI/mL and Xylanase = 0.735 UI/ mL. Thus, it can be concluded that the used organisms and substrates have offered potential for enzyme production processes in a semi-solid cultivation

Palma forrageira (Opuntia ficus indica e Nopalea cochenillifera) como matéria-prima para produção de etanol celulósico e enzimas celulolíticas

The need for new sources of energy and the concern about the environment have pushed the search for renewable energy sources such as ethanol. The use of lignocellulosic biomass as substrate appears as an important alternative because of the abundance of this raw material and for it does not compete with food production. However, the process still meets difficulties of implementation, including the cost for production of enzymes that degrade cellulose to fermentable sugars. The aim of this study was to evaluate the behavior of the species of cactus pear Opuntia ficus indica and Nopalea cochenillifera, commonly found in northeastern Brazil, as raw materials for the production of: 1) cellulosic ethanol by simultaneous saccharification and fermentation (SSF) process, using two different strains of Saccharomyces cerevisiae (PE-2 and LNF CA-11), and 2) cellulolytic enzymes by semi-solid state fermentation (SSSF) using the filamentous fungus Penicillium chrysogenum. Before alcoholic fermentation process, the material was conditioned and pretreated by three different strategies: alkaline hydrogen peroxide, alkaline using NaOH and acid using H2SO4 followed by alkaline delignification with NaOH. Analysis of composition, crystallinity and enzymatic digestibility were carried out with the material before and after pretreatment. In addition, scanning electron microscopy images were used to compare qualitatively the material and observe the effects of pretreatments. An experimental design 2² with triplicate at the central point was used to evaluate the influence of temperature (30, 40 and 45 °C) and the initial charge of substrate (3, 4 and 5% cellulose) in the SSF process using the material obtained through the best condition and testing both strains of S. cerevisiae, one of them flocculent (LNF CA-11). For cellulase production, the filamentous fungus P. chrysogenum was tested with N. cochenillifera in the raw condition (without pretreatment) and pretrated hydrothermically, varying the pH of the fermentative medium (3, 5 and 7). The characterization of cactus pear resulted in 31.55% cellulose, 17.12% hemicellulose and 10.25% lignin for N. cochenillifera and 34.86% cellulose, 19.97% hemicellulose and 15.72% lignin for O. ficus indica. It has also been determined, to N. cochenillifera and O. ficus indica, the content of pectin (5.44% and 5.55% of calcium pectate, respectively), extractives (26.90% and 9.69%, respectively) and ashes (5.40% and 5.95%). Pretreatment using alkaline hydrogen peroxide resulted in the best cellulose recovery results (86.16% for N. cochenillifera and 93.59% for O. ficus indica) and delignification (48.79% and 23.84% for N. cochenillifera and O. ficus indica, respectively). This pretreatment was also the only one which did not increase the crystallinity index of the samples, in the case of O. ficus indica. However, when analyzing the enzymatic digestibility of cellulose, alkali pretreatment was the one which showed the best yields and therefore it was chosen for the tests in SSF. The experiments showed higher yield of conversion of cellulose to ethanol by PE-2 strain using the pretreated N. cochenillifera (93.81%) at 40 °C using 4% initial charge of cellulose. N. cochenillifera gave better yields than O. ficus indica and PE-2 strain showed better performance than CA-11. N. cochenillifera proved to be a substrate that can be used in the SSSF for enzymes production, reaching values of 1.00 U/g of CMCase and 0.85 FPU/g. The pretreatment was not effective to increase the enzymatic activity values

Estudo da produção de pectinase por fermentação em estado sólido utilizando pedúnculo de caju como substrato

Pectinolytic enzymes, or simply pectinases, are complex enzymes that degrade pectic polymers. They have many uses, such as fruit juice extraction and purification, textile fiber treatment and vegetal oil extraction. The aim of this work was to study the kinetics of pectinases production by solid-state fermentation, using dry cashew apple residue as substrate and the microorganism Aspergillus niger CCT 0916. The influence of the initial medium moisture and medium supplementation with a source of nitrogen and phosphorus was evaluated using the factorial experimental planning and response surface methodology. Ammonia sulphate and potassium phosphate were used as nitrogen and phosphorus source, respectively. The variables time of contact (T) and ratio volume solvent/fermented medium (RZ), in systems with and without agitation, were evaluated in order to study the best extraction condition of the produced enzyme. Washed and unwashed cashew apple residues were tested as the growth medium. The unwashed residue was obtained by drying the residue after the extraction of the juice, while the washed residue was obtained by water washing 5 times using the proportion of 1 kg pulp/2 liters of water. Samples were taken every 12 hours for moisture content, pH, protein, reducing sugars, polygalacturonase activity (PG) and viscosity reduction. The physical-chemical composition of the residues had different sugar and pectin levels. For the unwashed residue, the peak activity was reached with 40% of initial moisture content, 1% of nitrogen supplementation without phosphorus addition after 30 hours of process. These conditions led to 16 U/g of PG activity and 82% of viscosity reduction. The calculated models reached similar values to the experimental ones in the same process conditions: 15.55 U/g of PG and 79.57% of viscosity eduction. Similarly, the greatest enzyme production for washed residue was reached with 40% initial moisture content, 1% nitrogen supplementation without phosphorus addition after 22 hours of cultivation. In this condition it was obtained polygalacturonase activity of 9.84 U/g and viscosity reduction of 81.36%. These values are close to experimental values that were of 10.1 U/g and 81%, respectively. The conditions that led to the best PG activity results was the agitated one and the best extraction condition was obtained with 100 minutes of solvent/medium contact and RZ of 5 (mL/g)

Secagem de misturas de polpa de frutas tropicais em leito de jorro

Drying of fruit pulps in spouted beds of inert particles has been indicated as a viable technique to produce fruit powders. Most of the processes employed to produce dried fruit pulps and juices, such as Foam Mat, encapsulation by co-crystallization and spray drying utilize adjuvant and additives (such as thickeners, coating materials, emulsifiers, acidulants, flavors and dyes), which is not always desirable. The fruit pulp composition exerts an important effect on the fruit powder production using a spouted bed. In the study by Medeiros (2001) it was concluded that lipids, starch and pectin contents play an important role on the process performance, enhancing the powder production; however, the drying of fruit pulps containing high content of reducing sugars (glucose and fructose) is practically unviable. This work has the objective of expanding the studies on drying of fruit pulps in spouted bed with aid of adjuvant (lipids, starch and pectin) aiming to enhance the dryer performance without jeopardizing the sensorial quality of the product. The optimum composition obtained by Medeiros (2001) was the basis for preparing the mixtures of pulps. The mixture formulations included pulps of mango (Mangifera indica), umbu (Spondias tuberosa) and red mombin (Spondia purpurea) with addition of cornstarch, pectin and lipids. Different products were used as lipids source: olive and Brazil nut oils, coconut milk, heavy milk, powder of palm fat and palm olein. First of all, experiments were conducted to define the best formulation of the fruit pulps mixture. This definition was based on the drying performance obtained for each mixture and on the sensorial characteristics of the dry powder. The mixture formulations were submitted to drying at fixed operating conditions of drying and atomizing air flow rate, load of inert particles, temperature and flow rate of the mixture. The best results were obtained with the compositions having powder of palm fat and palm olein in terms of the drying performance and sensorial analysis. Physical and physicochemical characteristics were determined for the dry powders obtained from the mixtures formulations. Solubility and reconstitution time as well as the properties of the product after reconstitution were also evaluated. According to these analyses, the powder from the mixtures formulations presented similar characteristics and compatible quality to those produced in other types of dryers. Considering that the palm olein is produced in Brazil and that it has been used in the food industry substituting the palm fat powder, further studies on drying performance were conducted with the composition that included the palm olein. A complete factorial design of experiments 23, with three repetitions at the central point was conducted to evaluate the effects of the air temperature, feeding flow rate and intermittence time on the responses related to the process performance (powder collection efficiency, material retained in the bed and angle of repose of the inert particles after the process) and to the product quality (mean moisture content, loss of vitamin C and solubility). Powder production was uniform for the majority of the experiments and the higher efficiency with lower retention in the bed (59.2% and 1.8g, respectively) were obtained for the air temperature of 80°C, mixture feed rate of 5ml/min in intervals of 10 min. The statistical analysis of the results showed that the process variables had individual or combined significant influences on the powder collection efficiency, material retention in the bed, powder moisture content and loss of vitamin C. At the experimental ranges of this work, the angle of repose and solubility were not influenced by the operating variables. From the results of the experimental design, statistical models were obtained for the powder moisture content and loss of vitamin C

Secagem de misturas de polpa de frutas tropicais em leito de jorro

Drying of fruit pulps in spouted beds of inert particles has been indicated as a viable technique to produce fruit powders. Most of the processes employed to produce dried fruit pulps and juices, such as Foam Mat, encapsulation by co-crystallization and spray drying utilize adjuvant and additives (such as thickeners, coating materials, emulsifiers, acidulants, flavors and dyes), which is not always desirable. The fruit pulp composition exerts an important effect on the fruit powder production using a spouted bed. In the study by Medeiros (2001) it was concluded that lipids, starch and pectin contents play an important role on the process performance, enhancing the powder production; however, the drying of fruit pulps containing high content of reducing sugars (glucose and fructose) is practically unviable. This work has the objective of expanding the studies on drying of fruit pulps in spouted bed with aid of adjuvant (lipids, starch and pectin) aiming to enhance the dryer performance without jeopardizing the sensorial quality of the product. The optimum composition obtained by Medeiros (2001) was the basis for preparing the mixtures of pulps. The mixture formulations included pulps of mango (Mangifera indica), umbu (Spondias tuberosa) and red mombin (Spondia purpurea) with addition of cornstarch, pectin and lipids. Different products were used as lipids source: olive and Brazil nut oils, coconut milk, heavy milk, powder of palm fat and palm olein. First of all, experiments were conducted to define the best formulation of the fruit pulps mixture. This definition was based on the drying performance obtained for each mixture and on the sensorial characteristics of the dry powder. The mixture formulations were submitted to drying at fixed operating conditions of drying and atomizing air flow rate, load of inert particles, temperature and flow rate of the mixture. The best results were obtained with the compositions having powder of palm fat and palm olein in terms of the drying performance and sensorial analysis. Physical and physicochemical characteristics were determined for the dry powders obtained from the mixtures formulations. Solubility and reconstitution time as well as the properties of the product after reconstitution were also evaluated. According to these analyses, the powder from the mixtures formulations presented similar characteristics and compatible quality to those produced in other types of dryers. Considering that the palm olein is produced in Brazil and that it has been used in the food industry substituting the palm fat powder, further studies on drying performance were conducted with the composition that included the palm olein. A complete factorial design of experiments 23, with three repetitions at the central point was conducted to evaluate the effects of the air temperature, feeding flow rate and intermittence time on the responses related to the process performance (powder collection efficiency, material retained in the bed and angle of repose of the inert particles after the process) and to the product quality (mean moisture content, loss of vitamin C and solubility). Powder production was uniform for the majority of the experiments and the higher efficiency with lower retention in the bed (59.2% and 1.8g, respectively) were obtained for the air temperature of 80°C, mixture feed rate of 5ml/min in intervals of 10 min. The statistical analysis of the results showed that the process variables had individual or combined significant influences on the powder collection efficiency, material retention in the bed, powder moisture content and loss of vitamin C. At the experimental ranges of this work, the angle of repose and solubility were not influenced by the operating variables. From the results of the experimental design, statistical models were obtained for the powder moisture content and loss of vitamin C

Desenvolvimento de bionanocompósitos: nano e microcristais de celulose com poli (álcool vinílico) e poli (ácido lático)

This work has the main objective to obtain nano and microcrystals of cellulose, extracted from the pineapple leaf fibres (PALF), as reinforcement for the manufacture of biocomposite films with polymeric matrices of Poly(vinyl alcohol) (PVA) and Poly(lactic acid) (PLA). The polymer matrices and the nano and microcrystals of cellulose were characterised by means of TGA, FTIR and DSC. The analysis was performed on the pineapple leaves to identify the macro and micronutrients. The fibers of the leaves of the pineapple were extracted in a desfibradeira mechanical. The PALF extracted were washed to remove washable impurities and subsequently treated with sodium hydroxide (NaOH) and sodium hypochlorite (NaClO) in the removal of impurities, such as fat, grease, pectates, pectin and lignin. The processed PALF fibers were hydrolysed in sulfuric acid (H2SO4) at a concentration of 13.5 %, to obtain nano and microcrystals of cellulose. In the manufacture of biocomposite films, concentrations of cellulose, 0 %, 1 %, 3 %, 6 %, 9% and 12% were used as reinforcement to the matrices of PVA and PLA. The PVA was dissolved in distilled water at 80 ± 5 oC and the PLA was dissolved in dichloromethane at room temperature. The manufacture of biocompósitos in the form of films was carried out by "casting". Tests were carried out to study the water absorption by the films and mechanical test of resistance to traction according to ASTM D638-10 with a velocity of 50 mm/min.. Chi-square statistical test was used to check for the existence of significant differences in the level of 0.05: the lengths of the PALF, lengths of the nano and microcrystals of cellulose and the procedures used for the filtration using filter syringe of 0.2 μm or filtration and centrifugation. The hydrophilicity of biocompósitos was analysed by measuring the contact angle and the thickness of biocompósitos were compared as well as the results of tests of traction. Statistical T test - Student was also applied with the significance level (0.05). In biodegradation, Sturm test of standard D5209 was used. Nano and microcrystals of cellulose with lengths ranging from 7.33 nm to 186.17 nm were found. The PVA films showed average thicknesses of 0.153 μm and PLA 0.210 μm. There is a strong linear correlation directly proportional between the traction of the films of PVA and the concentration of cellulose in the films (composite) (0,7336), while the thickness of the film was correlated in 0.1404. Nano and microcrystals of cellulose and thickness together, correlated to 0.8740. While the correlation between the cellulose content and tensile strength was weak and inversely proportional (- 0,0057) and thickness in -0.2602, totaling -0,2659 in PLA films. This can be attributed to the nano and microcrystals of cellulose not fully adsorbed to the PLA matrix. In the comparison of the results of the traction of the two polymer matrices, the nano and microcrystals have helped in reducing the traction of the films (composite) of PLA. There was still the degradation of the film of PVA, within a period of 20 days, which was not seen in the PLA film, on the other hand, the observations made in the literature, the average time to start the degradation is above 60 days. What can be said that the films are biodegradable composites, with hydrophilicity and the nano and microcrystals of cellulose, contribute positively in the improvement of the results of polymer matrices used.