Twin-screw extrusion impact on natural fibre morphology and material properties in poly(lactic acid) based biocomposites

Natural fibres from miscanthus and bamboo were added to poly(lactic acid) by twin-screw extrusion. The influence of extruder screw speed and of total feeding rate was studied first on fibre morphology and then on mechanical and thermal properties of injected biocomposites. Increasing the screw speed from 100 to 300 rpm such as increasing the feeding rate in the same time up to 40 kg/h helped to preserve fibre length. Indeed, if shear rate was increased with higher screw speeds, residence time in the extruder and blend viscosity were reduced. However, such conditions doubled electrical energy spent by produced matter weight without significant effect on material properties. The comparison of four bamboo grades with various fibre sizes enlightened that fibre breakages were more consequent when longer fibres were added in the extruder. Longer fibres were beneficial for material mechanical properties by increasing flexural strength, while short fibres restrained material deformation under heat by promoting crystallinity and hindering more chain mobility

Thermo-mechanical processing of sugar beet pulp. I. Twin-screw extrusion process

Sugar beet pulp (SBP) is the raffinate of sugar extraction. Composed of empty vegetal cells, three quarters of it consist of polysaccharides. As it is cheap and produced in great quantities SBP is a potential raw material for industrial applications other than cattle feeding. Twin-screw extrusion modified its structure and destructuring level depended on the specific mechanical energy provided (SME). By gradually increasing this energy, the rate of soluble matter increased, cell structure was progressively destroyed and SBP rheological behaviour was modified. For an SME of 745 W h kg-1, SBP examined through a scanning electron microscope showed a structure similar to that of a composite formed by a continued matrix consisting mainly of pectin and hemicelluloses filled with cellulose microfibres. Plasticized SBP was then formed by injection-molding. Thus treated, SBP becomes a cheap alternative to the use of thermoplastic starch for the production of biodegradable materials

Thermo-mechanical processing of sugar beet pulp. II. Thermal and rheological properties of thermoplastic SBP

Thermoplastic properties of extruded sugar beet pulp (SBP) are closely linked to water–polymer relationships. DSC analyses of water evaporation, water fusion and biopolymer relaxation according to SBP moisture content gave a more accurate estimation of SBP hydration steps than classical water adsorption isotherm. Three moisture contents (8%, 26%, 41% db) were then defined as limits of the different hydration behaviours. Melt viscosity measurements of SBP showed its shear thinning behaviour and the measured apparent viscosity is in the same range as thermoplastic starch viscosity. Using only water as plasticizer, to one temperature corresponded one moisture content to reach the optimal flowing properties: 110°C/35%, 120°C/25% and 130°C/20%. This "plasticization" temperature has been estimated through DSC measurements of large amounts of moistened SBP in pressure-resistant pans. This new kind of DSC measurement revealed a new sample mass dependent second order transition between 140 and 180°C, which temperature is linearly linked to the sample mass

Synthesis and properties of composites of starch and chemically modified natural rubber

A means is developed for forming polysaccharide-based composites with useful material properties through use of unmodified and chemically modified natural rubber latex (NRL). Starch was used as a model for polysaccharides. The NRL was modified by grafting with dimethylaminoethyl methacrylate (DMAEMA) to form a latex with cationic water-soluble polymeric “hairs” of polyDMAEMA, which should form hydrogen bonds with starch. Starch solutions, containing 20% glycerol as a film-forming aid, and the modified NRL were mixed and films allowed to form. The unmodified latex acted only as filler in the starch films, but with modified NRL, the mechanical properties of the films were significantly altered. The elastic modulus was greatly decreased and strain at break greatly increased. The glass transition temperature increased from –48°C to –32°C, suggesting significant compatibilization. Freeze-fracture TEM micrographs indicate strong interactions between the surface of the modified NRL and starch. The polyDMAEMA chains are more hydrophilic than the starch, and the addition of grafted latex results in a 20° drop of the water contact angle of the formed film, and a 25% increase of the water absorption compared to the native starch; with unmodified NRL, the opposite effect was observed

Thermo-mechanical processing of sugar beet pulp. III. Study of extruded films improvement with various plasticizers and cross-linkers

Thermoplastic sugar beet pulp (thermo-mechanical processing was discussed in previous studies) was formed into film strips by extrusion. Film tensile properties are discussed according to the molecular structure of external plasticizer. Sorbitol, fructose and adipic acid have a marked antiplasticizing effect, while urea and xylitol gave higher ultimate tensile stress than glycerol for a comparable strain at break. Xylitol can be considered as the best plasticizer with UTS and EL of, respectively, 4.9 MPa and 11.3% and water absorption (85%RH, 25°C) was less than 25%. Glycidyl methacrylate was directly used in the extrusion process as cross-linker. In high humidity atmosphere (97%RH, 25°C), film water absorption was then kept under 40% while the tensile properties were improved of 50% and with a 30 minute UV post-treatment the mass gain in absorption was even less than 30% after 5 days

Solid–liquid transport in a modified co-rotating twin-screw extruder-dynamic simulator and experimental validations

This work presents a dynamic transport model of a solid–liquid media through a twin-screw extruder (TSE). The application under consideration is the solid–liquid extraction of solute from raw plant substrate. Dynamic experiments are performed and compared with the simulated results for step functions on the solid feed rate and on the screw rotating speed. Despite some imperfections, results allow to validate the simulator

Extraction of oil from jatropha seeds using a twin-screw extruder: Feasibility study

The objective of this study was to evaluate the feasibility of mechanical pressing to extract oil from jatropha seeds using a twin-screw extruder. Experiments were conducted using a co-rotating (Clextral BC 21, France) twin-screw extruder. The influence of operating conditions on oil yield, specific mechanical energy and oil quality was examined. Operating conditions included screw configuration, pressing temperature and screw rotation speed. Generally, it was the screw configuration, or profile, that most affected oil extraction efficiency. The best oil yields, a minimum 57.5%, were obtained with a trituration zone composed of 10 monolobe and 10 bilobe paddles, and a pressing zone composed of 50 mm long, reverse pitch screws with a −33 mm pitch. In addition, oil extraction yield increased with decreasing temperature and screw rotation speed. Highest oil extraction yield (70.6%) with good press cake quality (residual oil content lower than 8%) was obtained under operating conditions of 153 rpm screw rotation speed, 5.16 kg/h inlet flow rate of jatropha seeds, and 80 ◦C pressing temperature. The corresponding expressed oil was inexpensive to produce (71 W h/kg seed processed or 314 W h/kg expressed oil for specific mechanical energy) compared with another continuous technique, i.e. the single expeller press, commonly used for mechanical extraction of jatropha oil. Its quality was also satisfactory for biodiesel production. The acid value, the density and the kinematic viscosity were 5.4 mg of KOH/g of oil, 915 kg/m3 and 36.7×10−6m2/s, respectively

Thermo-mechanical behaviour of the raffinate resulting from the aqueous extraction of sunflower whole plant in twin-screw extruder: manufacturing of biodegradable agromaterials by thermo-pressing

Biorefinery of sunflower whole plant can be realized using a twin-screw extruder. Thermo-mechanical fractionation and aqueous extraction are conducted simultaneously. A filter section is outfitted along the barrel to collect continuously an extract and a raffinate (cake meal). Oil yield obtained is 53%. Proteins are partly extracted at the same time, just as pectins and hemicelluloses. Protein yield is 46%. Cake meal is relatively moist (66% for the moisture content). It is first dried to make easier its conservation. It is largely composed of lignocellulosic fibres (59% of the dry matter) from depithed stalk. Lipid content is 13% of the dry matter or 35% of the oil in whole plant. Protein content is 7% of the dry matter or 45% of the proteins in whole plant. DSC measurements indicate that denaturation of proteins is almost complete in the cake meal. DMTA spectrum of its milled powder reveals a significant peak at high temperature (between 175 and 200°C). As already observed with industrial sunflower cake meal, it can be associated with the glass transition of proteins. As a mixture of fibres and proteins, the cake meal can be considered as a natural composite. It is successfully processed into biodegradable and value-added agromaterials by thermo-pressing. As for DMTA analysis, the glass transition of proteins in the cake meal is also observed with PVT analysis at around 180°C. It makes easier the choice of the best thermo-pressing conditions to produce panels with higher mechanical properties in bending. These properties increase simultaneously with temperature, pressure and time chosen for molding operation. The highest flexural strength at break (11.5 MPa) and the highest elastic modulus (2.22 GPa) are obtained for the next molding conditions: 200°C and 320 kgf/cm2 during 60 s. Drop angle measurements show that the corresponding panel is also the most resistant to water. No significant transition is observed inside this panel above 0°C and until 200°C with DMTA analysis. Proteins ensure the agromaterial cohesion without any phase change in this temperature range, and fibres entanglement also acts like reinforcement. This panel could be used as inter-layer sheets for pallets or for the manufacturing of biodegradable containers (composters, crates for vegetable gardening) by assembly of panels

Thermo-pressing of cake meal from sunflower whole plant, one only operation for two actions : expression of residual oil and molding of biodegradable agromaterials

The starting material used in this study was a cake generated during thermo-mechanical fractionation of sunflower (Helianthus annuus L.) whole plant in a Clextral BC 45 (France) twin-screw extruder. It was slightly deoiled (17.6% dry matter for residual oil content), leading to an oil extraction yield of 46.1% (yield based on the residual oil content in cake). As it was a mixture of fibers and proteins, it could be considered as a natural composite that was processed successfully into fiberboards by thermo-pressing. This study aimed to evaluate the influence of thermo-pressing conditions on oil expression yield during molding and on flexural properties of fiberboards manufactured from this cake. An experimental design with three variables was realized: from 250 to 500 kgf/cm² for pressure applied (in 5 levels), from 60 to 300 s for molding time (in 7 levels), and from 600 to 1200 mg/cm² for cake quantity (in 3 levels). Temperature of the aluminium mold positioned between the two plates of the heated hydraulic press (PEI, France) with 400 tons capacity was 200°C. All fiberboards were cohesive. As an internal binder, proteins ensured the agromaterial cohesion, and fibers entanglement also acted like reinforcement. Thermo-pressing was not only a molding operation. It also consisted in increasing the oil extraction efficiency. Oil expression yield during molding increased with the increase of pressure applied, and especially with the increase of molding time. At the same time, it was not so much influenced by the modification of cake quantity. Highest oil expression yield was 58.8% in proportion to the oil that the cake contained, leading to a total oil yield (oil extracted by water in twin-screw extruder, and oil expressed during molding) of 77.8% in proportion to the oil that the sunflower whole plant contained. It was associated with the next thermo-pressing conditions: 469 kgf/cm² for pressure applied, 300 s for molding time, and 697 mg/cm² for cake quantity. Flexural properties of the corresponding fiberboard were 8.1 MPa for flexural strength at break, and 1778 MPa for elastic modulus. Its thickness was 5.40 mm, leading to a mean apparent density of 1.25. Such flexural strength at break was a bit lower (-25%) than the one of the most resistant fiberboard (10.8 MPa), manufactured from the next thermo-pressing conditions: 250 kgf/cm² for pressure applied, 300 s for molding time, and 807 mg/cm² for cake quantity. For such conditions, oil expression yield was 48.0% in proportion to the oil that the cake contained, leading to a total oil yield close (-8%) to the highest yield obtained (71.9% in proportion to the oil that the sunflower whole plant contained instead of 77.8%). Thermo-pressing of cake from sunflower whole plant led to two actions in a single step: the expression of part of residual oil in cake that contributed to the improvement of the oil extraction efficiency, and the molding of biodegradable fiberboards. Their flexural properties were promising. Moreover, because residual oil content in fiberboards was at least 8.0% dry matter, they were not too water-sensitive (i.e. more durable than other thermo-pressed agromaterials). Such fiberboards were value-added agromaterials that may have direct industrial applications. Indeed, they would be potentially usable as inter-layer sheets for pallets, for the manufacturing of biodegradable containers (composters, crates for vegetable gardening), or for their heat insulation properties in building trade

The twin-screw extrusion technology, an original and powerful solution for the biorefinery of sunflower whole plant

The objective of this study was to evaluate the feasibility of an aqueous process for the biorefinery of sunflower whole plant using a twin-screw extruder. Aqueous extraction of oil was chosen as an environment-friendly alternative to the solvent extraction. The extruder was used to carry out three essential unit operations: grinding, liquid/solid extraction, and liquid/solid separation. Wringing out the mixing was effective. However, drying of the cake meal was not optimal. Lixiviation of cotyledon cells was also incomplete. Extraction efficiency depended on operating conditions: screw rotation speed, and input flow rates of whole plant and water. In the best conditions, oil yield was 57%. Residual oil content in the cake meal was 14%. These conditions leaded to the co-extraction of proteins, pectins, and hemicelluloses. The corresponding protein yield was 44%. Oil was extracted in the form of two oil-in-water emulsions. These hydrophobic phases were stabilized by phospholipids and proteins at interface. An aqueous extract containing part of the water-soluble constituents, mainly proteins and pectins, was also generated. As a mixture of fibers and proteins, the cake meal was molded by thermo-pressing. Panels produced had interesting mechanical properties in bending. The obtained fractions may have applications as bases for industrial products