Defining of the microfibrillation of one-step twin-screw-extruded cellulose fibers by its rheological properties (original) (raw)
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Carbohydrate Polymers 240 (2020) 116342, 2020
Twin-screw extrusion (TSE) is a rather recent method to produce cellulose nanofibrils (CNFs) at a high solid content under continuous feeding. Here, never-dried commercial eucalyptus pulp was used as starting material to produce CNFs by TSE after a chemical pretreatment to introduce carboxylic groups via TEMPO-mediated oxidation and carboxymethylation. Five samples with a carboxyl content ranging from 800 to 1300 μmol.g −1 were produced to explore how the carboxyl content affects the aptitude of cellulose fibers to be broken down to nanoscale. The properties of the resulting CNFs in terms of nanosized fraction, morphology and rheological properties were investigated. A critical carboxyl content of 700 μmol.g −1 was a prerequisite for the successful conversion of cellulose fibers into a CNF gel by TSE, regardless the pretreatment method. The degree of swelling of the fibers was put forward to account for this critical parameter.
Cellulose, 2018
The influence of the degree of fibrillation (DoF), i.e. the fibril width distribution, on the rheological properties of microfibrilated cellulose (MFC) suspensions was investigated. To extend the understanding of the dominating effect of either fibril diameter alone or diameter size distribution, flow curves (viscosity against shear rate) and viscoelastic measurements were performed on single, double and ternary component mixtures of medium and highly fibrillated MFCs and pulp fibres across a range of solids content. The data were quantified using classical and recently introduced descriptors, and presented in comprehensive 3D/ternary contour plots to identify qualitative trends. It was found that several rheological properties followed the trends that are generally described in the literature, i.e. that an increasing DoF increases the MFC suspension network strength. It was, however, also found that coarse pulp fibres can have additional effects that cannot be explained by the increased fibril widths alone. It is hypothesised that the increased stiffness (directly caused by the larger fibril width) as well as the reduced mobility of the pulp fibres are additional contributors. The data are discussed in relation to recent findings in the field of rheology and related morphological models of MFC suspension flow behaviour.
Cellulose, 2020
In this work, the defibrillation of cellulose fibers (CF) in the presence of hydroxyethyl cellulose (HEC) within the one-step twin-screw extrusion (TSE) process was examined. The effect of the TSE on cellulose fiber size reduction as well as CF-HEC biocomposites properties were investigated. The results showed that the TSE of cellulose fiber-hydroxyethyl cellulose (CF-HEC) with different cellulose fiber contents (50, 65, and 80 wt%) resulted in partial defibrillation of the cellulose fibers. The fractionation test of the cellulose fibers confirmed that their size was reduced and some fibrillation was observed in microscopy studies. The maximum width reduction of 46% occurred with 80 wt% cellulose content. However, the partial width reduction was also observed with 50% and 65 wt% of cellulose contents. Based on rheological measurements, the shear-viscosity trend of CF-HEC dispersion abruptly dropped when higher fiber content (80 wt%) was extruded, which was related to the fibrillatio...
Cellulose, 2020
Industrial production of low-charge microfibrillated cellulose (MFC) typically results in wide fibril size distributions. This polydispersity influences viscosity, overall colloidal stability, and rheological properties of MFC suspensions and gels in aqueous systems. In this work, a systematic rheological analysis is performed for industrially prepared MFC and fractions of different size distributions. Gel formation and flow characteristics (e.g., shear-thinning) of each fraction are examined under neutral and acidic conditions and compared with the unfractionated MFC suspension. The effects of size, aspect ratio, and surface charge on the rheology of semi-dilute MFC suspensions are discussed. The results demonstrate that particle size and aspect ratio distribution control the viscoelasticity and shear-thinning properties of MFC suspensions. An increased fraction of small diameter nanofibrils, by ex situ addition of the fine particles with high aspect ratio or removal of the coarses...
Morphological, Physical and Thermal Characterization of Microfibrillated Cellulose
Revista Árvore, 2018
The aim of this study was to characterize microfibrillated cellulose (MFC) produced with a Masuko Sangyo Super Masscolloider using bleached and unbleached pulp of Eucalyptus spp. The MFC was characterized regarding morphology (TEM), crystallinity, viscosity, zeta potential and thermal properties (TGA). Regardless of the fiber type, the processing dramatically reduced the dimensions of the material, so as to obtain structures with nanometric dimensions. MFC produced with unbleached pulp preserved the original brown color of the pulp, which may be advantageous for some applications in the packaging sector, while films produced with bleached pulp were more translucent. The MFC showed lower values of viscosity and crystallinity index in relation to cellulosic pulp. The zeta potential was influenced by the type of fiber used. The main thermal transitions in MFC occurred after 200 ºC, demonstrating the potential of this material forhigh-temperature applications.
Cellulose, 2017
Flow curve and viscoelastic measurements were performed on microfibrillated cellulose (MFC) suspensions of different solids content using both cylinder and cup (smooth and rough) as well as vane in cup geometries. To compare the data quantitatively from amplitude sweep measurements and dynamic flow curves several descriptors were newly introduced to parameterize the observed two-zone behaviour separated by a transition region. It was observed that the cylinder cup geometries are prone to erroneous effects like slip, wall depletion and/or shear banding. However, those effects were not observed when the MFC suspension was not stressed beyond the dynamic critical stress (yield) point, i.e. when still in the linear viscoelastic regime. The vane in cup system on the other hand, seems to be less affected by flow inhomogeneities. By following the rheological properties as a function of the MFC suspension solids content, it could be shown that the global property trends remained alike for all investigated measurement systems, despite the presence of erroneous effects in some geometries. The observed effects were linked to recent model hypotheses in respect to the morphology of MFC suspensions under changing shear situations.
BioResources, 2012
Microfibrillated celluloses, liberated from macroscopic lignocellulosic fibers by mechanical means, are sub-fiber elements with lengths in the micron scale and diameters ranging from 10 to a few hundred nanometers. These materials have shown strong water interactions. This article describes an investigation and quantification of the 'hard-toremove (HR) water content' in cellulose fibers and microfibrillated structures prepared from fully bleached softwood pulp (BSW). The fiber/fibril structure was altered by using an extended beating process (up to 300 minutes), and water interactions were determined with isothermal thermogravimetric analysis (TGA). Isothermal TGA is shown to be a convenient and insightful characterization method for fiber-water interactions for fibers and microfibrils at small sample size. In addition, scanning electron microscopic (SEM) images depict the differences between fibers and microfibrils with respect to beating time in the dried consolidated structures. Highly refined pulps with microfibrils were determined to have two critical drying points, i.e., two minima in the second derivative of weight versus time, not before reported in the literature. Also in this study, hard-to-remove (HR) water content is related to the area above the first derivative curve in the constant rate and falling rate drying zones. This measure of HR water correlates with a previous measurement method of HR water but is less ambiguous for materials that lack a constant drying rate zone. Blends of unbeaten fibers and microfibril containing samples were prepared and show potential as composite materials.
Rheological Studies of Microfibrillar Cellulose Water Dispersions
Journal of Polymers and the Environment, 2011
The rheological behaviour of microfibrillar cellulose (MFC) water dispersions has been investigated. For the first time a detailed study of shear dependent viscosity at low and high shear rate is presented. A peculiar time dependent behaviour measured in the area between 0 and 1000 s -1 was identified. The study shows a hysteresis loop in the shear rate-viscosity relationship at low shear rate. Additional time dependent shear rate measurements were performed, and a hypothesis for a mechanism of interaction and formation of a fibrils network was suggested. Higher temperature caused lower viscosity values, and this difference was increased at higher shear rate values. Oscillatory measurements showed how the closeness of the fibrils helps network creations. Data obtained from high shear measurements showed that 1% MFC water dispersions had a dilatant behaviour at ultra high shear rates with values increasing from 120 to 300 Pa s in the area between 180,000 and 330,000 s -1 .
Pipe rheology of microfibrillated cellulose suspensions
Cellulose
The shear rheology of two mechanically manufactured microfibrillated cellulose (MFC) suspensions was studied in a consistency range of 0.2–2.0% with a pipe rheometer combined with ultrasound velocity profiling. The MFC suspensions behaved at all consistencies as shear thinning power law fluids. Despite their significantly different particle size, the viscous behavior of the suspensions was quantitatively similar. For both suspensions, the dependence of yield stress and the consistency index on consistency was a power law with an exponent of 2.4, similar to some pulp suspensions. The dependence of flow index on consistency was also a power law, with an exponent of − 0.36. The slip flow was very strong for both MFCs and contributed up to 95% to the flow rate. When wall shear stress exceeded two times the yield stress, slip flow caused drag reduction with consistencies higher than 0.8%. When inspecting the slip velocities of both suspensions as a function of wall shear stress scaled wi...
Carbohydrate polymers, 2014
The rheological properties of enzymatically hydrolyzed and TEMPO-oxidized microfibrillated/nanofibrillated cellulose (MFC/NFC) aqueous suspensions were investigated in oscillation and steady-flow modes and were compared with the morphology of the studied materials. The flow instabilities, which introduce an error in the rheological measurements, were discovered during flow measurements. A wall-slip (interfacial slippage on the edge of geometry tools and suspension) was detected at low shear rates for two types of NFC suspensions while applying cone-plate geometry. A roughening of the tool surfaces was performed to overcome the aforementioned problem. Applying to TEMPO-oxidized NFC, a stronger suspension response was detected at low shear rates with higher values of measured shear stress. However, a shear banding (localization of shear within a sample volume) became more pronounced. The use of serrated tools for enzymatically hydrolyzed NFC produced lower shear stress at the moderate...