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Cellulose, combined with lignin in some instances, was used to prepare mats made of fibers preferentially oriented in one direction. The aim of this study was evaluating the influence of this polysaccharide on the end properties of the mats when a thermoplastic polymer (in this case recycled polyethylene terephthalate; PET) is used as the primary component of solutions subjected to electrospinning. All of the prepared mats were composed mostly of ultrathin fibers. The mechanical properties were evaluated in the preferred and perpendicular directions of the alignment of the fibers. The storage and elastic moduli, as well as the tensile strength, were higher in the preferred direction. Cellulose led to mats with higher Tg PET values, indicating interactions at the molecular level between the chain segments of both polymers. One of the cellulose mats, (PETC-2), showed a superior alignment index (AI = 0.72 ± 0.03) and a higher average preferred orientation (APO = 88 ± 1°), which, in turn, led to higher mechanical properties, storage modulus, tensile strength, and elastic modulus when evaluated in the preferred direction of fiber alignment (PETC-2 dir), compared to the others. The results reveal that cellulose can be used to tune various properties of mats based on thermoplastics, thereby significantly increasing the range of applications of these materials.

Blend solutions of poly(e-caprolactone) (PCL) and N-(2-hydroxy)-propyl-3-trimethylammonium chitosan chloride (QCh) were successfully electrospun. The weight ratio PCL/QCh ranged in the interval 95/5–70/30 while two QCh samples were used, namely QCh1 ( D Q ¯ = 47.3%; D P v ¯ = 2218) and QCh2 ( D Q ¯ = 71.1%; D P v ¯ = 1427). According to the characteristics of QCh derivative and to the QCh content on the resulting PCL/QCh nonwoven, the nanofibers displayed different average diameter (175 nm–415 nm), and the nonwovens exhibited variable porosity (57.0%–81.6%), swelling capacity (175%–425%) and water vapor transmission rate (1600 g m−2 24 h–2500 g m−2 24 h). The surface hydrophilicity of nonwovens increases with increasing QCh content, favoring fibroblast (HDFn) adhesion and spreading. Tensile tests revealed that the nonwovens present a good balance between elasticity and strength under both dry and hydrated state. Results indicate that the PCL/QCh electrospun nonwovens are new nanofibers-based biomaterials potentially useful as wound dressings.

Brazil has played a leading role in the global cultivation of sugarcane, used in the production of sugar and ethanol, which results in sugarcane bagasse as agrowaste. This agroresidue generates electricity and second-generation ethanol, but the colossal amount available allows for alternative applications. Currently, mechanized harvesting/unburn predominates over manual harvesting/burn. The present study was conducted in this scenario and investigated the use of fibers from unburned sugarcane bagasse (SBU) in bio-based composites. Phenolic thermoset was chosen as a matrix due to its excellent properties. The mechanization/unburn method allows the use of variable length fibers (this study: 1/3/5 cm, 30 wt%). SBU was characterized in detail, highlighting the characterization via inverse gas chromatography (IGC, which provides information regarding the polarity of the groups present on the surface of the fibers). Briefly, the composition of SBU shows no significant differences compared to burnt bagasse (SBB), and IGC showed that SBU has more polar groups on the surface than SBB, which favors intermolecular interactions and then adhesion with the phenolic matrix. Composites reinforced with 3- and 5-cm fibers presented a storage modulus higher than that of the unreinforced thermoset, and the impact strength of all composites was higher than that of the thermoset (up to 45%). This set of results points to applications such as rigid packaging, non-structural parts of buildings and automotive vehicles, which increases the applications of the investigated agrowaste within the circular bioeconomy.

Electrospun nanofibers obtained from cellulose acetate before (CA) and after (DCA) deacetylation were used as electrolyte membranes in dye-sensitized solar cells. As holders of the active components of the device and compared to the reference system, the CA and DCA membranes increased the average device efficiency by as much as 14%. The membranes enhanced the charge transfer at the counter electrode (assessed by the Ohmic and charge transfer resistance and corresponding Helmholtz capacitance). Simultaneously, the photoelectrode did not interfere with the performance as measured by the short-circuit current density, open circuit voltage, fill factor and conversion efficiency. Long-term stability tests (light soaking) showed that the CA- and DCA-based solar cells sustain operation for at least 500 h. For long term use and/or to serve as a scaffold for other purposes, DCA performs better than CA. The proposed active electrolyte membranes are expected to open the way toward rapid and continuous assembly of dye sensitize solar cells using cellulose esters. Graphical abstract: [Figure not available: see fulltext.].

Interest in the use of renewable raw materials in the preparation of materials has been growing uninterruptedly in recent decades. The aim of this strategy is to offer alternatives to the use of fossil fuel-based raw materials and to meet the demand for materials that are less detrimental to the environment after disposal. In this context, several studies have been carried out on the use of lignocellulosic biomass and its main components (cellulose, hemicelluloses, and lignin) as raw materials for polymeric materials. Lignocellulosic fibers have a high content of cellulose, but there has been a notable lack of investigations on application of the electrospinning technique for solutions prepared from raw lignocellulosic biomass, even though the presence of cellulose favors the alignment of the fiber chains during electrospinning. In this investigation, ultrathin (submicrometric) and nanoscale aligned fibers were successfully prepared via electrospinning (room temperature) of solutions prepared with different contents of lignocellulosic sisal fibers combined with recycled poly(ethylene terephthalate) (PET) using trifluoroacetic acid (TFA) as solvent. The “macro” fibers were deconstructed by the action of TFA, resulting in solutions containing their constituents, i.e., cellulose, hemicelluloses, and lignin, in addition to PET. The “macro” sisal fibers were reconstructed at the nanometer and submicrometric scale from these solutions. The SEM micrographs of the mats containing the components of sisal showed distinct fiber networks, likely due to differences in the solubility of these components in TFA and in their dielectric constants. The mechanical properties of the mats (dynamic mechanical analysis, DMA, and tensile properties) were evaluated with the samples positioned both in the direction (dir) of and in opposition (op) to the alignment of the nano and ultrathin fibers, which can be considered a novelty in the analysis of this type of material. DMA showed superior values of storage modulus (E’ at 30 °C) for the mats characterized in the preferential direction of fiber alignment. For example, for mats obtained from solutions prepared from a 0.4 ratio of sisal fibers/PET, Sisal/PET0.40dir presented a high E’ value of 765 MPa compared to Sisal/PET0.40op that presented an E’ value of 88.4 MPa. The fiber alignment did not influence the Tg values (from tan δ peak) of electrospun mats with the same compositions, as they presented similar values for this property. The tensile properties of the electrospun mats were significantly impacted by the alignment of the fibers: e.g., Sisal/PET0.40dir presented a high tensile strength value of 15.72 MPa, and Sisal/PET0.40op presented a value of approximately 2.5 MPa. An opposite trend was observed regarding the values of elongation at break for these materials. Other properties of the mats are also discussed; such as the index of fiber alignment, average porosity, and surface contact angle. To our knowledge, this is the first time that the influence of fiber alignment on the properties of electrospun mats based on untreated lignocellulosic biomass combined with a recycled polymer, such as PET, has been evaluated. The mats obtained in this study have potential for diversified applications, such as reinforcement for polymeric matrices in nanocomposites, membranes for filtration, and support for enzymes, wherein the fiber alignment, together with other evaluated properties, can impact their effectiveness in these applications.

Cellulose nanocrystals (CNC) were prepared from curaua fibers via acid hydrolysis, and used as reinforcing phase for high-density biopolyethylene (HDBPE) or green polyethylene. Castor oil (CO), epoxidized soybean oil (ESO) and epoxidized linseed oil (ELO) were chosen as compatibilizers for this study. Nanocomposites reinforced with CNC (3, 6, and 9 wt %) were processed by extrusion, using CO (3, 6, and 9 wt %) to evaluate its action as CNC dispersing agent in the HDBPE matrix. From the results obtained for these films, the CNC and oil contents were set at 3 wt%. In addition to CO, ELO, and ESO were also used, and besides processing by extrusion, extrusion/hot-pressing process was also considered, in order to compare the two processing techniques. The nanocomposites were characterized by microscopic, thermal, mechanical, and rheological analyses. The presence of oil leads to less opaque films and improved dispersion. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2015, 53, 1010–1019

Enzymatic saccharification of sisal cellulosic pulp has been investigated. Brazil leads global production of lignocellulosic sisal fiber, which has high cellulose content, an important property for producing glucose via saccharification. Hence, sisal pulp can be a good alternative for use in biorefineries. Prior to enzymatic hydrolysis, the starting pulp [85 ± 2% α-cellulose, 15 ± 2% hemicelluloses, 1.2 ± 2% insoluble lignin, viscometric average molar mass (MMvis) 19,357 ± 590 g mol−1, crystallinity index (CI) 74%] was pretreated with alkaline aqueous solution (mercerization, 20 g of pulp L−1, 20% NaOH, 50 °C). The changes in the properties of the cellulosic pulp during this pretreatment were analyzed [α-cellulose content, MMvis, CI, pulp fiber dimensions, and scanning electron microscopy (SEM)]. The unmercerized and mercerized (97.4 ± 2% α-cellulose, 2.6 ± 2% hemicelluloses, 0.3 ± 0.1% insoluble lignin, MMvis 94,618 ± 300 g mol−1, CI 68%) pulps were subjected to enzymatic hydrolysis (48 h, commercial cellulase enzymes, 0.5 mL g−1 pulp); during the reactions, aliquots consisting of unreacted pulp and liquor were withdrawn from the medium at certain times and characterized (unreacted pulp: MMvis, CI, fiber dimensions, SEM; liquor: high-performance liquid chromatography). The changes in pulp properties observed during mercerization facilitated access of enzymes to cellulose chains, and the yield of the hydrolysis reaction increased from 50.2 (unmercerized pulp) to 89.0% (mercerized pulp). These initial results for enzymatic hydrolysis of sisal pulp indicate that it represents a good alternative biomass for bioethanol production.

Bio-based films were prepared from LiCl/DMAc solutions containing sisal cellulose esters (acetates, butyrates and hexanoates) with different degrees of substitution (DS 0.7–1.8) and solutions prepared with the cellulose esters and 20 wt% sisal cellulose. A novel approach for characterizing the surface morphology utilized field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and contact angle analysis. XPS and ToF-SIMS were a powerful combination while investigating both the ester group distribution on the surface and effects of cellulose content on the film. The surface coverage by ester aliphatic chains was estimated using XPS measurements. Fibrous structures were observed in the FE-SEM images of the cellulose and bio-based films, most likely because the sisal cellulose chains aggregated during dissolution in LiCl/DMAc. Therefore, the cellulose aggregates remained after the formation of the films and removal of the solvent. The XPS results indicated that the cellulose loading on the longer chain cellulose esters films (DS 1.8) increased the surface coverage by ester aliphatic chains (8.2 % for butyrate and 45 % for hexanoate). However, for the shortest ester chains, the surface coverage decreased (acetate, 42 %). The ToF-SIMS analyses of cellulose acetate and cellulose hexanoate films (DS 1.8) revealed that the cellulose ester groups were evenly distributed across the surface of the films.

The aim of this study was to evaluate the influence of cellulose and/or lignin on the properties of mats prepared from dissolution (for 48 h or 72 h, solvent: trifluoroacetic acid) of recycled poly (ethylene terephthalate) (PET). Briefly, the presence of cellulose led to a tendency of higher average fiber diameter and average pore area as well as lower average porosity compared to the neat mat (PETref, 242 ± 59 nm, 9.6 ± 1.1 104 nm2 and 19.0 ± 1.1%, respectively). The Tg values for electrospun PET combined with cellulose and/or lignin were higher than that of PETref (92.5 ± 0.1 °C), and the tensile strength increased with the cellulose and/or lignin loading. In addition, the presence of lignin (72 h of dissolution) led to a mat with an elongation at break of 149 ± 9% compared to 14 ± 2% for PETref. The results indicated that the properties of mats based on PET can be tuned by adding cellulose and/or lignin to solutions posteriorly electrospun as well as by varying the dissolution time.

The use of products and byproducts from the agro-industry and forest biorefinery is essential for the development of value-added and low environmental-impact materials. In this study, polyurethanes were prepared using sodium lignosulfonate (NaLS) and castor oil (CO) as reagents and were used to prepare composites reinforced with lignocellulosic fibers, namely, curaua and coir fibers (30 wt %, 3 cm length, and randomly oriented). The SEM images of fractured surfaces of the composites revealed excellent adhesion at the fiber/matrix interface of both coir and curaua composites, which probably resulted from the favorable interactions between polar groups, as well as amid low polarity domains that are present in both the matrix and the reinforcements. The composites exhibited different impact/flexural and strength/flexural moduli (NaLS/CO/Curaua = 465 Jm−1/44 MPa/2 GPa; NaLS/CO/Coir = 180 Jm−1/25 MPa/1 GPa). The higher tensile strength/aspect ratio of the curaua fibers (485 MPa/259) compared with that of the coir fibers (120 MPa/130) most likely contributes to the enhanced performance of its composite. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013

Composites of high-density biopolyethylene (HDBPE) obtained from ethylene derived from sugarcane ethanol and curaua fibers were formed by first mixing in an internal mixer followed by thermopressing. Additionally, hydroxyl-terminated polybutadiene (LHPB), which is usually used as an impact modifier, was mainly used in this study as a compatibilizer agent. The fibers, HDBPE and LHPB were also compounded using an inter-meshing twin-screw extruder and, subsequently, injection molded. The presence of the curaua fibers enhanced some of the properties of the HDBPE, such as its flexural strength and storage modulus. SEM images showed that the addition of LHPB improved the adhesion of the fiber/matrix at the interface, which increased the impact strength of the composite. The higher shear experienced during processing probably led to a more homogeneous distribution of fibers, making the composite that was prepared through extruder/injection molding more resistant to impact than the composite processed by the internal mixer/thermopressing.

The present work is inserted into the broad context of the upgrading of lignocellulosic fibers. Sisal was chosen in the present study because more than 50% of the world’s sisal is cultivated in Brazil, it has a short life cycle and its fiber has a high cellulose content. Specifically, in the present study, the subject addressed was the hydrolysis of the sisal pulp, using sulfuric acid as the catalyst. To assess the influence of parameters such as the concentration of the sulfuric acid and the temperature during this process, the pulp was hydrolyzed with various concentrations of sulfuric acid (30–50%) at 70 °C and with 30% acid (v/v) at various temperatures (60–100 °C). During hydrolysis, aliquots were withdrawn from the reaction media, and the solid (non-hydrolyzed pulp) was separated from the liquid (liquor) by filtering each aliquot. The sugar composition of the liquor was analyzed by HPLC, and the non-hydrolyzed pulps were characterized by viscometry (average molar mass), and X-ray diffraction (crystallinity). The results support the following conclusions: acid hydrolysis using 30% H2SO4 at 100 °C can produce sisal microcrystalline cellulose and the conditions that led to the largest glucose yield and lowest decomposition rate were 50% H2SO4 at 70 °C. In summary, the study of sisal pulp hydrolysis using concentrated acid showed that certain conditions are suitable for high recovery of xylose and good yield of glucose. Moreover, the unreacted cellulose can be targeted for different applications in bio-based materials. A kinetic study based on the glucose yield was performed for all reaction conditions using the kinetic model proposed by Saeman. The results showed that the model adjusted to all 30–35% H2SO4 reactions but not to greater concentrations of sulfuric acid. The present study is part of an ongoing research program, and the results reported here will be used as a comparison against the results obtained when using treated sisal pulp as the starting material.

In this work, composites based on a phenolic matrix and untreated- and treated sisal fibers were prepared. The treated sisal fibers used were those reacted with NaOH 2% solution and esterified using benzophenonetetracarboxylic dianhydride (BTDA). These treated fibers were modified with the objective of improving the adhesion of the fiber-matrix interface, which in turn influences the properties of the composites. BTDA was chosen as the esterifying agent to take advantage of the possibility of introducing the polar and aromatic groups that are also present in the matrix structure into the surface of the fiber, which could then intensify the interactions occurring in the fiber-matrix interface. The fibers were then analyzed by SEM and FTIR to ascertain their chemical composition. The results showed that the fibers had been successfully modified. The composites (reinforced with 15%, w/w of 3.0 cm length sisal fiber randomly distributed) were characterized by SEM, impact strength, and water absorption capacity. In the tests conducted, the response of the composites was affected both by properties of the matrix and the fibers, besides the interfacial properties of the fiber-matrix. Overall, the results showed that the fiber treatment resulted in a composite that was less hygroscopic although with somewhat lower impact strength, when compared with the composite reinforced with untreated sisal fibers.

The (bio)degradation of polyolefins can be accelerated by modifying the level of crystallinity or by incorporation of carbonyl groups by adding pro-oxidants to masterbatches or through exposure to ultraviolet irradiation. In this work, we sought to improve the degradation of PP by adding cobalt, calcium or magnesium stearate to Ecoflex ® , PP or Ecoflex ® /PP blends. The effect of the pro-oxidants on biodegradability was assessed by examining the mechanical properties and fluidity of the polymers. PP had higher values for tensile strength at break and Young's modulus than Ecoflex ® , and the latter had little influence on the properties of PP in Ecoflex ® /PP blends. However, the presence of pro-oxidants (except for calcium) reduced these properties. All of the pro-oxidants enhanced the fluidity of PP, a phenomenon that facilitated polymer degradation at high temperatures.

Thermoset phenolic composites reinforced with sisal fibers were prepared to optimize the cure step. In the present study, processing parameters such as pressure, temperature, and time interval were varied to control the vaporization of the water generated as a byproduct during the crosslinking reaction. These molecules can vaporize forming voids, which in turn affect the final material properties. The set of results on impact strength revealed that the application of higher pressure before the gel point of the phenolic matrix produced composites with better properties. The SEM images showed that the cure cycle corresponding to the application of higher values of molding pressure at the gel point of the phenolic resin led to the reduction of voids in the matrix. In addition, the increase in the molding pressure during the cure step increased the resin interdiffusion. Better filling of the fiber channels decreased the possibility of water molecules diffusing through the internal spaces of the fibers. These molecules then diffused mainly through the bulk of the thermoset matrix, which led to a decrease in the water diffusion coefficient (D) at all three temperatures (25, 55 and 70 °C) considered in the experiments.

Curaua fibers were treated with ionized air to improve the fiber/phenolic matrix adhesion. The treatment with ionized air did not change the thermal stability of the fibers. The impact strength increased with increase in the fiber treatment time. SEM micrographs of the fibers showed that the ionized air treatment led to separation of the fiber bundles. Treatment for 12h also caused a partial degradation of the fibers, which prompted the matrix to transfer the load to a poorer reinforcing agent during impact, thereby decreasing the impact strength of the related composite. The composites reinforced with fibers treated with ionized air absorbed less water than those reinforced with untreated fibers.

Sisal fibers have been chemically modified by reaction with lignins, extracted from sugarcane bagasse and Pinus-type wood and then hydroxymethylated, to increase adhesion in resol-type phenolic thermoset matrices. Inverse gas chromatography (IGC) results showed that acidic sites predominate for unmodified/modified sisal fibers and for phenolic thermoset, indicating that the phenolic matrix has properties that favor the interaction with sisal fibers. The IGC results also showed that the phenolic thermoset has a dispersive component closer to those of the modified fibers suggesting that thermoset interactions with the less polar modified fibers are favored. Surface SEM images of the modified fibers showed that the fiber bundle deaggregation increased after the treatment, making the interfibrillar structure less dense in comparison with that of unmodified fibers, which increased the contact area and encouraged microbial biodegradation in simulated soil. Water diffusion was observed to be faster for composites reinforced with modified fibers, since the phenolic resin penetrated better into modified fibers, thereby blocking water passage through their channels. Overall, composites' properties showed that modified fibers promote a significant reduction in the hydrophilic character, and consequently of the reinforced composite without a major effect on impact strength and with increased storage modulus.

Resol type resins were prepared in alkaline conditions (potassium hydroxide or potassium carbonate) using furfural obtained by acid hydrolysis of abundant renewable resources from agricultural and forestry waste residues. The structures of the resins were fully determined by 1H, 13C, and 2D NMR spectrometries with the help of four models compounds synthesized specially for this study. MALDI-Tof mass spectrometry experiments indicated that a majority of linear oligomers and a minority of cyclic ones constituted them. Composites were prepared with furfural–phenol resins and sisal fibers. These fibers were chosen mainly because they came from natural lignocellulosic material and they presented excellent mechanical properties. Thermal analyses (dTG and DSC) and electron microscopy images indicated that the composites displayed excellent adhesion between resin and fibers. Impact strength measurement showed that mild conditions were more suitable to prepare thermosets. Nevertheless, mild conditions induced a high-diffusion coefficient for water absorption by composites. Composites with good properties could be prepared using high proportion of materials obtained from biomass without formaldehyde. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008

The question posed in the title has been addressed by studying the swelling of celluloses at 20 °C by twenty protic solvents, including water; linear- and branched-chain aliphatic alcohols; unsaturated aliphatic alcohols, and alkoxyalcohols. The biopolymers investigated included microcrystalline cellulose, MC, native and never-dried mercerized cotton cellulose, cotton and M-cotton, and native and never-dried mercerized eucalyptus cellulose, eucalyptus and M-eucalyptus, respectively. In most cases, better correlations with the physico-chemical properties of the solvents were obtained when the swelling was expressed as number of moles of solvent/anhydroglucose unit, nSw, rather than as % increase in sample weight. The descriptors employed in these correlations included, where available, Hildebrand’s solubility parameters, Gutmann’s acceptor and donor numbers, solvent molar volume, VS, as well as solvatochromic parameters. The latter, employed for the first time for correlating the swelling of biopolymers, included empirical solvent polarity, ET(30), solvent “acidity”, αS, “basicity”, βS, and dipolarity/polarizability, π S * , respectively. Small regression coefficients and large sums of the squares of the residues were obtained when values of nSw were correlated with two solvent parameters. Much better correlations were obtained with three solvent parameters. The most statistically significant descriptor in the correlation equation depends on the cellulose, being π S * for MC, cotton, and eucalyptus, and VS for M-cotton and M-eucalyptus. The best correlations were obtained with the same set of four parameters for all celluloses, namely, solvent pKa (or αS) βS, π S * , and VS, respectively. These results indicate that the supra-molecular structure of the biopolymer, in particular the average sizes of crystallites and micro-pores, and the presence of its chains in parallel (cellulose I) or anti-parallel (cellulose II) arrangements control its swelling. At least for the present biopolymer/solvent systems, use of solvatochromic parameters is a superior alternative to Hildebrand’s solubility parameters and/or Gutmann’s acceptor and donor numbers. The relevance of these results to the accessibility of the hydroxyl groups of cellulose, hence to its reactivity, is briefly discussed.

Fiberboards were prepared using phenolic type resins (phenol-formaldehyde) and sugarcane bagasse fibers. Lignin extracted through an organosolv process from sugarcane bagasse was used as substitute of phenol in phenolic resins from 40 (lignin-phenol-formaldehyde) to 100 wt.-% (lignin-formaldehyde) substitution. Some of the fibers were chemically modified by oxidation with chlorine dioxide and treatment with furfuryl alcohol (FA), leading to fibers coated with polyfurfuryl alcohol. Thermal analysis (DSC and TGA) of the prepolymers allowed setting up an efficient curing to prepare fiberboards. Impact strength and water absorption were measured showing the importance of the curing pressure to obtain good performance. When chemically modified fibers were used to prepare board samples, enhanced durability against white root fungi is observed, and to a less degree against brown root fungi. Sugarcane bagasse fiberboards were prepared from prepolymers where lignin substituted phenol up to 100%. This replaces these materials in advantageous position, relating to those prepared from phenol-formaldehyde resins, due to their high content of renewable raw materials. The results obtained are promising for the utilization of sugarcane bagasse as raw materials for preparing fiberboards to be used in tropical areas.

This study used infrared spectroscopy to compare the degree of conversion (DC) of Z250 resin composite at different depths, using a variety of light-curing sources. Photo-activation was performed with: plasma arc (PAC) light, a blue light emitting diode (LED) and four different exposure scenarios using quartz–tungsten–halogen (QTH) light. Cured composite cylinders were transversally cut into 300 μm-thick slices corresponding to surface, 1–5 mm depths. Each disc was finely pulverized, incorporated into KBr pellets, and analyzed by FTIR. Results demonstrated that for the surface and depths of 1 and 2 mm, conversion values did not differ significantly between lights or exposure treatments. At 3 and 4 mm depths, the LED source showed significantly higher DC than did the PAC light. All QTH methods were not significantly different to either LED or PAC. At 5 mm, there was no significant difference in DC between methods, except that PAC was not able to cure the composite.

The study and development of polymeric composite materials, especially using lignocellulosic fibers, have received increasing attention. This is interesting from the environmental and economical viewpoints as lignocellulosic fibers are obtained from renewable resources. This work aims to contribute to reduce the dependency on materials from nonrenwable sources, by utilizing natural fibers (sisal) as reinforcing agents and lignin (a polyphenolic macromolecule obtained from lignocellulosic materials) to partially substitute phenol in a phenol-formaldehyde resin. Besides, it was intented to evaluate how modifications applied on sisal fibers influence their properties and those of the composites reinforced with tem, mainly thermal properties. Sisal fibers were modified by either (i) mercerization (NaOh 10%), (ii) esterification (succinic anhydride), or (iii) ionized air treatment (discharge current of 5 mA). Composites were made by mould compression, of various sisal fibers in combination with either phenol-formaldehyde or lignin-phenol-formaldehyde resins. Sisal fibers and composites were characterized by thermogravimetry (TG) and DSC to establish their thermal stability. Scanning electron microscopy (SEM) was used to investigate the morphology of unmodified and modified surface sisal fibers as well as the fractured composites surface. Dynamic mechnical thermoanalysis (DMTA) was used to examine the influence of temperature on the composite mechanical properties. The results obtained for sisal fiber-reinforced phenolic and lignophenolic composites showed that the use of lignin as a partial substitute of phenol in phenolic resins in applications different from the traditional ones, as for instance in other than adhesives is feasible.

Linters cellulose was subjected to different treatments (mercerization and ionized air) before acetylation with acetic anhydride, in homogeneous medium, using DMAc/LiCl as solvent system. Before derivatization, the treated fibres were characterized by Scanning Electron Microscopy, X-ray diffraction, alpha-cellulose content, Inverse Gas Chromatography and viscosimetry. It was shown that except a decrease in the dispersive surface energy, the treatments induced small changes in the cellulose. The degree of acetylation of these fibers was found to follow a linear behavior with the stoichiometry between acetic anhydride and glucose unit, but this linearity obeyed high rate up to a DS of 2.0. The order of reactivity observed for all samples, C6>>C2>C3, confirms the higher reactivity of OH in C6 position, because this group is the least sterically hindered of the anhydroglucose unity.

The cellulose solvent dimethylsulfoxide/tetrabutylammonium fluoride trihydrate (TBAF·3 H2O) was studied as reaction medium for the synthesis of benzyl cellulose (BC) by treating the dissolved polymer with benzyl chloride in the presence of solid NaOH or aqueous NaOH solution. BC samples with degree of substitution (DS) between 0.40 and 2.85 were accessible applying different molar ratios. The studies show that both the TBAF·3 H2O concentration and the molar ratio of the reagents to repeating unit influence the DS. The solubility of the BC synthesized in a different way, however, of comparable DS is different. Structural analyses were carried out by means of FTIR-, 1H- and 13C NMR spectroscopy. SEC measurements revealed polymer aggregation in samples of low DS synthesized in a solvent containing 9.0% TBAF·3 H2O. At higher concentration of TBAF·3 H2O in the solvent, the BC samples obtained do not form aggregates. BC of high DS is crystalline and shows thermotropic liquid crystalline behavior as analyzed by means of DSC. Melting point and degradation temperature are not related to the DS.

This study evaluated the degree of conversion (DC) by FTIR spectroscopy and Knoop hardness (KHN) of Z250 composite, using seven photo-activation methods: continuous light (800 mW/cm 2 −40 s); exponential light (0–800 mW/cm 2 -40 s); intermittent light (2 s-600 mW/cm 2 ; 2 s without light-80 s); stepped light (10 s-150 mW/cm 2 ; 30 s-650 mW/cm 2 ); PAC (1320 mW/cm 2 −3 s); LED1 (100 mW/cm 2 -40 s); LED2 (350 mW/cm 2 −40 s). For FTIR analysis, the specimens were finely pulverized and, after 24±1 h, pressed with KBr and analyzed. For Knoop hardness tests, the specimens were measured on the surface and at 1 and 2 mm depth. The results showed that there was no statistical difference in DC values between the photo-activation methods. The highest Knoop hardness value was obtained for continuous light, followed by stepped, exponential and LED2 with no difference between them. For intermittent light, no difference was observed compared with stepped, exponential LED2 and PAC. The KHN for PAC was lower than those of stepped and exponential light. LED1 demonstrated the lowest KHN, which was statistically different to the other methods.

Composites based on phenolic matrices and unmodified and chemically modified sugar cane bagasse and curaua fibers were prepared. The fibers were oxidized by chlorine dioxide, mainly phenolic syringyl and guaiacyl units of the lignin polymer, followed by grafting furfuryl alcohol (FA), which is a chemical obtained from a renewable source. The fibers were widely characterized by chemical composition analysis, crystallinity, UV−vis diffuse reflectance spectroscopy, SEM, DSC, TG, tensile strength, and 13C CP-MAS NMR. The composites were analyzed by SEM, impact strength, and DMA. The SEM images and DMA results showed that the oxidation of sugar cane bagasse fibers followed by reaction with FA favored the fiber/matrix interaction at the interface. The same chemical modification was less effective for curaua fibers, probably due to its lower lignin content, since the reaction considered touches mainly the lignin moiety. The tensile strength results obtained showed that the fibers were partially degraded by the c...

The new cellulose solvent dimethyl sulfoxide (DMSO)/tetrabutylammonium fluoride (TBAF) was applied as reaction medium for the carboxymethylation of mercerized cellulose from sisal and cotton linters. The reaction parameters studied were the molar ratio of reagent and NaOH to anhydroglucose unit (AGU) and the addition of the NaOH either as an aqueous solution or as solid particles. Size Exclusion Chromatography results (SEC) indicated that the dissolution medium and/or derivatizing method used in the present work causes a certain depolymerization on the cellulose chains The pattern of substitution within the AGU and along the polymer chains of the carboxymethylcellulose (CMC), which was analyzed by 1H NMR spectroscopy and HPLC after acidic depolymerization of the CMC, is in the order O-6>O-2≥O-3. With regard to the mole fractions of the different repeating units, samples prepared using aqueous NaOH possess a statistic content, while by using solid NaOH a deviation from statistically calculated values was observed. As a consequence of the non-statistics, the solubility in water of these samples starts at a DS 0.85, while conventionally prepared CMC are water-soluble at a DS as low as 0.4.

Sugar cane bagasse and curaua acidolysis lignins were used to get a better understanding of the mechanism involved in a new chemical modification of sugar cane bagasse and curaua fibres, consisting in a selective oxidation of lignin by chlorine dioxide and reacting some of the created unsaturated units (quinones or muconic derivatives) with furfuryl alcohol (FA). The objective of the treatment was to create a fibre coating increasing compatibility between fibres and phenolic resins in composites. The lignins were reacted with chlorine dioxide to oxidize the phenolic units of the polymer and then treated with furfuryl alcohol. Weight percent gain of 14% and 10% were obtained for sugar cane bagasse and curaua, respectively. 1 H and 31 P NMR, as well as FT-IR results showed that bagasse lignin had more guaiacyl than syringyl units and the reverse for curaua lignin. 1 H NMR of oxidized lignins revealed a decrease of the aromatic and methoxy content after the ClO 2 oxidation, due to partial degradation of the macromolecule. Thermal analysis showed that sugar cane lignin decomposes at lower temperature than curaua lignin, partly due to the high content of condensed structural units present in curaua lignin. Condensed units decompose at higher temperatures than uncondensed ones. The reaction of oxidized lignin with FA shifted the decomposition exotherm to lower temperature for both curaua and sugar cane bagasse lignins, due to the modification introduced into their structures.

A new chemical modification of sugar cane bagasse fibers for phenolic thermoset composites is presented. It consists in creating quinones in the lignin portions of fiber and react them with furfuryl alcohol to create a coating around the fiber more compatible with the phenolic resins used to prepare polymeric matrix. Sodium periodate was used in suitable conditions to oxidize mainly phenolic syringyl and guaiacy units of the lignin polymer to create quinones, which were characterized by UV-visible diffuse reflectance spectroscopy by comparison with model compounds. The reactivity of furfuryl alcohol (FA) with fibers was greatly enhanced after they were oxidized: 13% weight percent gain compared to 2% without oxidation. Chemical analysis of unmodified and FA-modified fibers have shown an important degradation of hemicellulose and a slight one of cellulose which almost maintains its crystallinity. A 25% decrease of strength and length properties of the fibers after FA chemical treatment was measured by dynamic mechanical analysis. The lignin-like proportion of the fiber was greatly enchanced after the FA-treatment. This was confirmed by thermal analysis, DSC, and TGA experiments, on unmodified and FA-modified fibers. SEM analysis of the fibers and of phenolic composites with modified fibers have confirned the FA grafting and shown a better comptability at the interface between the chemically modified fibers and the phenolic matrix. Nevertheless, the chemical treatment of the fibers decreased the impact strength of the composite, which could be caused by the fiber damage suffered during the chemical modification and for the more intense adhesion at the interface, wich in some cases decrease somewhat the impact strength.

Thermoset polymers (phenolic and lignophenolic) are used as matrix materials for polymeric composites. A great deal of effort has been done in order to use vegetal fibers, obtained from sugarcane bagasse and sisal, to reinforce such matrices, because they are readily available and they are renewable resources. Carbon reinforced materials are usually obtained by using high strength carbon fibers for high-tech demanding aerospace and aeronautical uses. Phenolic type resins are commonly used as carbon matrix source for such applications. In this work a reinforced carbon material is obtained by a controlled pyrolysis from lignophenolic matrix/bagasse and lignophenolic/sisal polymeric composites. The ex-vegetable fibers carbon composites were analyzed by flexural tests. The conversion of the vegetable fiber into a carbon fiber takes place in situ all over the matrix material resulting in carbon reinforced materials having a flexural strength as high as 21 MPa and flexural modulus in the range of 11–13...

Lignin, extracted from sugarcane bagasse, was used as a partial substitute of phenol in phenolic closed cells foams. The thermal conductivity of phenolic and lignophenolic thermosets and phenolic and lignophenolic closed cells foams were studied using the hot wire technique, adapted for polymeric materials. Results of other properties—for instance, compression strength, Shore D hardness, closed cells content—are also reported for both foams. The thermal conductivity analyses data showed that the phenolic and lignophenolic thermosets have nearly the same behavior, demonstrating the presence of lignin does not affect this property. Thermal conductivity data obtained for closed cells, phenolic and lignophenolic foams, also showed that, in this case, the presence of lignin does not alter this property in a significant way, that is both foams can be used as thermal insulator materials. Regarding the mechanical properties and others, the data obtained showed that the partial replacement of phenol by li...

Two types of Sisal cellulose were studied as starting material for homogeneous acylation in the solvent dimethyl sulfoxide (DMSO)/tetrabutylammonium fluoride trihydrate (TBAF). The native Sisal cellulose investigated contains 14% hemicellulose (mainly composed of xylose) as confirmed by 13C-NMR spectroscopy in DMSO-d6/TBAF and HPLC analysis after complete polymer degradation. Alkali treatment of Sisal cellulose decreases the amount of hemicellulose, the degree of polymerization and the crystallinity. Both Sisal cellulose samples can be dissolved in DMSO/TBAF after treatment at elevated temperature. GPC measurements showed high aggregation in the solution. Different homogeneous acylation reactions using carboxylic acid anhydrides and vinyl esters were carried out, showing a pronounced tendency of the anhydride towards hydrolysis in the solvent. This disadvantage can be diminished by decreasing the amount of the salt hydrate (TBAF trihydrate) or by a distillative removal of the majority of water. A strong interaction of the polymer with the water in the solvent was observed.

Composites based on phenolic matrices and both untreated and alkali and ionized air–treated jute fibers were prepared. Different fiber lengths and fiber content were used to reinforce the phenolic matrices. The jute fibers were characterized with respect to lignin, holocellulose, ash, and humidity contents and also to the crystallinity index. The mechanical properties of fibers were investigated by means of tensile analysis and the morphology by SEM. The untreated and treated jute fiber–reinforced composites were characterized as to water absorption. The mechanical property and morphological aspects of the composites were evaluated by impact strength and photomicrographs obtained from SEM. Among the jute fiber treatments considered in the present work, the treatment with a solution of 5% NaOH presented the best results because: (1) the fiber presented a higher tensile strength, and a larger percentage of elongation at break; (2) the composite reinforced with this fiber presented the highest impact strength results when this was the unique treatment (20% of fiber), as well as when it was combined with ionized air (30% of fiber); and (3) the composite that presented the lowest water uptake was that reinforced with this fiber. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 1077–1085, 2004

Lignocellulosic sisal fiber (LSF) and sisal pulp (SP) were electrospun at room temperature from solutions in trifluoroacetic acid (TFA) prepared at concentrations of 2 × 10−2 g mL−1 and 3 × 10−2 g mL−1, respectively. Scanning electron microscopy images of the electrospun LSF showed fibers with diameters ranging from 120 to 510 nm. The presence of defects decreased along with increasing the flow rate of the SP solution, which generated nanofibers and ultrathin fibers with diameters in the range of 40–60 (at 5.5 µL min−1) up to 90–200 nm (at 65.5 µL min−1). Despite the known ability of TFA to esterify the hydroxyl groups present in the starting materials, the Fourier transform infrared spectra indicated the absence of trifluoroacetyl groups in the electrospun samples. The thermal stability of the final materials proved suitable for many applications even though some differences were observed relative to the starting materials. This study demonstrated a feasible novel approach for producing nano/ultrathin fibers from lignocellulosic biomass or its main component, which allows for a wide range of applications for these materials. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41826.

In the present work, the action of a cationic polyelectrolyte (the ammonium hydroxy-propyl-trimethyl chloride of the polysaccharide guar gum, commercially know as cosmedia guar, CG) in aqueous alumina suspension was investigated. This polymer was used aiming to find alternatives for synthetic polymers, as for instance, sodium polyacrylate– PANa, normally used as a deflocculant agent of alumina suspension. Due to its positive charge, this polyelectrolyte (CG) can have electrostatic attractive interactions with the negative charges present on the surface of alumina in alkaline pH. Besides, the presence of hydroxyl groups in this polymer enables attractive interactions with alumina, by means of hydrogen bonds, thus preventing the approximation of other particles and leading to steric stabilization, as occurs when electrostatic attractive interactions (CG/alumina) are present. The study was carried out using the Fiber Optic Quasi-Elastic Light Scattering (FOQELS) technique, aiming to determine partic...

Lignin, extracted from sugarcane bagasse, was used as a partial phenol substitute in phenolic closed cell foams. The thermal stability of phenolic and lignophenolic foams were studied using thermogravimetric (TG) and differential scanning calorimetry (DSC) techniques, under air and nitrogen atmospheres. The results of apparent densities (Dapp) are also reported for both foams. The thermal analyses data showed that the decomposition depends on the atmosphere, that is, this process is not only a thermal one and, that it is feasible to replace part of the phenol by lignin in closed cell foams. Regarding the apparent density, that replacement was extremely advantageous because the Dapp value obtained placed the lignophenolic foam in the structural foam class.

The action of polyacrilates as stabilizing agents in alumina aqueous suspensions has been investigated using viscometry, zeta potential, and photon correlation spectroscopy (PCS) measurements. The present work emphasizes that the study of stability of dispersions using polyelectrolytes must necessarily include several techniques in order to evaluate different physicochemical properties of colloidal suspensions, and thus attain a wide comprehension of the system under analysis. In our point of view, this is necessary because, for instance, while viscosity measurements suggest that there is no advantage in the use of the polyelectrolyte at some pH values, particle size measurement as a function of time shows that the presence of PANa at that pH values allows a longer handling time in suspension processing. Low molecular sodium polyacrylate presented a good performance as a deflocculating agent, because it leads to dispersions of low viscosity, stable at a wide range of pH, and also low variation in...

Lignin, extracted from sugarcane bagasse by the organosolv process, was used as a partial substitute of phenol (40 w/w) in resole phenolic matrices. Short sugarcane fibers were used as reinforcement in these polymeric matrices to obtain fiber-reinforced composites. Thermoset polymers (phenolic and lignophenolic) and related composites were obtained by compression molding and characterized by mechanical tests such as impact, differential mechanical thermoanalysis (DMTA), and hardness tests. The impact test showed an improvement in the impact strength when sugarcane bagasse was used. The inner part of the fractured samples was analyzed by scanning electron microscopy (SEM), and the results indicated adhesion between fibers and matrix, because the fibers are not set free, suggesting they suffered a break during the impact test. The modification of fiber surface (mercerization and esterification) did not lead to an improvement in impact strength. The results as a whole showed that it is feasible to replace part of phenol by lignin in phenolic matrices without loss of properties. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 880–888, 2002

Cellulose samples from cotton linters, sisal, and sugar cane bagasse have been successively acylated (acetate, propionate, butyrate, and acetate/butyrate) under homogeneous reaction conditions, in LiCl/N,N-dimethylacetamide (DMAC), by the following procedure: (i) cellulose and LiCl are heated under reduced pressure, at 110°C; (ii) cellulose is dissolved in LiCl/DMAC by heating at 155°C, followed by cooling to 40°C; (iii) the solubilized polymer is acylated at 60°C for 18 h. Attractive features of this one-pot procedure include: easy control and high reproducibility of the degree of substitution; elimination of base catalyst; negligible degradation of the natural polymer; and recovery/recycling of high purity DMAC and acid anhydride. Reaction conditions employed for the present celluloses are different from those previously used for Avicel PH 101 microcrystalline cellulose because their fibrous nature, higher indices of crystallinity and higher molecular weights retard their dissolution and decrease their rates of acylation by acid anhydrides.

Commercially available cellulose (Avicell PH101) was successfully acylated under homogeneous solution conditions by the following procedure: 2.0 g of cellulose were stirred with 75 mL of N,N-dimethylacetamide for 1 h at 150°C, 3.5 g of LiCl were added, the temperature was raised to 170°C, ca. 18.5 mL of the solvent were distilled and the suspension was cooled to room temperature and stirred overnight. The temperature of the clear cellulose solution was raised to 110°C, kept at that temperature for 1 h, an acid anhydride was added and the solution stirred at 110°C for additional 4 h. Acetates, propionates, butyrates, and acetate/propionate mixed ester were prepared with excellent control of the degree of substitution, DS, 1 to 3 for acetates, 2 and 3 for propionates and butyrates, and 3 for acetate/propionate. The degree of polymerization of cellulose is negligibly affected under these reaction conditions. The distribution of the acetyl moiety among the three OH groups of the anhydroglucose unit shows a preference for the C6 position. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 1357–1363, 1999

The purpose of this paper is to draw a general picture for viscometric behaviour of polyelectrolytes. The polymers tested are hyaluronan (λ=0.7) and sodium polystyrene sulfonate (λ=2.8) with different molecular weights. The viscometric behaviour in isoionic dilution is examined and one demonstrates that k′[η]∼Cs−3/2. Dilution in water or with solvent of low salt concentration causes the reduced viscosity to pass through a maximum for a given polymer concentration. The position of the maximum and the amplitude of this maximum is analyzed for the low molecular weight samples in the dilute regime. The electrostatic contribution dominates and the treatment adopted gives good agreement between calculated and experimental data.

This investigation focuses on the preparation of bio-based composites from recycled poly (ethylene terephthalate) (PET) and sisal fibers (3 cm, 15 wt %), via thermopressing process. Plasticizers derived from renewable raw materials are used, namely, glycerol, tributyl citrate (TBC) and castor oil (CO), to decrease the melting point of the recycled PET (Tm ∼ 265°C), which is sufficiently high to initiate the thermal decomposition of the lignocellulosic fiber. All used materials are characterized by thermogravimetric analysis and differential scanning calorimetry, and the composites are also characterized via dynamic mechanical thermal analysis. The storage modulus (30°C) and the tan δ peak values of CT [PET/sisal/TBC] indicate that TBC also acts as a compatibilizing agent at the interface fiber/PET, as well as a plasticizer. To compare different processing methods, rheometry/thermopressing and compression molding are used to prepare the recycled PET/sisal/glycerol/CO composites. These two different methods of processing show no significant influence on the thermal properties of these composites. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40386.

Lignin can be recovered from sugar cane bagasse, which is widely available in Brazil as a residue from sugar mills. Many reports can be found in the literature on the partial replacement of phenol by lignin in phenolic-type resins, but normally only their application as an adhesive is considered. This work is part of a study intended to look for other uses for lignin-phenol resins; for instance, in molded materials. Resols were prepared with the partial replacement of phenol by organosolv sugar cane bagasse lignin (10, 20, 40, 100% w/w), and the pre-polymers were characterized by TGA and DSC. The cure reaction was performed in a mold in a process monitored by infrared spectroscopy. The resins obtained were characterized by TGA, DSC, and DMTA. TGA and DSC results revealed that endothermic and exothermic steps are probably involved in the cure reaction. From infrared results it can be inferred that lignin is really incorporated to the phenol polymer chain, where it acts as a chain extender. DMTA an...

Welan, purified as its sodium salt from unpasteurised culture broth, was analyzed by dilute aqueous viscometry. Measurements in water and at low ionic strength were carried out to evaluate the change effect on intrinsic viscosity. The value of intrinsic viscosity at low ionic strength, determined by the isoionic dilution method, is close to that obtained at higher salt concentrations. A comparison is made among the stiffness parameters determined by different treatment of experimental data. The results agree with previous reports on the weak polyelectrolyte character and high stiffness of the welan chain.

The hot-wire standard technique, mostly used for ceramic materials, was adapted to determine the thermal conductivity of nylon 6,6, polypropylene, poly(vinyl chloride), and poly(methyl methacrylate). The results obtained showed that the hot-wire standard technique can be used with accuracy and reproducibility to measure the thermal conductivity of polymers. In the second stage, to verify the effect of the use of a lignin (a “macromonomer”) in the thermal conductivity of phenolic resins, this technique was applied to phenol-formaldehyde and phenol–lignin–formaldehyde resins. © 1996 John Wiley & Sons, Inc.

This study was undertaken to evaluate both the properties of cellulose acetate films as a function of their degree of substitution (DS) and the possibility of generating reinforcements during film preparation. Sisal was selected for the entire study, among other reasons, because it is a rapidly growing source of cellulose. Cellulose acetates with various DS values were prepared in a homogeneous medium (dimethylacetamide/lithium chloride as the solvent system) and characterized. In DMAc/LiCl, cellulose and cellulose acetate films (mixed or not mixed with sisal cellulose) were successfully prepared and characterized. The films with high DS values exhibited lower hygroscopicity, a distinct morphology (scanning electron microscopy images), and lower tensile strength. In some cases, the films prepared from acetates/cellulose exhibited higher tensile strength and/or storage modulus than the acetate films. This result suggested a reinforcing action of the auto-organized cellulose chains that enabled the generation of both a film and reinforcement in a one-pot process.

The use of natural macromolecules from rejects of the fishing industry, such as chitosan and derivatives, may be advantageous in replacing synthetic polymers to stabilize ceramic suspensions. In this paper, a carboxymethylated chitosan (CMCh) was synthesized, characterized with FTIR, 1H NMR and SEC methods, and tested as stabilizing agent of alumina suspensions. Close to the point of zero charge (pzc) of the alumina suspensions (approximately pH 7), the incorporation of only 0.2 wt% of CMCh (DS, degree of substitution, 0.8) caused the suspension viscosity to decrease from ca. 40 × 103 Cps to approximately 16 × 103 Cps. This decrease in viscosity was accompanied by a decrease in particle size, as the incorporation of CMCh led to a narrower distribution of smaller particles. Furthermore, at the pzc of the aqueous alumina suspension, negative zeta potentials were measured when CMCh was added. Upon combining information from viscosity, particle size and zeta potential, it was possible to infer that CMCh induced the stabilization of alumina suspensions via steric and electrosteric effects. Because the latter can be tuned by changing parameters of the suspensions as well as of the CMCh derivatives, one may envisage further applications of alumina suspensions with tailored properties.

The enzymatic hydrolysis of cotton raw cellulose (RC) samples, sieved RC samples through meshes

The aim of this work was to study the properties of the carboxylated polyelectrolyte obtained from guar gum. The C-6 alcohol functions of galactose units side chains were oxidized first by GO-ase to aldehyde groups and then to carboxylic groups by halogen oxidation. The enzymic oxidation step was followed by the Dische method, by viscosity and light scattering measurements. With regard to previous reports, some changes were introduced in the two-step reaction, in order to prevent polymer degradation. Several characteristics of the carboxylated polyelectrolyte have been studied, such as molecular weight distribution, degree of substitution, viscosity, intrinsic viscosity determined by the isoionic method, radius of gyration, charge parameter and apparent intrinsic persistence length. The charged macromolecule formed from native guar showed all the typical characteristics of a polyelectrolyte. The viscometry results indicate that carboxylated guar has a much higher viscosity in low salt content than the native polymer, which improves its thickening properties.