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In the second part of this series of studies, the bicomponent adsorption of safranin-T (ST) and auramine-O (AO) on trimellitated sugarcane bagasse (STA) was evaluated using equimolar dye aqueous solutions at two pH values. Bicomponent batch adsorption was investigated as a function of contact time, solution pH and initial concentration of dyes. Bicomponent kinetic data were fitted by the pseudo-first-order and pseudo-second-order models and the competitive model of Corsel. Bicomponent equilibrium data were fitted by the real adsorbed solution theory model. The antagonistic interactions between ST and AO in the adsorption systems studied contributed to obtain values of maximum adsorption capacity in mono- (Q max,mono ) and bicomponent (Q max,multi ) lower than unity (Q max,multi /Q max,mono at pH 4.5 for ST of 0.75 and AO of 0.37 and at pH 7 for ST of 0.94 and AO of 0.43). Mono- and bicomponent adsorption of dyes in a fixed-bed column was evaluated at pH 4.5. The breakthrough curves were fitted by the Thomas and Bohart-Adams original models. Desorption of ST in a fixed-bed column was studied. The results obtained from the bicomponent batch and continuous adsorption showed that the presence of ST most affected the AO adsorption than the presence of AO affected the ST adsorption., (Copyright © 2019 Elsevier Inc. All rights reserved.)

Sugarcane bagasse cellulose succinate trimellitate (SBST) was prepared by a one-pot synthesis method. The synthesis of this novel mixed ester was investigated by a 2 3 -factorial design. The parameters investigated were time, temperature, and succinic anhydride mole fraction (χ SA ). The responses evaluated were the adsorption capacity (q Co2+ and q Ni2+ ), weight gain (wg), and number of carboxylic acid groups (n T,COOH ). 13 C Multiple Cross-Polarization solid-state NMR spectroscopy, 1 H NMR relaxometry, and Fourier-transform infrared spectroscopy were used to elucidate the SBST structure. The best SBST reaction conditions were 100 °C, 660 min, and χ SA of 0.2, which yielded SBST with a wg of 57.1%, n T,COOH of 4.48 mmol g -1 , and q Co2+ and q Ni2+ of 0.900 and 0.963 mmol g -1 , respectively. The maximum adsorption capacities (Q max ) (pH 5.75, 25 °C) estimated by the Redlich-Peterson model for Co 2+ and Ni 2+ were 1.16 and 1.29 mmol g -1 . The Δ ads H° values for Co 2+ and Ni 2+ adsorption obtained by isothermal titration calorimetry were 8.03 and 6.94 kJ mol -1 . Regeneration and reuse of SBST were investigated and the best conditions applied for fixed-bed column adsorption in five consecutive cycles. SBST was fully desorbed and Q max values for Co 2+ (0.95 mmol g -1 ) and Ni 2+ (1.02 mmol g -1 ) were estimated using the Bohart-Adams model., (Copyright © 2019 Elsevier Inc. All rights reserved.)

Sugarcane bagasse cellulose mixed ester succinate phthalate (SBSPh) was synthesized by a novel one-pot reaction method. The effects of temperature, time and mole fraction of succinic anhydride (χ SA ) on the responses weight gain (wg), number of carboxylic acid groups (n T,COOH ), and adsorption capacity (q) of Co 2+ and Ni 2+ were evaluated by a 2 3 experimental design. The chemical structure of the material was elucidated by Fourier transform infrared, 13 C Multiple Cross-Polarization solid-state NMR spectroscopy and 1 H NMR relaxometry. The best SBSPh synthesis condition (100 °C, 11 h, χ SA of 0.2) yielded a wg of 59.1%, n T,COOH of 3.41 mmol g -1 , and values of q Co 2+ and q Ni 2+ of 0.348 and 0.346 mmol g -1 , respectively. The Sips model fitted better the equilibrium data, and the maximum adsorption capacities (pH 5.75 and 25 °C) estimated by this model were 0.62 and 0.53 mmol g -1 for Co 2+ and Ni 2+ , respectively. The Δ ads H° values estimated by isothermal titration calorimetry were 8.43 and 7.79 kJ mol -1 for Co 2+ and Ni 2+ , respectively. Desorption and re-adsorption efficiencies were evaluated by a 2 2 experimental design, which showed that SBSPh adsorbent can be recovered and reused without significant loss of adsorption capacity., (Copyright © 2018 Elsevier Inc. All rights reserved.)

Cellulose (Cel) and sugarcane bagasse (SB) were oxidized with an H 3 PO 4 -NaNO 2 mixture to obtain adsorbent materials with high contents of carboxylic groups. The oxidation reactions of Cel and SB were optimized using design of experiments (DOE) and response surface methodology (RSM). The optimized synthesis conditions yielded Cox and SBox with 4.8mmol/g and 4.5mmol/g of carboxylic acid groups, respectively. Cox and SBox were characterized by FTIR, TGA, PZC and solid-state 13 C NMR. The adsorption of the model cationic dyes crystal violet (CV) and auramine-O (AO) on Cox and SBox in aqueous solution was investigated as a function of the solution pH, the contact time and the initial dye concentration. The adsorption of CV and AO on Cox was described by the Elovich equation and the pseudo-first-order kinetic model respectively, while the adsorption of CV and AO on SBox was described by the pseudo-second-order kinetic model. Adsorption isotherms were well fitted by the Langmuir and Konda models, with maximum adsorption capacities (Q max ) of 1117.8mg/g of CV and 1223.3mg/g of AO on Cox and 1018.2mg/g of CV and 682.8mg/g of AO on SBox. Desorption efficiencies were in the range of 50-52% and re-adsorption capacities varied from 65 to 81%, showing the possibility of reuse of both adsorbent materials., (Copyright © 2017 Elsevier Inc. All rights reserved.)

In the context of a sugarcane biorefinery, sugarcane bagasse produced may be pretreated generating a solid and liquid fraction. The solid fraction may be used for 2G bioethanol production, while the liquid fraction may be used to produce biogas through anaerobic digestion. The aim of this study consisted in evaluating the anaerobic digestion performance of hemicellulose hydrolysate produced after hydrothermal pretreatment of sugarcane bagasse. For this, hydrothermal pretreatment was assessed in a continuous upflow anaerobic sludge blanket (UASB) reactor operated at a hydraulic retention time (HRT) of 18.4h. Process performance was investigated by varying the dilution of sugarcane bagasse hydrolysate with a solution containing xylose and the inlet organic loading rate (OLR). Experimental data showed that an increase in the proportion of hydrolysate in the feed resulted in better process performance for steps using 50% and 100% of real substrate. The best performance condition was achieved when increasing the organic loading rate (OLR) from 1.2 to 2.4gCOD/L·d, with an organic matter removal of 85.7%. During this period, the methane yield estimated by the COD removal would be 270LCH 4 /kg COD. Nonetheless, when further increasing the OLR to 4.8gCOD/L·d, the COD removal decreased to 74%, together with an increase in effluent concentrations of VFA (0.80gCOD/L) and furans (115.3mg/L), which might have inhibited the process performance. On the whole, the results showed that anaerobic digestion of sugarcane bagasse hydrolysate was feasible and may improve the net energy generation in a bioethanol plant, while enabling utilization of the surplus sugarcane bagasse in a sustainable manner., (Copyright © 2017 Elsevier B.V. All rights reserved.)

A new carboxylated cellulose derivative (CTA) was prepared from the esterification of cellulose with 1,2,4-Benzenetricarboxylic anhydride. CTA was characterized by percent weight gain (pwg), amount of carboxylic acid groups (nCOOH), elemental analysis, FTIR, TGA, solid-state (13)C NMR, X-ray diffraction (DRX), specific surface area, pore size distribution, SEM and EDX. The best CTA synthesis condition yielded a pwg and nCOOH of 94.5% and 6.81mmolg(-1), respectively. CTA was used as an adsorbent material to remove Co(2+), Cu(2+) and Ni(2+) from monocomponent spiked aqueous solution. Adsorption studies were developed as a function of the solution pH, contact time and initial adsorbate concentration. Langmuir model better fitted the experimental adsorption data and the maximum adsorption capacities estimated by this model were 0.749, 1.487 and 1.001mmolg(-1) for Co(2+), Cu(2+) and Ni(2+), respectively. The adsorption mechanism was investigated by using isothermal titration calorimetry. The values of ΔadsH° were in the range from 5.36 to 8.09kJmol(-1), suggesting that the mechanism controlling the phenomenon is physisorption. Desorption and re-adsorption studies were also performed. Desorption and re-adsorption efficiencies were closer to 100%, allowing the recovery of both metal ions and CTA adsorbent., (Copyright © 2016 Elsevier Inc. All rights reserved.)

This study aimed at optimizing the net energy recovery from hydrogen and methane production through anaerobic digestion of the hemicellulose hydrolysate (HH) obtained by desirable conditions (DC) of autohydrolysis pretreatment (AH) of sugarcane bagasse (SB). Anaerobic digestion was carried out in a two-stage (acidogenic-methanogenic) batch system where the acidogenic phase worked as a hydrolysis and biodetoxification step. This allowed the utilization of more severe AH pretreatment conditions, i.e. T=178.6°C and t=55min (DC3) and T=182.9°C and t=40.71min (DC4). Such severe conditions resulted in higher extraction of hemicelluloses from SB (DC1=68.07%, DC2=48.99%, DC3=77.40% and DC4=73.90%), which consequently improved the net energy balance of the proposed process. The estimated energy from the combustion of both biogases (H2 and CH4) accumulated during the two-stage anaerobic digestion of HH generated by DC4 condition was capable of producing a net energy of 3.15MJ·kgSB(-1)dry weight., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

In this study the adsorption of cationic dyes by modified sugarcane bagasse with EDTA dianhydride (EB) was examined using methylene blue (MB) and gentian violet (GV) as model compounds in aqueous single solutions. The synthesized adsorbent (EB) was characterized by FTIR, elemental analysis, and BET. The capacity of EB to adsorb dyes was evaluated at different contact times, pH values, and initial dye concentrations. According to the obtained results, the adsorption processes could be described by a pseudo-second-order kinetic model. The adsorption isotherms were well fitted by the Langmuir model. Maximum adsorption capacities for MB and GV on EB were found to be 202.43 and 327.83 mg/g, respectively. The free energy change during adsorption of MB and GV was found to be -22.50 and -24.21 kJ/mol, respectively, suggesting that chemisorption is the main mechanism controlling the adsorption process., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

This paper describes the organosolv delignification of depithed bagasse using glycerol-water mixtures without a catalyst. The experiments were performed using two separate experimental designs. In the first experiment, two temperatures (150 and 190°C), two time periods (60 and 240 min) and two glycerol contents (20% and 80%, v/v) were used. In the second experiment, which was a central composite design, the glycerol content was maintained at 80%, and a range of temperatures (141.7-198.3°C) and time (23-277 min) was used. The best result, obtained with a glycerol content of 80%, a reaction time of 150 min and a temperature of 198.3°C, produced pulps with 54.4% pulp yield, 7.75% residual lignin, 81.4% delignification and 13.7% polyose content. The results showed that high contents of glycerol tend to produce pulps with higher delignification and higher polyoses content in relation to the pulps obtained from low glycerol content reactions. In addition, the proposed method shows potential as a pretreatment for cellulose saccharification., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

This study describes the preparation of two new chelating materials, MMSCB 3 and 5, derived from succinylated twice-mercerized sugarcane bagasse (MMSCB 1). MMSCB 3 and 5 were synthesized from MMSCB 1 using two different methods as described by Gurgel and Gil (2009). In the first method MMSCB 1 was activated with 1,3-diisopropylcarbodiimide and in the second with acetic anhydride (to form an internal anhydride) and later both were reacted with triethylenetetramine in order to obtain MMSCB 3 and 5. New obtained materials were characterized by mass percent gain, concentration of amine groups, FTIR, and elemental analysis. MMSCB 3 and 5 showed mass percent gain of 19.9 and 57.1%, concentration of amine groups of 2.0 and 2.1 mmol/g, and nitrogen content of 5.8 and 4.4%. The capacity of MMSCB 3 and 5 to adsorb Cu(2+), Cd(2+), and Pb(2+) from aqueous single metal ion solutions was evaluated at different contact times, pHs, and initial metal ion concentrations. Adsorption isotherms were well fitted by Langmuir model. Maximum adsorption capacities of MMSCB 3 and 5 for Cu(2+), Cd(2+), and Pb(2+) were found to be 59.5 and 69.4, 86.2 and 106.4, 158.7 and 222.2 mg/g, respectively.

Succinylated mercerized cellulose (cell 1) was used to synthesize an anion exchange resin. Cell 1, containing carboxylic acid groups was reacted with triethylenetetramine to introduce amine functionality to this material to obtain cell 2. Cell 2 was reacted with methyl-iodide to quaternize the amine groups from this material to obtain cell 3. Cells 2 and 3 were characterized by mass percent gain, degree of amination and quaternization, FTIR and CHN. Cells 2 and 3 showed degrees of amination and quaternization of 2.8 and 0.9 mmol/g and nitrogen content of 6.07% and 2.13%, respectively. Cell 3 was used for Cr (VI) adsorption studies. Adsorption equilibrium time and optimum pH for Cr (VI) adsorption were found to be 300 min and 3.1, respectively. The Langmuir isotherm was used to model adsorption equilibrium data. The adsorption capacity of cell 3 was found to be 0.829 mmol/g. Kinetic studies showed that the rate of adsorption of Cr (VI) on cell 3 obeyed a pseudo-second-order kinetic model.

This work describes the preparation of new chelating material from mercerized cellulose. The first part treats the chemical modification of non-mercerized cellulose (cell 1) and mercerized cellulose (cell 2) with succinic anhydride. Mass percent gains (mpg) and degree of succinylation (DS) of cell 3 (from cell 1) and cell 4 (from cell 2) were calculated. Cell 4 in relation to cell 3 exhibited an increase in mpg and in the concentration of carboxylic functions of 68.9% and 2.8 mmol/g, respectively. Cells 5 and 6 were obtained by treatment of cells 3 and 4 with bicarbonate solution to release the carboxylate functions and characterized by FTIR. The second part compares the adsorption capacity of cells 5 and 6 for Cu2+, Cd2+, and Pb2+ ions in an aqueous single metal solution. Adsorption isotherms were developed using Langmuir model. Cell 6 in relation to cell 5 exhibited an increase in Qmax for Cu2+ (30.4 mg/g), Cd2+ (86.0 mg/g) and Pb2+ (205.9 mg/g).

This work describes the application of raw and chemically modified cellulose and sugarcane bagasse for ipso-hydroxylation of aryl boronic acids in environmentally friendly reaction conditions. The catalytic efficiency of five support-[Cu] materials was compared in forming phenols from aryl boronic acids. Our investigation highlights that the CEDA-[Cu] material (6-deoxy-6-aminoethyleneamino cellulose loaded with Cu) leads to the best results under very mild reaction conditions. The optimized catalytic sequence, allowing a facile transformation of boronic acids to phenols, required the mandatory and joint presence of the support, Cu2O, and KOH at room temperature. CEDA-[Cu] was characterized using 13C solid-state NMR, ICP, and FTIR. The use of CEDA-[Cu] accounts for the efficacious synthesis of variously substituted phenol derivatives and presents very good recyclability after five catalytic cycles. [ABSTRACT FROM AUTHOR]

Abstract: Sugarcane bagasse cellulose was subjected to the extremely low acid (ELA) hydrolysis in 0.07% H2SO4 at 190, 210 and 225°C for various times. The cellulose residues from this process were characterized by TGA, XRD, GPC, FTIR and SEM. A kinetic study of thermal decomposition of the residues was also carried out, using the ASTM and Kissinger methods. The thermal studies revealed that residues of cellulose hydrolyzed at 190, 210 and 225°C for 80, 40 and 8min have initial decomposition temperature and activation energy for the main decomposition step similar to those of Avicel PH-101. XRD studies confirmed this finding by showing that these cellulose residues are similar to Avicel in crystallinity index and crystallite size in relation to the 110 and 200 planes. FTIR spectra revealed no significant changes in the cellulose chemical structure and analysis of SEM micrographs demonstrated that the particle size of the cellulose residues hydrolyzed at 190 and 210°C were similar to that of Avicel. [Copyright &y& Elsevier]

Abstract: In a previous work, chemically modified cellulose (EMC) and sugarcane bagasse (EMMB) were prepared from mercerized cellulose (MC) and twice-mercerized sugarcane bagasse (MMB) using ethylenediaminetetraacetic dianhydride (EDTAD) as modifying agent. In this work we described in detail the modification of these materials in function of reaction time and EDTAD amount in the reaction media. The resistance of ester bond at pH 1, 2, 11, and 12 was also evaluated by FTIR. The results were used to model the hydrolysis process and a kinetic model was proposed. The modified materials (EMMB and EMC) were used to adsorb Ca2+ and Mg2+ ions from aqueous single solutions. The adsorption isotherms were developed at two pH values. These materials showed maximum adsorption capacities for Ca2+ and Mg2+ ions ranging from 15.6 to 54.1mg/g and 13.5 to 42.6mg/g, respectively. The modified material from sugarcane bagasse (EMMB) showed larger maximum adsorption capacities than modified material from cellulose (EMC) for both metals. [Copyright &y& Elsevier]

Abstract: This work describes the preparation of new chelating materials derived from cellulose and sugarcane bagasse for adsorption of Cu2+, Cd2+, and Pb2+ ions from aqueous solutions. The first part involved the mercerization treatment of cellulose and sugarcane bagasse with NaOH 5mol/L. Non- and mercerized cellulose and sugarcane bagasse were then reacted with ethylenediaminetetraacetic dianhydride (EDTAD) in order to prepare different chelating materials. These materials were characterized by mass percent gain, X-ray diffraction, FTIR, and elemental analysis. The second part consisted of evaluating the adsorption capacity of these modified materials for Cu2+, Cd2+, and Pb2+ ions from aqueous single metal solutions, whose concentration was determined by atomic absorption spectroscopy. These materials showed maximum adsorption capacities for Cu2+, Cd2+, and Pb2+ ions ranging from 38.8 to 92.6mg/g, 87.7 to 149.0mg/g, and 192.0 to 333.0mg/g, respectively. The modified mercerized materials showed larger maximum adsorption capacities than modified non-mercerized materials. [Copyright &y& Elsevier]

Abstract: This study describes the preparation of two new chelating materials derived from succinylated mercerized cellulose (cell 1). Cell 1 was activated through two different methods by using diisopropylcarbodiimide and acetic anhydride (to form an internal anhydride) and reacted with triethylenetetramine in order to obtain cell 2 and 4. New modified celluloses were characterized by mass percent gain, concentration of amine functions, elemental analysis, and infrared spectroscopy. Cell 2 and 4 showed degrees of amination of 2.8 and 2.3mmol/g and nitrogen content of 6.07% and 4.61%, respectively. The capacity of cell 2 and 4 to adsorb Cu2+, Cd2+, and Pb2+ ions from single aqueous solutions were examined. The effect of contact time, pH, and initial concentration of metal ions on the metal ions uptake was also investigated. Adsorption isotherms were well fitted by the Langmuir model. The maximum adsorption capacity of cell 2 and 4 were found to be 56.8 and 69.4mg/g for Cu2+; 68.0 and 87.0mg/g for Cd2+; and 147.1 and 192.3mg/g for Pb2+, respectively. [Copyright &y& Elsevier]

This study described the anaerobic degradation of the azo dye Remazol Golden Yellow RNL (RGY-RNL) using cellulose-immobilized riboflavin (MC 3) as the redox mediator. This new solid support containing immobilized riboflavin was synthesized from succinylated mercerized cellulose, and was characterized by elemental analysis, FTIR, and solid-state 13 C NMR. MC 3 was resistant to pH 2–9, and anaerobic degradation of RGY-RNL using MC 3 in the presence of anaerobic sludge yielded a zero order degradation rate constant ( k 0,obs ) equal to 0.189 mg/L h, which was 56% better than experiments carried out without a redox mediator. Color removal efficiency after 48 h of degradation averaged 89.4% in experiments with MC 3 and 72% without the addition of a redox mediator. These results showed that MC 3 can be used to immobilize redox mediators, allowing reduction of wastewater treatment costs. [ABSTRACT FROM AUTHOR]

A bioadsorbent (CEDA) capable of adsorbing As(V) and Cu(II) simultaneously was prepared by tosylation of microcrystalline cellulose (MC) and nucleophilic substitution of the tosyl group by ethylenediamine. MC, tosyl cellulose, and CEDA were characterized by elemental C, H, N, and S analysis, infrared spectroscopy, and 13C solid-state nuclear magnetic resonance spectroscopy. The adsorption of As(V) and Cu(II) on CEDA was evaluated as a function of solution pH, contact time, and initial solute concentration. The maximum adsorption capacities of CEDA for As(V) and Cu(II) were 1.62 and 1.09 mmol g−1, respectively. The interactions of As(V) and Cu(II) with CEDA were elucidated using thermodynamic parameters, molecular quantum mechanics calculations, and experiments with ion exchange of Cd(II) by Cu(II), and As(V) by SO 4 2−. Adsorption enthalpies were determined as a function of surface coverage of the CEDA, using isothermal titration calorimetry, with Δ ads H ° values of −32.24 ± 0.07 and −93 ± 2 kJ mol−1 obtained for As(V) and Cu(II), respectively. The potential to reuse CEDA was evaluated and the interference of other ions in the adsorption of As(V) and Cu(II) was investigated. Multi-component experiments showed that Cd(II), Co(II), Ni(II), and Pb(II) did not interfere in the adsorption of Cu(II), while SO 4 2− inhibited As(V) adsorption. [ABSTRACT FROM AUTHOR]

In the second part of this series of studies, the competitive adsorption of three binary systems Cu 2+ –Co 2+ , Cu 2+ –Ni 2+ and Co 2+ –Ni 2+ on a carboxylated cellulose derivative (CTA) was evaluated in binary equimolar (1:1) metal–ion aqueous solutions. Bicomponent adsorption studies were developed as a function of contact time and initial metal ion concentration. Bicomponent adsorption kinetic data was modeled by monocomponent kinetic models of pseudo-first- (PFO) and pseudo-second-order (PSO) and a competitive kinetic model of Corsel. Bicomponent adsorption isotherm data was modeled by the ideal adsorbed solution theory (IAST) and real adsorbed solution theory (RAST) models. The monocomponent isotherm models implemented into the IAST were the Langmuir and Sips models, whereas for the RAST model only the Langmuir model was implemented because this model provided the best prediction of the bicomponent isotherm data. The surface of the CTA adsorbent after bicomponent adsorption of metal ions was also examined by SEM-EDX. The effect of one metal ion on the adsorption capacity of another metal ion was discussed in detail with basis on the kinetic and thermodynamics parameters. The selectivity and performance of the CTA adsorbent for the removal of Cu 2+ , Co 2+ and Ni 2+ was also evaluated and discussed. [ABSTRACT FROM AUTHOR]