Valorization of Sawdust Biomass For Biopolymer Extraction Via Green Method: Comparison With Conventional Process

Received: 29 October 2021 Revised: 30 April 2022 Accepted: 5 May 2022
DOI: 10.1002/er.8112
SPECIAL ISSUE RESEARCH ARTICLE
Valorization of sawdust biomass for biopolymer extraction

via green method: Comparison with conventional process
Roberto Cardenas-Zapata1 | Diana Palma-Ramírez1 |

1
Abelardo I. Flores-Vela | Miguel A. Domínguez-Crespo2 |
Aidé M. Torres-Huerta2 | Héctor Dorantes-Rosales 3
| Silvia B. Brachetti-Sibaja4
1
Instituto Politécnico Nacional IPN, Centro Mexicano para la Producci
on mas Limpia (CMP+L), Ciudad de México, México
2
Instituto Politécnico Nacional-IPN, Unidad Profesional Interdisciplinaria de Ingeniería (UPIIH), San Agustín Tlaxiaca, México
3
Instituto Politécnico Nacional, Escuela Superior de Ingeniería Química e Industrias Extractivas (ESIQIE), Ciudad de México, México
4
Tecnol
ogico Nacional de México, IT de Cd. Madero, Cd. Madero, México
Correspondence
Diana Palma-Ramírez, Instituto Summary
Politécnico Nacional IPN, Centro The valorization of sawdust (SW) biomass by-product, to extract cellulose
Mexicano para la Produccion mas Limpia
through alkali and bleaching processes, including side-streams to recover
(CMP+L), Av. Acueducto s/n, la Laguna
Ticoman, C.P. 07340 México City, México. hemicellulose and lignin, is performed with the intention of evaluating differ-
Email: [email protected] ences with a proposed green method (GM). The study is developed with the
intention of having a process at laboratory scale without leading to the compli-
Funding information
Instituto Politécnico Nacional, Grant/ cated nanoscale processing. This study contemplates a process with scalable
Award Numbers: SIP2022-0548, characteristics for the future, which contributes to wood processing waste
SIP2022-0668, SIP2022-0671,
around the world. Particularly, agroindustrial wastes from Durango (SWT1)
SIP2022-0672, SIP2022-1111,
SIP2022-1153, SIP2022-1155 and Hidalgo (SWT2), local communities of Mexico, were studied. SWT1 and
SWT2 samples were processed with ethanol, sodium hydroxide followed by
bleaching with sodium chlorite/acetic acid to remove, extractives (E), hemicel-
lulose (H) and lignin (L), respectively. Selected-SWT2 was processed through a
proposed GM using hydrogen peroxide/sodium hydroxide. On the basis of
results including Fourier transform infrared spectroscopy, thermogravimetric/
differential analysis (TGA/DTG), X-ray diffraction (XRD), dynamic light scat-
tering, high heating value, scanning electron microscopy techniques and chem-
ical composition, GM was capable of producing a biomass rich in α-cellulose
(58.0%: SWT2-C), whereas processed SWT1 and SWT2 through conventional
method led to a more percentage of H, β- and γ-C mixtures than α-polymor-
phous; 41.0% and 51.0%, respectively. This new method could impact of an
Abbreviations: C, cellulose; CC, chemical composition; DLS, dynamic light scattering; E, extractives; FT-IR, Fourier transform infrared spectroscopy;
GM, green method; H, hemicellulose; HC, holocellulose; HHV, High heating value; L, lignin; LCA, life cycle analysis; LG, lignocellulosic; MCC,
microcrystalline cellulose; SEM, scanning electron microscopy; SW, sawdust; SWT1- E, sawdust from Hidalgo region with removed extractives; SWT1-
H, sawdust from Hidalgo region with removed hemicellulose through conventional method; SWT1, sawdust from Hidalgo region; SWT1-C, sawdust
from Hidalgo region with removed lignin through conventional method (cellulose); SWT2, sawdust from Durango region; SWT2-C, sawdust from
Durango region with removed lignin through conventional method (cellulose); SWT2-C-GM, sawdust from Durango region with removed lignin
through green method (cellulose); SWT2-E, sawdust from Durango region with removed extractives; SWT2-H, sawdust from Durango region with
removed hemicellulose through conventional method; TGA/DTG, thermogravimetric/differential analysis; XRD, X-ray diffraction.
Int J Energy Res. 2022;1–24. wileyonlinelibrary.com/journal/er © 2022 John Wiley & Sons Ltd. 1
2 CÁRDENAS-ZAPATA ET AL.
important manner to the development of biodegradable thermoplastics. The

approximation, from deconvolution of TGA/DTA, led to determine adequately
the composition of hemicellulose (SWT1-C: 51.0%, SWT2-C: 36.0–0.00%), lignin
(SWT1-C: 17.0%, SWT2-C: 20.0%) and cellulose (SWT1-C: 32.0%, SWT2-C: 44.0%).
XRD analysis also indicated that samples contain the following percentage of
polymorphous cellulose compounds: SWT1-C (Type II: 71.3%), SWT2-C (Type I
α: 44.6% and II: 41.4%) and SWT2-C-GM (Type II: 38.8%), which confirms that
the combination of the type of biomass and the applied pretreatment plays a
fundamental role for final applications; in this case, it can be appropriate for
elastomers and thermoplastic uses. As a final point, the cellulose composition
and thermal stability of both sources is comparable with the commonly used
raw material for commercial products.
KEYWORDS
biopolymers, cellulose extraction, clean energy solutions, green bleaching, sawdust
valorization, wood waste
1 | INTRODUCTION materials, such as crosslinking agents, chemicals and

fuels,8 for example, raw materials for bio-hydrogen
Constant use and incorrect disposal of plastic products, production,9 solar cells,10 wastewater treatment11 and
fabricated from non-renewable resources, cause the dete- solar-steam-assisted desalination,12 to name a few. In
rioration of ecosystem generating the white pollution fact, biomass also has great potential in the functional
problem1; a topic related to single-use plastics discarded materials field of high performance.13 In this sense,
as solid wastes after just one use.2 This problem can be pyrolysis of LG biomass has been used to obtain
mitigated using biopolymers during bioplastic fabrication advanced biofuels using zeolite-based catalysts.14 In addi-
because energy requirement is typically less than those tion, biochar from algae15 and activated carbon from
required for petroleum resources. Additionally, bio- pinecone16 biomasses have been proposed and converted
plastics achieve low environmental footprint.3 For exam- into high performance supercapacitors.
ple, it has been reported mean value of energy Among biomass, sawdust (SW), the by-product from
requirement, ca. 57.0 and 77.0 MJ/kg, for bio- and fossil- forestry industry, is an example of a source of zero cost
based plastic production, respectively.4 Nowadays, there and great availability that can be used for extracting lig-
are diverse sources to make biopolymers, such as polysac- nocellulosic (LG) biopolymers and converting them into
charides, proteins and lipids, having different properties, value-added bioplastics emerging to a circular econ-
which can be extracted and processed to be used in differ- omy.17 It is important to clarify that biomass of SW, with-
ent areas.5 out physical or chemical modification, can be only used
On the other hand, a great opportunity to extract bio- to generate energy through combustion, representing
degradable polymers is found in the biomass from by- excessive particulate matter release and therefore, envi-
products of agrowastes, which are considered as second ronmental18 pollution. For this reason, biopolymers of
generation of feedstocks.6 The use of biomass, a clean cellulose (C), hemicellulose (H) and lignin (L), as the
and renewable energy, has been proposed by environ- main SW components, can be successfully extracted to
mental committees around the world with the aim of increase value-added and furthermore to propose them
reducing carbon dioxide emissions.7 Renewable biomass for specific applications in the bioplastic field for clean
removes CO2 from atmosphere maintaining it stored in energy solutions. To reach this goal, it is required to per-
the whole product life, which can be prolonged if form some pretreatments before using it for the bio-
recycled. This is an advantage for bioplastic products plastics transformation processes.19 In this sense, it is
because it mitigates the problems of climate change and important to consider that LGs have low deformability
global warming.7 and no melting temperature, reason why melt-
Additional to bioplastics, valorization of organic bio- compounding process using a thermoplastic matrix is
mass can led us to obtain sustainable and valuable required to obtain an optimal dispersibility.20 This is the
CÁRDENAS-ZAPATA ET AL. 3
reason why fibers need to be pretreated to permit the them to valorize these side-streams when cellulose is
adhesion with polymeric matrixes; thus improving their obtained. For this reason, precipitation methods using
interlocking.21 antisolvents (methanol, ethanol, acetone)39 and acids40
Biomass pretreatment has the purpose of letting cellu- can be performed.
lose almost intact while removing some H and L con- The removal of H and L, can also be done using green
tent.22 Although now, there are numerous methods to methods (GMs) including hydrogen peroxide (H2O2) and
perform it, among which, each one has its own advan- sodium hydroxide reagents for bleaching process.41 In
tages and drawbacks.23 The latest biomass pretreatment comparison with chlorine methods, which release haz-
trends include (a) chemical (acid, alkali, organosolv, oxi- ardous pollutants,42 H2O2 decomposes into non-toxic
dant), (b) physical (grinding, extrusion, freezing, micro- products such as oxygen and water,27 reason why it is
wave, ultrasonic bath), (c) physical-chemical (steam classified as eco-friendly.43 On the other hand, the use of
explosion, ammonia fiber explosion, and percolation of NaOH, is highly efficient to degrade lignin through free
ammonia recycling, chemical microwave, liquid hot radicals44 enhancing the delignification.45 Both has the
water and hydrothermal liquefaction) and (d) biological advantage of being less corrosive than chlorine-based
(fungi and bacteria), which in turn depends on the eco- methods.46 In this context, although several synthesis
nomic factor, the type of raw material and environmental methods have been proposed to separate cellulosic com-
impacts.24,25 For example, steam explosion and fiber pounds. The chemical methods are still the most used
explosion, technologies of pretreatment using high- because there is no special requirements as well as they
pressured saturated steam, are able to reduce fiber size can be operated at low temperatures.47,48 By comparing
and improve accessibility of cellulose for its further deg- the chemical methods, it has been stated that typical
radation, but with the disadvantage of recovering a low Kraft pulping process requires many operation steps with
polymerization degree.26 Additionally, it has some limita- water, sodium sulfide (Na2S), NaOH, and bleaching with
tions with respect to the incomplete disruption of lignin- free- or based-methods49; whereas simple alkaline treat-
carbohydrate matrix and high content lignin.27 Pretreat- ment has the advantage of requiring inexpensive
ments can be either physical (eg, milling, grinding, chemicals, processing in mild conditions and high effi-
microwave, sonication, and pyrolysis) or a physicochemi- ciency in lignin and xylan removal with minimal sugar
cal process (ammonia, supercritical fluids).28 In addition, degradation.49 Furthermore, caustic salts can be recov-
biological pretreatments involving bacteria, fungi and ered and regenerated.50 Similarly, bleaching through
metabolites such as enzymes to hydrolyze and degrade L, chlorine-based method is more effective in removing lig-
H and C. This method has the advantage of being free of nin from the inner wall of the fiber than from surface.51
chemicals, however, it is a very slow process.29 Then, it is considered that it has a better efficiency than
Chemical pretreatments (CP) typically degrade side GMs for the removal of residual hemicellulose and lig-
chains of esters and glycosides.30 Alkali and bleaching nin.52 Sodium chlorite treatment provides more deli-
processes lead to H and L liberations through disrupting gnified fibers compared with the Kraft method.53
cell walls and cleaving bonds, respectively.31,32 In this Current research around the world related to SW
sense, sodium and potassium hydroxides (NaOH and waste processing is focused on the extraction of the
KOH) with concentrations between 8.00% and 10.0%, cellulose-derived compounds such as crystalline or amor-
have shown efficacy in cleaving uronic and acetic esters, phous.54 Especially, as nanocrystals55 and
α-ether linkages (phenolic)33 for hemicelluloses removal 56
nanofibrillated cellulose where the final properties can
and solubilization in the media.34 be conveniently adjusted with the aforementioned
On the other hand, the oxidative bleaching (mostly methods combined with acid hydrolysis. Recent
sodium chlorite) process considers oxidizing insoluble researchers on the SW topic in which the contribution
water lignin compounds to break the aryl ether, carbon- related to C, L and H are highlighted are shown in
carbon and β-O-4 bonds35 which produces toxic organo- Table S1. As noted, most studies focus on C, L and H con-
chlorine such as chlorine dioxide (ClO2).36 Sodium chlo- tents in raw SW, but not after pretreatment, which is key
rite/acetic acid treatment is accessible and inexpensive for final properties.54,55,57-61 In fact, some works do not
leading to remove up to 60 wt% of lignin and improving report data of the initial composition.56 The only is the
purity and brightness of biomass, with minimum cellu- case of sulfonated SW59 in which the products after the
lose content losses and high recovery of hemicellulose.37 isolation of hemicellulose and cellulose during a multi-
In both cases, hemicellulose and lignin are dissolved product biorefinery process were analyzed.62 In this
in aqueous media, then, sent to be burned to generate sense, the most recent works focus on obtaining micro-
energy, losing the chance of giving value as raw chemi- fibrillated (MFC)55 and nanocrystalline cellulose56 from
cal.38 Thus, it is very important to consider extracting SW residues.54 These reports include an analysis of the
synthesis parameters and their influence on the degree of composition and the polymorphous quantification from
crystallinity degree,54,56,59 morphologies,55,60 conductivity X-ray diffraction (XRD), the isolated cellulose is pro-
and compressibility57 as well as yield of hemicellulose59 posed, as raw material, for the synthesis of specific bio-
and lignin after pretreatment to obtain glucose.61 Unfor- plastics. (c) To determine the effect of type of
tunately, polymorphic content, which is key to determine pretreatment, conventional vs. green, on the amount of
potential applications, is missing from those works. Thus, hemicellulose and lignin removal, its dependence on the
to our knowledge, overall valorization of side-streams is final properties of the cellulose such as structural, ther-
rarely included in previous reports57,58 which does not mal, morphological, particle size and HHV properties,
allow to accurately predict the final properties of a prod- was analyzed.
uct. In fact, this is one of the reasons why the
nanocellulose extraction process is very difficult to scale-
up, so few pilot plants exist. Given this scenario, the pro- 2 | MATERIALS AND METHODS
duction of valuable materials from biomass residues as
well as the determination of polymorphic content is a The SW, labelled as SWT1 and SWT2, were collected
great challenge around the world but particularly in from community sawmills from Hidalgo and Durango,
developing countries leading to mismanagement of pol- states of México, respectively, which mostly come from
luting waste.63 pine. Biomasses were dried at 60.0 C during 48.0 h and
Unfortunately, as the chemical composition milled through a 0.30 mm mesh using a mill (CT 293
(CC) varies from one region to another according to the Cyclotec model) from FOSS Analytical Co.
type of biomass, it is necessary to study its CC before and Analytical grade chemicals, including ethanol abso-
after being pre-treated to evaluate the quality of samples lute (CH3CH2OH, 99.9%, J.T. Baker), sodium hydroxide
while focusing efforts on minimizing the amounts of (NaOH, 98.0%, J.T. Baker), sodium chlorite (NaClO2,
waste through the valorization. The pretreatments of bio- 80.0%, Sigma Aldrich), acetic acid (CH3COOH, 99.7%,
mass from agro-industrial waste have been the spotlight J.T. Baker), hydrochloric acid (HCl, 36.5-38.0%, Golden
of researchers around the world to extract raw materials Bell), hydrogen peroxide (H2O2, 30.0%, J.T. Baker), sulfu-
for different industrial products. In Mexico, efforts to val- ric acid (H2SO4, 95.0-98.0%, Vohler), acetone (Meyer,
orize biomass from residues are still in progress, espe- technical grade), were used without further purification.
cially at the local communities having rural operations 30.0 g of SWT1 and SWT2 were introduced into cellu-
for wood processing. lose extraction thimbles (Whatman International Ltd.,
For the above reason, this research work contributes, 4.30 12.3 cm) and transferred to the extraction cham-
in communities around the world, to solve the problem ber (500 mL) of the Soxhlet apparatus, which was fitted
of SW waste providing an insight related to chemical pro- with condenser and placed on a round distillation flask
cess to obtain raw materials for biopolymers and so mak- containing 450 mL of CH3CH2OH. Biomasses were
ing the transition to a circular economy. Here, it is extracted to remove waxes and extractives at 85 C for 2 h
important to clarify that although there are many studies under reflux, then, dried at 60 C for 2 h (SWT1- or
stating that cellulose, as a raw material, is a great alterna- SWT2-E). Extractive components were estimated consider-
tive for commercial chemicals, the sources of biomass ing that all the weight loss in the glass thimble is due to
and their treatments need to be firstly studied before those compounds.
industrial scaling, which was an essential part of this To perform the hemicellulose removal, 1.50 g of them
study. Particularly, the study focuses on SW wastes treat- were suspended in a flask containing a solution of 0.10 M
ment from Hidalgo and Durango regions of Mexico (cen- of NaOH at a ratio of 1:20 (w/v), heated using a glycerol
tral and northwest) to extract cellulosic compounds. bath at 100 C for 2 h under constant stirring, filtered
Then, this work is an initial effort to know the funda- under vacuum, washed with hot water until neutrality
mental composition and thermal stability properties of (SWT1-H or SWT2-H). Then, the filtrate was used to precip-
SW biomass after applying alkali and acid conventional itate the hemicellulose by adding 200 ml of acetone into
pretreatments. Additionally, a new GM is also reported it. Solution was let it for 48.0 h at room temperature.
as an alternative to produce rich cellulosic compounds to After, it was filtered using 617 and 590 filter paper and
evaluate the impact in the development of biodegradable the filtrate was centrifugated at 1010 gf to recover a major
thermoplastics. Derived from the above, the investigation part of biopolymer. The recovered solid was dried at 50 C
contemplates the following novelties: (a) perform a for 24 h and storage for further analysis.
deconvolution from DTG curves to propose a method to To extract cellulose from SW (SWT1-C and SWT2-C),
determine the composition of SW in terms of hemicellu- SWT1- or SWT2-H solids were suspended into 30.0 ml of a
lose, cellulose and lignin. (b) According to this 3.00% (w/v) solution of NaClO2 activated with
CH3COOH (1:50 v/v), heated under a glycerol bath at software version 3.12. Crystallinity percentage (%) was
80 C for 2 h, then, filtered under vacuum and washed calculated considering the amorphous and crystalline
with hot water until neutral pH. This last reaction regions of each sample.
required to be repeated once more, giving a total of 8 h of Particle size estimations were performed through
treatment to obtain biomass with higher cellulose con- dynamic light scattering (DLS) analysis using a particle
tent (SWT1- and SWT2-C). The lignin-containing liquid analyzer from Anton Paar (Litesizer 500) company.
residue was also recovered by precipitation using 200 mL 0.100 mg/L of biomass were dispersed in ethanol and fil-
of filtrate with 5.00 mL of HCl. Thereafter, it was allowed tered through a 0.200-μm syringe filter of
to stand for 15.0 min and then centrifuged at 1010 gf. The poly(tetrafluoroethylene) (PTFE) and centrifugated at
remaining solid was recovered and dried at room temper- 4030 gf for 20.0 min to remove the particles of highest
ature for 24 h. To confirm repeatability of extractives size. Then, filtrate was sonicated for 30.0 min. Absor-
removal at each step, procedures were performed more bance and refraction index of samples were analyzed
than 30 times. with an Anton Paar refractometer (Abbemat performance
A green process to extract cellulose from selected- model) equipment (Table S2).
SWT2 (SWT2-C-GM) was performed using a mixture con- The high heating value (HHV) was analyzed in a cal-
sisting of NaOH and H2O2 (10.0 wt%) solutions for 2 h at orimeter pump (IKA-C200). 0.5 g of each biomass was
80 C. Sample was filtered under vacuum and the proce- weighed into a burning crucible, introduced in the adia-
dure was repeated again, filtered and washed until neu- batic pump and burned up to ash using high-purity oxy-
trality. Repeatability was confirmed after ca. 15 times. gen (99.9% of purity) at 3.00 MPa for 12.0 min.
To identify the functional groups of pretreated SW The morphology of selected SWT2 at each pre-
and the possible structural changes at each step pretreatment stage was monitored by scanning electron
treatment, a structural analysis was performed using microscopy (SEM). Ultra-high-resolution field emission
Fourier transform infrared spectroscopy (FT-IR). Analy- (FE) microscope, JEOL JSM-6701F was used to assurance
sis was performed on a Perkin Elmer spectrometer quality observations of the surfaces. Specific used condi-
(Spectrum 100 model) equipped with an attenuated total tions were resolution from 25 to 650,000 at 15 kV and
reflectance (ATR) accessory between 4000 and 400 cm1 a pressure about 1 108 Pa. To avoid biomass degrada-
using 10 scans. An analysis of the residual precipitate, tion under electron beam, samples were coated with
after the alkali and bleaching process was also gold-palladium (Au-Pd) during 30.0 s on a Quorum
carried out. Q150T ES system.
Thermogravimetric and differential ther-
mogravimetric analysis (TGA/DTG) were carried out in a
synchronous thermal analyzer, SDT-Q600 3 | RESULTS A ND DISCUSSION
(TA Instrument Inc.). To acquire the TGA and DTG ther-
mograms, ca. 10.0 mg of samples were placed in alumina 3.1 | Analysis of functional groups
crucibles and analyzed at 30 C for 5.00 min. Then, the during cellulose extraction
analysis was carried out in the temperature range of 30–
700 C under argon atmosphere using 10 C min1. Over- Functional groups monitoring through the three main
lapping holocellulose (HC) signals were deconvoluted by steps of biomass processing on both types of SW can be
Gaussian equation to estimate the percentage contribu- observed in the FT-IR spectra of Figure 1A,B. These fig-
tion of hemicellulose and cellulose. ures display the spectrum of raw SW samples (SWT1 and
CC was also evaluated by analyzing the HC, cellulose, SWT2), after removing wax and pigments (SWT1-E and
hemicellulose and lignin content while considering the SWT2- E), hemicellulose (SWT1-H and SWT2-H) and lignin
ASTM-D 1106,64 ASTM-D 110465 and ASTM-D 110366 (SWT1-c and SWT2-c), respectively. Figure 1C displays the
essays. DTG deconvolution and CC were compared. spectrum of biomass rich in cellulose obtained through
XRD patterns were collected in a Bruker diffractome- GM (SWT2-C-GM). In this Figure, SWT1-C and SWT2-C, are
ter (D8 Advanced model), equipped with Bregg Bentano also included for comparison with spectrum of commer-
geometry, from 10 to 50 (2θ) range at 40.0 kV and cial cellulose.
40.0 mA, using CuKα radiation (λ = 0.154 nm), 0.02 per The following bands were identified: stretching of
step. The main signal of XRD patterns (19–28 ) were ana- hydroxyl groups bonded, OH in cellulose, hemicellulose
lyzed through peak deconvolution of integrated profiles. and lignin (3334 cm1),67 CH2 asymmetric stretching and
Specifically, type I and II polymorphous contributions stretching of CH3 (2922 cm1), CH2 symmetric stretching
were studied to know their presence. In addition, phase in methyl and methylene (2853 cm1),68 C=O stretching
compositional analysis was obtained using the Match! of ester and acetyl in xylans (1740 cm1),69 absorbed
(A) (B)
CH
CH OH COC
OH
C=O
CH
CH ,CH
COH
SWT2
CH
OH
CH2 CH
CC
Transmittance (a.u.)
2
SWT1
COH
CO
CC
SWT2-E
OH
C=C
CH
CO
CO
SWT1-E
C=O
C=C
C=O
CH2
CH2
SWT2-H
CH2
SWT1-H
CH3
C=O
COC
SWT1-C SWT2-C
CH3
4000 3500 3000 2500 2000 1500 1000 4000 3500 3000 2500 2000 1500 1000
Wavenumber (cm ) -1
Wavenumber (cm-1)
(C)
CH
SWT2-C-GM
CH
CH
SWT1-C
OH
CO
COH
CH2
CH
CO
OH
COC
SWT2-C
Commercial CO
cellulose
4000 3500 3000 2500 2000 1500 1000

Wavenumber (cm-1)
F I G U R E 1 FT-IR spectra of functional group monitoring from cellulose extraction process using (A) SWT1, (B) SWT2 samples and
(C) comparison of the extracted celluloses with that obtained through GM and commercial cellulose
OH + conjugated CO of lignin (1650 cm1),70 asymmet- In fact, this band of cellulose and hemicellulose is
ric CH3, symmetric CH3 and CH2 asymmetric bending higher in intensity in SWT1 sample. Similarly, CH3 sym-
modes (1465 cm1),71 CO skeletal stretching + CH3 metric bending in lignin and hemicellulose signals
bending in amorphous zone of cellulose (1370 cm1),72 appears at 1380 cm1 (Δ = 10.0 cm1) in SWT2. SWT2
CH2 symmetric bending in amorphous cellulose I spectrum displays higher-intensity bands of ring
(1420 cm1),73 CO stretching in cellulose and hemicellu- stretching than SWT1 in quinone, aromatic skeletal, and
lose (1377 cm1),74 C-O vibration in guaiacyl rings C=C of aromatic ring + C=O of extractive compounds,
(1260 cm1),75 C-O-C asymmetrical stretching which appear at 1600 and 1506 cm1,78 respectively. This
(1160 cm1),70 C-O-C symmetric stretching + OH associ- suggests that SWT1 may be slightly less abundant of lig-
ating band in cellulose and hemicellulose (1110 cm1),76 nin functional groups than SWT2. Another important
CO stretching of secondary alcohols (1049 cm1),77 OH observation is the presence of CH2 bending vibration in
out of plane deformation of carboxylic acids (945 cm1)77 crystalline cellulose type I at 1425 cm173 in SWT2, which
and C-O-H bending out of plane (720 cm1). The assign- was not present in SWT1. Marked differences were also
ments of both types of SW (SWT1 and SWT2) indicate sim- obtained in the amorphous region of the cellulose in the
ilar functional groups with some bands more intense CH3 vibration (1370 cm1)72 where again the SWT1 sam-
than the others. Compared with SWT1, SWT2 spectra dis- ple showed higher intensity than the counterpart (SWT2).
play a displacement at the C=O bands towards lower Finally, unlike SWT1, SWT2 display a weak C1-O-C
wavenumbers (10.0 ± 1.00 cm1). The displacement only β-glycosidic linkage signal at 898 cm1.79
correlates with the type of biomass source because the After wax and pigments removal treatment (extractive
processing was performed under similar experimental components), an increase of intensity of the OH and
parameters. C-O-C bands in polysaccharides as well as CH of the
lignin was evidenced. Thus, in turn, it allows us to SW and isolated CNC after pretreating SW with a similar
observe other functional groups of lignocellulosic com- procedure using NaOH but apparently all CNC spectra
pounds. In addition, C=O signals become weaker in also show remnant C=O clusters. In addition, Fagbemi
intensity (Figure S1) as consequence of the removal treat- et al.56 conclude from the FT-IR study that the structural
ment. The conjugated CO of lignin, initially detected at and compositional integrity of CNC isolate from SW on
1653 cm1,70 shifts towards lower wavenumbers acid hydrolysis still show apparent signs of C=O groups,
(1645 cm1) while the CH bands corresponding to CH3O which are remnant of hemicelluloses and lignin.
of lignin are reduced. A new band, corresponding to the After bleaching process in SWT1-C, a new band of very
CH2 of the amorphous cellulose, appears after removing weak intensity corresponding to C=O groups was
the extractives. Likewise, additional bands were observed at 1720 cm1 which probably corresponds to
observed, such as those at 896 and 810 cm1 the remnant of hemicellulose or oxidized lignin.91,92 Fur-
corresponding to C-O-C stretching at the β(1 ! 4)- thermore, the high-intensity bands of C-C-, aromatic
glycosidic linkage of cellulose and mannans of rings, in lignin at 1600 and 1506 cm1 seen in SWT1-H
hemicellulose,80 respectively. Both samples, SWT1-e and spectra, disappear after bleaching treatment. Small sig-
SWT2- E, display the CH2 signals of amorphous nals of lignin are observed at 141593 and 1260 cm1,75
(1315 cm1) and crystalline (1335 cm1) cellulose,77 with indicating that they were not completely eliminated dur-
the amorphous phase being the one the highest in inten- ing the process. Similar trend of the reduction of signals
sity. In comparison with SWT1-e, SWT2- E did not show from hemicellulose and lignin was observed in SWT2-C
significant changes after extractive components were samples. In recent SW-related works, lignin-associated
removed. The only change observed was the reduction of FT-IR bands, from biomass after being pretreated with a
C=O band in intensity which agreed with the SWT1-e binary solvent system, indicate that lignin bands are not
spectrum. visible for microcrystalline cellulose (MCC). However,
It is well known that the determination of extractable the MCC spectrum stills shows low-intensity bands, that
compounds has an important role in the inhibition of SW is, commercial products still have residual lignin.94 Addi-
hydrolysis54 however, it is common to isolate lignocellu- tionally, Trevorah et al.59 monitored lignin signals on the
losic compounds without a detailed analysis of the FT-IR spectrum (1720, 1505,1456, and 1320 cm1), which
extractable compounds. On the other hand, other were reduced in intensity reflecting a significant after SW
researches focus on the removal of extractable com- fractioning.
pounds in different media such as ethanol/toluene, cyclo- The FT-IR analysis of both types of biomasses was
hexane/ethanol and ethanol/water,54,81 but the studies compared with commercial cellulose (Sigma Aldrich)
lack of a structural evaluation58,82-84; highlighting the and the results are shown in Figure 1C. The contrast was
value of this work. realized to detect if the raw used cellulose for fabricating
After the NaOH pretreatment, the initial contained products is free of extractives, mainly hemicellulose and
band of the C=O groups (1730 cm1) in acetyl and lignin. As observed, the biomass rich in cellulose
uronic ester of xylans in hemicellulose85 were completely extracted from SWT1 and SWT2 still contains some rem-
removed in both samples (SWT1-H and SWT2-H). This nant of those compounds. Both spectra analyzed above
observation indicates that treatment was effective in agreed well with the bands of the commercial cellulose,
removing almost all the hemicellulose content. For exam- even those representing the hemicellulose and lignin
ple, removal of C=O bands from hemicellulose with remnants. A marked difference is observed with OH-
dilute H2SO4, is also an effective pretreatment for SW.54 band which is very intense compared with SWT1-C and
Another highlighted result is the disappearance of signal SWT2-C. In that Figure, it is also plotted the FT-IR spec-
at 1645 cm1 corresponding to the OH86 and C=O trum of the cellulose extracted from SWT2 through the
groups absorbed in lignin87 because the treatment also GM (SWT2-C-GM). Quite similarity can be observed
eliminates an important part of the lignin content. There- between the samples and the differences only correlate
fore, as a consequence of the hemicellulose removal in with the presence of lignin at 1593 cm1. Likewise, to
samples SWT1-H and SWT2-H, the lignin signals become have greater certainty of the extracted biomass, the sam-
stronger. For example, the intensity of the band of aro- ples were also compared with commercial cellulose prod-
matic ring increases at 1593 cm1.88 Consistent with pre- ucts. In this case, spectra of filter paper and disposable
vious reports, hemicellulose is an unstable compound cups can be observed in Figure S2 in which all bands
when lignocellulosic material is subjected to sodium matched well with FT-IR spectra of the samples under
hydroxide treatment,89 which explained the missing investigation. These observations reveal that although
bands in the FT-IR spectra. A. Macías-Almazan et al.90 there are slight differences on the hemicellulose and lig-
mentioned that there was no appreciable change between nin signals of the analyzed specimens, the cellulose
(A) (B)
CH
COCH
CH
G+S
100 100
C=O +C-O
Transmittance (%)
COC
Transmittance (%)
80
unc
80
CH
OH of glucoronic acid
unc
C=O
β xylan
60 CH
G+S
CH
60
Acetyl C=O
OH CH
CC
Condensed S and G
OH
G+S
40
conj
40
+C=O
Pyranose
C=O
Hemicellulose Lignin
G ring
20
20
H2O
Skeletal
CC
0
0
4000 3500 3000 2500 2000 1500 1000
4000 3500 3000 2500 2000 1500 1000
Wavenumber (cm-1) Wavenumber (cm-1)
F I G U R E 2 FT-IR spectrum of recovered fraction from (A) liquors from NaOH pretreatment (hemicellulose) and (B) liquors from
bleaching process using NaClO2/CH3COOH (lignin)
extraction process is suitable for producing new items and CH2 (2936 cm1), C=O of unconjugated ketone
with quality similar to filter paper and single-use cups. stretching (1715 cm1), C=O of conjugated p-substituted
aryl ketones (1654 cm1), aromatic skeletal with C=O of
syringyl and guaiacyl rings stretching (1594 cm1), aro-
3.2 | Identification of functional groups matic skeletal of syringyl and guaiacyl rings (1507 cm1),
in valorized hemicellulose and lignin from CH stretching of CH3 and CH2 (1454 cm1), aromatic
residues skeletal and CH in plane vibrations (1420 cm1), con-
densed syringyl and guaiacyl rings (in position 5)
The spectrum of the recovered fraction after the NaOH (1331 cm1) as weak signal, guaiacyl ring and C=O
treatment (liquors) of selected-SW process (SWT2) can be stretching (1264 cm1), CH in plane deformation of aro-
observed in Figure 2A. It can be seen the OH stretching matic of guaiacyl syringyl, CO of primary alcohols and
(3300 cm1) and CH stretching (2917 and 2850 cm1) unconjugated C=O stretching (1025 cm1), CH out of
vibrations.39 The signal at 1740 cm1 corresponds to the plane (2, 5 and 6 position in guaiacyl) (823 cm1); signals
carbonyl of acetyl and uronic ester groups.95 The appear- representative of the lignin biopolymer.103 Then, hemi-
ance of this signal is contrary to reports where the lack of cellulose and lignin can be successfully valorized from
this is reported due to the saponification of the ester com- side-streams derived from conventional process to isolate
pounds when using alkaline pretreatments.96 Addition- cellulose, solving the lack of these data in the
ally, the water bending mode (1600 cm1),97 CH2 literature.104-110
bending related to the xylan ring98 and symmetric
stretching vibrations of glucuronic acid groups99 (1465
and 1413 cm1), CH vibrations of carbohydrates on the 3.3 | Thermal stability during cellulose
rings (1370 cm1),39 CO bending (1335 cm1), OH bend- extraction at each step and biopolymers
ing + carboxylic acid vibrations of glucuronic acid side quantification (%) using DTG
group (1242 cm1),31 C-O-C stretching of glycosidic link- deconvolution
ages of xylans (1105, 1081, 1015 cm1),100 pyranose rings
of glucose, galactose, and mannose of Thermal stability of the raw-SWT1 and SWT2 samples and
galactoglucomannans (890 cm1),101 C-C stretching of those obtained after each stage was analyzed by
pyranose ring (780 cm1) at the anomeric region TGA/DTG/thermograms (Figure 3A–D). Table 1 summa-
(700-950 cm1),102 were identified in the spectrum. These rizes the thermal transitions at each treatment during cel-
main functional groups suggest that the removed fraction lulose extraction. SWT1 and SWT2 display weight loss
from liquors consists of the hemicellulose biopolymer. starting from 30 C while ending at 211 (1.45) C (5.83
On the other hand, The FT-IR analysis of the other [0.66] wt%) and 202 (1.02) C (3.99 [0.66] wt%), respec-
recovery fraction before bleaching process indicates that tively. The stage corresponds to the weakly bonded water
the main functional groups correspond to the signals of molecules as well as the hydrolysis reaction of extractive
lignin (Figure 2B). These signals were identified as fol- compounds, that is, dehydration region.111 SWT1 and
lows: OH stretching (3343 cm1), CH stretching of CH3 SWT2 DTG thermograms, display a small exothermic
(A) (B)
100 SWT1 0
SWT1-H
SWT1-C -2
Weight loss (%)

80
DTG (%/°C)
373 °C
60 55 °C SWT1
713 °C
-4
209 °C
SWT1-H
40 I II III -6 SWT1-C
295 °C
20
-8
305 °C 350 °C
0
-10
0 100 200 300 400 500 600 700 800 100 200 300 400 500 600 700
Temperature (°C) Temperature (°C)
(C) (D)
100 SWT2 0
SWT2-H
Weight loss (%)
-2
SWT2-C
DTG (%/°C)
80
376 °C
-4
60
646 °C
SWT2
-6 SWT2-H
40 I II III
-8 308 °C SWT2-C
20
-10 350 °C
0 331 °C
-12
0 100 200 300 400 500 600 700 800 100 200 300 400 500 600 700
Temperature (°C) Temperature (°C)
FIGURE 3 Thermogravimetric and differential analysis thermograms of (A, B) SWT1 and (C, D) SWT2 through their processing
peak between 30 and 80 C (4.80 [0.10] wt%) at DTGpeak Although the decomposition of both biopolymers is

I = 51.20 (0.70 C), and 30 and 65 C (5.88 [0.11] wt%) at overlapped in the same signal, the greatest mass loss was

DTGpeak I = 50.60 (0.36) C), respectively. It is well observed for cellulosic compounds. Finally, the last stage
stablished that the percentage of these peaks is correlated ending at 712.00 (0.57) C (28.03 [0.14] wt%) and 648.00
with weight loss, and then at this stage, SWT2 displays a (1.20) C (28.83 [0.55] wt%) for SWT1 and SWT2 is due to
greater weight loss at low temperatures. the lignin decomposition through the formation of aro-
After these temperatures, a second degradation stage matic, phenols, hydroxyphenols as well as the typical
starts concluding at 373.30 (0.88) C (63.70 [0.14] wt%) compounds of guaiacyl and syringyl rings.115 Compared
and 381.00 (4.55) C (64.00 [0.58] wt%) for SWT1 and with SWT2 in which the DTG curve shows a maximum at
SWT2, in which both SW types, coincide on the DTG cur- DTGpeak III = 546.11 (4.66) C (15.89 [0.29] wt%), SWT1 do
ves at DTGpeak II = 350.00 (1.23) C (43.60 [0.69] wt%) not display lignin signals due to the low amount con-
and DTGpeak II = 349.00 (0.60) C (33.70 [0.45] wt%), tained in the sample. This remark corroborates the FT-IR
respectively. This stage represents the continuous pyroly- observations of high-intensity lignin signals in SWT2.
sis of the hemicellulose together with the cellulose bio- After NaOH treatment, the weight loss starts at 180.96
mass.112 Specifically, this zone is due to the (1.06) C (4.16 [0.11] wt%) and 213.96 (0.59) C (6.20 [0.29]
decomposition of the structures linked by acetal and wt%) for SWT1-H and SWT2-H, respectively. The results
pyranose rings, fragmented into lower molecular weights, showed a clear reduction of the thermal stability ca.
releasing CO, CO2, organic and volatiles compounds 36.0 C (SWT1-H) and 30.0 C (SWT2-H). This stage ends at
from the amorphous hemicellulose and amorphous/ 327.45 (1.19) C (49.40 [0.73] wt%), DTGpeak II = 292.33
crystalline cellulose phases.113,114 Other works have (1.20) C with (64.10 [0.40] wt%) for SWT1-H and 338.33
reported this stage as the degradation of hemicelluloses, (0.74) C (54.30 [0.55] wt%); DTGpeak II = 309.42 (0.39) C
the breaking of the cellulose glycosidic bond and the with 53.40 (0.29) wt%, for SWT2-H. A similar behaviour in
beginning of lignin degradation84; the latter is incorrect bamboo fibers with NaOH pretreatments has been previ-
since lignin begins to degrade at higher temperatures.115 ously reported.116 The third stage of lignin decomposition
10
TABLE 1 Thermogravimetric analysis (TGA) and differential analysis (DTG) transitions for stage during cellulose extraction from SWT1 and SWT2
Char
Td1 offset DTGpeak I Td2 offset DTGpeak II Td3 offset DTGpeak III (700 C)

Sample wt% C wt% C wt% C wt% C wt% C wt% C wt%
a a
SWT1 5.83 211 (1.45) 4.80 51.20 63.70 37.30 43.60 350 (1.23) 28.03 712.00 1.66 (0.11)
(0.66) (0.10) (0.70) (0.14) (0.88) (0.69) (0.14) (0.57)
a a
SWT1-H 4.16 180.96 2.45 51.10 49.40 327.45 64.10 292.33 28.4 712.27 7.92 (0.06)
(0.11) (1.06) (0.19) (0.11) (0.73) (1.19) (0.4) (1.20) (0.14) (0.45)
SWT1-C 12.1 165.42 4.53 50.94 49.90 335.00 48.8 306.60 37.00 577.57 17.40 490.23 0.12 (0.01)
± 0.030 (0.21) (0.21) (0.01) (0.46) (0.71) (0.28) (0.88) (0.02) (0.57) (0.32) (0.14)
SWT2 3.99 202 (1.02) 5.88 50.60 64.00 381.00 33.70 349.00 28.83 (648.00 15.89 546.11 1.72 (0.09)
(0.66) (0.11) (0.36) (0.58) (4.55) (0.45) (0.60) (0.55) (1.20) (0.29) (4.66)
SWT2-H 6.20 213.96 2.80 60.60 54.3 338.33 53.40 309.42 38.0 552.37 12.7 463.7 (0.31) 0.15 (0.02)
(0.29) (0.59) (0.02) (0.36) (0.55) (0.74) ± 0.29 (0.39) (0.26) (0.34) (0.04)
SWT2-C 5.40 95.32 1.11 50.83 68.01 352.22 42.10 331.12 23.40 620.92 (11.40 529.33. 2.06 (0.08)
(0.26) (0.54) (0.11) (0.13) (0.27) (0.68) (0.33) (0.63) (0.43) (1.90) (0.26) (12.70)
a
Not observed.
CÁRDENAS-ZAPATA ET AL.
T A B L E 2 Extractives, hemicellulose, cellulose and lignin percentages estimated from differential analysis (DTG) and chemical
composition (CC)
Extractives (wt%) Holocellulose (wt%) Lignin (wt%) Cellulose (wt%) Hemicellulose (wt%)
Sample CC DTG CC DTG CC DTG CC DTG CC

SWT1 6.43 80.0 78.0 20.0 22.0 31.0 43.0 49.0 35.0
SWT1-C N/A 83.0 91.0 17.0 8.00 32.0 41.0 51.0 51.0
SWT2 9.65 78.0 65.0 22.0 39.0 26.0 39.0 52.0 26.0
a
SWT2-C 80.0 86.0 20.0 13.0 44.0 47.0 36.0 39.0
a a a a a a a
SWT2-C-GM 18.0 58.0
a a a a a a a a
Single-use cup 66.0
a
Undetermined.
is more pronounced in SWT2-H (38.00 [0.26] wt%) 200 C.82 However, SWT1-C and SWT2-C are less stable
between 338.33 (0.74) and 552.37 (0.34) C (DTGpeak than extracted cellulose nanostructures treated by acid

III = 463.70 [0.31] C) (12.7 [0.04] wt%) than in SWT1-H hydrolysis, sodium chlorite, sodium hydroxide and ball
(28.40 [0.14] wt%) at the 327.45 (0.07)–712.27 (0.45) C milling process, respectively.84
range (DTGpeak III not observed), corroborating that the Then, the thermal analysis reveals that alkaline and
highest wt% of decomposed lignin is obtained in SWT2-H. bleaching processes for eliminating hemicellulose and
The bleaching process to remove lignin generates a lignin apparently remove similar amounts of both types
less stable biomass (SWT1-C) losing 12.10 (0.03) wt% until of SWs. This analysis demonstrates that although SWT1-C
165.42 (0.21) C at DTGpeak I = 50.94 (0.01) C (4.53 (0.21) and SWT2-C display slightly less thermal stability than
wt%) which may be due to the high humidity absorption SWT1 and SWT2, both have appropriate thermal proper-
of the cellulose. After this stage, the second decomposi- ties for being processed to obtain a bioplastic product for
tion of cellulose is reached between 165.42 (0.21) and energy applications.
335.00 (0.71) C with a weight loss of 50.8% (DTGpeak To know a percentage estimation of HC and lignin of

II = 306.60 [0.88] C, 48.80 [0.28] wt%). The third stage the final samples, DTG curves were integrated and the
between 335.00 (0.71) and 577.57 (0.57) C is related to area (%) of each signal was determined (Table 2 and
the lignin remnant, 37.00 (0.02) wt% (DTGpeak Table S3). From DTG analysis, SWT1 displays 80.0% of

III = 490.23 [0.14] C with 17.40 (0.32) wt%. On the other HC which is in good agreement with the expected CC
hand, after bleaching process in the SWT2-C samples, a (78.0%). In the case of SWT2, the maximum amount of
more stable cellulose biomass with a weight loss of 5.40 isolated HC was around 65.0% which is 13.0% far from
(0.26) wt% (95.32 [0.54] C) was observed (DTGpeak the optimal value. By evaluating the percentage of lignin

I = 50.83 [0.13] C with 1.11 (0.11) wt%. Cellulose decom- from DTG curves, a percentage between 20.0% and 22.0%
position was observed at 352.22 (0.68) C with 68.01 (0.27) was obtained for both types of SW sources. This repre-
wt% (DTGpeak II = 331.12 [0.63] C (42.10 [0.33] wt%) sents a deviation from 17.0% to 19.0% with respect to CC
while for lignin decomposition is up to 620.92 (1.90) C (39.0%). Integration of DTG curves after cellulose isola-
(23.40 [0.43] wt%) (DTGpeak III = 529.33 [12.70] C with tion showed that SWT1-C and SWT2-C samples contain
11.40 [0.26] wt%). 83.0% and 80.0% of HC, respectively. These values
The comparison of thermal stability with other cellu- showed a low deviation in comparison with the normal-
loses extracted from SW indicates similar behaviour. For ized estimated values from ASTM D1103,66 D1106,64
example, SWT1-C and SWT2-C start to degrade at a similar D1104,65 which were 91.0% and 86.0%, separately. It is
temperature compared with an extracted cellulose treated well known that mismatches between DTG and CC are
with sulfuric acid (200 C). common in this type of systems due to the variability of
The one treated with hydrochloric acid shows a chemical structure and the interactions of three biopoly-
higher thermal stability than SWT1-C and SWT2-C.108 In mers that lead changes on degradation tempera-
addition, they behave very similarly to extracted cellulose tures.117,118 However, the results confirm an adequate
with ethanosolv pretreatment using AlCl3, FeCl3 and extraction of lignocellulosic compounds.
AlCl3 catalysts.110 For example, Goenka et al.118 compared the content
They are even very similar to extracted cellulose from of HC, C, H, L of different samples, such as sugarcane
waste pencil shavings with stable temperatures bagasse, coconut pith, rice husk, SW and wheat husk
demonstrating important differences in dependence of evaluation of CC of single-use cups made of cellulose,

the synthesis method and operating conditions; although, was carried out. Results confirmed that these compounds
unfortunately it fails in the deconvolution of the TGA sig- contains 66.0% of cellulose and 34.0% of a combination of
nals and separation each contributions. hemicelulose and lignin. Another point to consider is
For this reason, in this study, the HC signals on the that if hemicellulose is present in the biomass, it could
DTG plots were also deconvoluted into cellulose and increase the tensile properties.124 Therefore, it could be
hemicellulose to assess the percentage contribution of an advantage when this biomass could be used as bio-
each biopolymer and compare them with the expected plastic reinforcement.
composition (CC). This analysis indicated that in general
there are lower amounts of cellulose compared with
hemicellulose. By comparing them, CC samples display 3.4 | Polymorphous identification and
an opposite trend, that is, the cellulose content is greater compositional phase quantification (%)
than hemicellulose. Differences in the cellulosic com- through X-ray diffraction analysis
pounds were found about 5.00 wt%, which were better
for CC than SW samples. It is important to note that dur- To evaluate the effects of SW pretreatments on the poly-
ing the CC determination, only α-cellulose was consid- morphous phases as well as the crystallinity %, XRD pat-
ered, but it also contains other cellulose polymorphous terns were analyzed taking into account the main
such β- and/or γ-cellulose. Thus, it is recognized that β- diffraction peaks. Results are shown in Figure 4 and
and γ-celluloses can be solubilized by using 17.50% of Table 3. In agreement with PDF # 00-056-1719 and #
NaOH. Therefore, a part of the hemicellulose estimated 00-056-1718 charts, SWT1 and SWT2 patterns were inde-
through CC can be also considered as β- and γ-cellulose xed as α-triclinic and β-monoclinic polymorphous of cel-
under the experimental conditions, which must be ana- lulose type I through the (011), (110), (201), (114) and
lyzed by other methods to clarify the information pro- (231) planes, respectively. After the alkaline pretreat-
vided.119 From these results, it is clear that the low ments, no significant changes were observed in the pat-
concentration of alkaline solution is unable to solubilize terns of both samples. The result seems to be similar after
all the hemicellulose content because it is highly applying the bleaching process to isolate the cellulose.
bounded to lignin, but results are within the range of pre- Some differences that can be highlighted are for example;
vious reports. SWT1-C patterns show a new low-intensity plane (201) at
According to ASTM D1103, the minimum concentra- 26.7 coinciding with the α-phase. It is well known that
tion of NaOH to remove lignin and hemicellulose is polymorphic cellulose typically shows different signals
4.30 M. For this reason, it was proposed soft conditions between the main peak (17.0–30.0 ) that overlaps. It is
using a proposed GM. As a consequence of the mild con- probably that this small signal overlaps with other phases
ditions (0.10 M), a partial separation of lignin and hemi- of the different cellulose phases. In the case of SWT2-C
cellulose from cellulose was expected. The particular patterns, new narrow signals were observed in the range
analysis of the SWT1-C-GM and SWT2-C-GM samples related of 30.9–32.0 and 44.3–45.9 , which seems to correspond
to the composition of the final liquor showed 58.0% of to the triclinic (type I) and monoclinic (type II) phases of
α-cellulose, 18.0% of lignin whereas the balance must cor- cellulose. To confirm and separate the signals from the
respond to hemicellulose. An important point to note is polymorphic cellulose, a Gaussian deconvolution from
that green bleaching process can remove similar amounts the XRD diffractogram was performed at each treatment
of lignin and hemicellulose compared with the tradi- stage for both types of SW (Figure 5A–C). Likewise, a
tional alkaline process. Both, SWT2 analyzed biomasses, spectra analysis of the treated samples through the GM
appears to improve performance than that observed for was performed (Figure 6A–D). In general, the
SWT1. In general, results here obtained agree with those deconvolution of a certain XRD profile has been used to
reported in literature for SW.120,121 The used method can determine the percentage of crystallinity of the cellulose
be justified if the composition of different processed prod- taking into account only the crystalline and amorphous
ucts with commercial cellulose is examined. For example, peaks that appear at 22.0 and 18.0 , respectively; but not
it can be observed that they have some percentage, in to assess the other plane contributions of Type I or Type
some cases significant, of hemicellulose and lignin, such II polymorphic celluloses.125-127 For this reason, signal
as the case of either writing and printing paper122 or separation was performed on the main (110) plane and
newspaper, which typically have 40.0–55.0% of cellulose, the compositions of each phase were estimated using
25.0–40.0% of hemicellulose and 18.0–30.0% of lignin, Match software (Table S4). The results indicated that
respectively.123 In fact, as a part of this study and to con- independently of the SW source, both show a similarity
firm the composition of comercial products, the between the percentages of alpha and beta polymorphs.
F I G U R E 4 X-ray (A) (B)

diffraction patterns of (A) SWT1,
(B) SWT2 at each pretreatment
stage and (C) comparison
among celluloses extracted
(C)
TABLE 3 Compositional phase (%) and crystallinity (%) at the different pretreatment stages of SWT1 and SWT2 samples.
Type I Alpha Type I Beta Type II Crystallinity (%) Rp factor(%)

SWT1 51.0 49.0 — 35.5 10.6
SWT1-H 47.2 32.6 20.0 29.0 6.80
SWT1-C 28.3 0.00 71.3 24.1 10.2
SWT2 49.0 51.0 — 29.8 7.40
SWT2-H 34.6 56.7 8.60 32.4 8.91
SWT2-C 44.6 14.0 41.4 34.4 7.70
SWT2-C-GM 35.0 26.2 38.8 25.5 6.54
The alkaline treatment did not significantly modify the to obtain higher amounts of type II cellulose (38.8%). The
alpha phase but led to the appearance of type II cellulose large quantity of α-cellulose can be potentially used for
in SWT1-H (20.0%). The same behaviour for alpha was the production of paper. It has been stated that there is a
observed in SWT2-H, however, the change of content from relationship with the content of α-cellulose and various
beta phase to cellulose II is very low (8.60%). Bleaching properties such as thermal stability, molecular weight
produces the total disappearance of beta structure gener- and crystallinity, in general, when it is used as a
ating a high percentage of cellulose type II in SWT1-C filler.131,132 In this context, Nieschlag et al.124 demon-
(71.3%). In contrast, SWT2-C consists of 14.0% of beta strated that percentages higher than 34.0% are appropri-
phase and low percentage of type II cellulose (41.4%). ated for these purposes. Thus, the SW as agro-industrial
Therefore, the used process in combination with the type residues, treated through the GM, can be suitable for the
of cellulose source led to transform the cellulose from production of pulp and paper. At this point, it is essential
type I to type II.128-130 to clarify that the percentage contribution of polymorphs
On the other hand, the GM involved a reduction of after being treated by conventional and GMs has not
alpha (35.0%) and beta (26.2%) phases, which in turn led been reported in other works. The closest work was
(A) (B) F I G U R E 5 Deconvolution of

main signal from X-ray
diffraction patterns of (A) SWT1,
(B) SWT1-H and (C) SWT1-C
(C)
(A) (B) F I G U R E 6 Deconvolution of

main signal from X-ray diffraction
patterns of (A) SWT2, (B) SWT2-H,
(C) SWT2-C and (D) SWT2-C-GM
(C) (D)
reported by Samayan et al.133 who identified the presence Likewise, Pires de Figueiredo et al.134 estimated the
of the two phases (cellulose I and II) in powder and fiber amorphous contribution in MCC through Rietveld analy-
diffraction data but without percentage estimations. sis but not the phases present.
(A) (B) (C)
(D) (E) (F)
(G) (H) (I)
F I G U R E 7 Dynamic light scattering analysis of SWT1 and SWT2 samples at each pretreatment stage and its comparison with
commercial cellulose
3.5 | Particle size analysis during nanostructured cellulose and 438 nm for MCC, both
cellulose extraction using acid hydrolysis.84,135 So, it is clear that GM pro-
duces sizes even smaller than those reported for nano-
The hydrodynamic variation of the particle size at each and microcellulose. Thus, this study demonstrates that
stage of the pretreatment was analyzed by DLS using conventional and ecological methods to extract cel-
(Figure 7). It can be observed that the initial size of SWT1 lulose, comparable sizes can be obtained without the
was 247 (16) nm after hemicellulose content is removed. need of acid hydrolysis. Such as is the case of C. Verma
The size becomes higher due to agglomeration of parti- et al.136 who used conventional method followed by acid
cles (7.0 [1.4] μm). However, by removing lignin, SWT1-C hydrolysis to obtain CNC of 120–140, 100–130 and 70–
displays smaller size (228 (4) nm). In contrast, SWT2 dis- 100 nm from softwood, hardwood and non-wood sam-
plays a high initial hydrodynamic particle size compared ples, respectively. A method that can be applied at the
with SWT1 (618 (40) nm), classified as polydispersed. industry has been reported by Souza et al.84 who
After chemical treatment, to remove hemicellulose and extracted nanostructures of cellulose with a minimum
lignin compounds, the size was fairly constant even using and maximum particle size of 61.0 and 1600 nm, respec-
the GM. The hydrodynamic particle size of all samples is tively. As it can be seen, the size of SWT1-C, SWT2-C and
comparable with that observed for commercial cellulose. SWT2-C-GM did not reach the maximum; the methodology
Comparison with other related works showed that hydro- implies four pretreatments (sulfuric acid, sodium chlo-
dynamic particle size is of the order of 192 nm for ride, sodium hydroxide/potassium hydroxide mixture
T A B L E 4 High heating value

Sample HHV (MJ/kg) H (%) VC (%) FC (%)
(HHV), humidity (H), volatile carbon
SWT1 17.2 1.13 (0.06) 94.58 (0.19) 4.29 (0.16) (VC) and fixed carbon (FC) at each
SWT1-H 17.3 1.05 (0.08) 94.59 (0.06) 4.36 (0.18) pretreatment stage of the samples
SWT1-C 15.6 1.23 (0.06) 94.64 (0.09) 4.13 (0.08)
SWT2 18.4 1.68 (0.09) 94.58 (0.10) 4.29 (0.16)
SWT2-E 18.4 — — —
SWT2-H 18.5 5.33 (0.15) 94.59 (0.04) 4.36 (0.18)
SWT2-C 16.5 2.23 (0.06) 94.64 (0.09) 4.13 (0.08)
SWT2-C-GM 16.3 — — —
Commercial cellulose 15.5 — — —
Abbreviations: –, Undetermined; H = Humidity %; VC % = Volatile carbon %, FC = Fixed carbon %.
and then a ball milling with ethanol solution). Other were used to evaluate the changes at each pretreatment
bleached SWs have been reported to have larger sizes stage. From Table 4, it was observed that neither removing
(645 ± 91.4) than SWT1-C, SWT2-C and SWT2-C-GM samples the extractive components nor the hemicellulose, the HHV
confirming that after acid hydrolysis, a small size ca. value does not change substantially because values between
2.8 ± 0.5 nm can be achieved.104 Although the observed 17.2 and 17.3 MJ/kg (SWT1 ! SWT1-H) and 18.4-18.5 MJ/kg
particle size distribution is classified as polydispersity sys- (SWT2 ! SWT2-H) were found. This agrees with the work of
tem, it can be used for the incorporation of other poly- Joshua et al.91 in which the non-extracted sample and
meric systems that require an improvement of the extractive free sample were very close each other of HHV.
interfacial interactions.137 In fact, as indicated above, the Compared with Demirbas et al.141 who indicated that
observed dispersion is not a limitation for the production extractives have the highest HHV, we found that extracts in
of pulp and paper. SW did not influence on the HHV after being removed from
SW. Another work indicating something similar is that of
Telmo and Lousada140 in which it is indicated that HHV is
3.6 | Effect of extractives removal from more related to presence of extractives than to lignin.
sawdust on higher heating value In contrast, when some of the lignin content is
estimations to extract cellulose removed, the HHV changes greatly. The obtained cellu-
loses decreased by 9.30% (SWT1 ! SWT1-C), 10.3%
The HHV data to evaluate the effect of hemicellulose and (SWT2 ! SWT2-C) and 11.4% (SWT2 ! SWT2-C-GM) of
lignin removal from SW samples can be seen in Table 4. their initial HHV value. Among them, the highest HHV
In this table is also included the humidity (H) %, volatile was found for those obtained processing SWT2 with
carbon % and fixed carbon %. From the table, the humid- 16.5 MJ/kg (SWT2-C), using the traditional method, and
ity value in all samples are within the typical ranges of 16.3 MJ/kg applying the GM to isolate the cellulose
natural humidity in the biomass, which is from 5% to (SWT2-C-GM). Comparison with commercial cellulose
10% by weight.138 Previously, Roy and Ray139 reported (15.5 MJ/kg) shows at best, a difference in HHV of
that the volatile matter can be reduced after acid pre- around 0.60% (SWT1-C), 6.10% (SWT2-C) and 4.90%
treatment whereas delignification can increased the vola- (SWT2-C-GM). Then, in contradiction with previous
tile matter content, however, the pretreatment used in reports, we did not find a relationship between the poly-
this work did not show any modification. morphous content with the HHV, but with lignin. Conse-
On the other hand, SWT1 shows a lower HHV value quently, HHV value strongly depends on the lignin
than SWT2, which were ca. 17.2 and 18.4 MJ/kg, respec- content in the biomass.
tively. Different researchers have been previously found
correlation of the HHV with the HC, lignin and extractive
contents.140 A. Demirbas et al.141 found a relationship 3.7 | Morphological analysis of
between HHV with dry, ash-free basis of lignocellulosic extractives removal from sawdust to
materials. In addition, Shafizadeh and DeGroot142 related extract cellulose
the content of HC, lignin and extractives on a dry basis.
Then, continuing with the quantification and correla- Morphology through the pretreatment of selected SWT2
tion of properties as a function of phases, selected samples sample was monitored, see Figure 8. Initially, fibers after
F I G U R E 8 SEM micrographs of
(A) SWT2- E, (B) SWT2-H, (C, D) SWT2-C
and (E) SWT2-C-GM
wax and pigments removal, display a rough morphology biopolymers: biomass mostly rich of cellulose, with
with agglomerated fibers measuring up to 1140 μm and minor amount of hemicellulose and lignin. The detected
consisting of individual fibers c.a. 18.0–40.0 μm, see inset content of polymorphs allows us to suggest polymers in
Figure 8A. After being pretreated to remove most of specific to be used in the processing of these biomasses in
hemicellulose, the fiber morphology become soft, and new bioplastic products whereas the thermal stability led
there is more presence of individual fibers with sizes of to predict the processing temperature if blended with
33.0 and 39.0 μm, which was for the fibrillation process. other types of polymers. Cleaner energy solutions need to
As previously reported in other works, the packed be performed using these biomasses to reduce environ-
together fibers split after alkaline pretreating.143 In this mental impact while finding optimal properties of final
sample, there is the presence of semispherical particles bioplastic products. Then, this work will continue analyz-
on surface in some areas, which are due to dissolution, ing energetic consumption of extrusion and injection
hydrolysis and peeling of hemicellulose during the pro- polymer processing. In addition, as suggested by Soltian
cess.144 In addition, the typical morphology inside of fiber et al.,145 the aspects of the environmental impacts related
can be observed. When cellulose is obtained, individual to the cellulose, hemicellulose and lignin extraction and
fibers among 38.0 and 48.0 nm are more prominent and their conversions, manufacture, use of final products and
easier to detect in the micrographs (Figure 8C,D). This their disposal, through life cycle assessment (LCA), must
feature is detected regardless the performed pretreatment be considered in the near future. Similarly, it is proposed
in SWT2, that is, conventional (Figure 8C) or GM to consider the exergetic analysis associated with techni-
(Figure 8D). cal, economic and environmental approaches to deepen
The above results show that SW from two regions of study of the sustainability of the lignocellulosic perfor-
Mexico can be successfully processed into value-added mance of these processes.146
The main limitation of this study was the large of biopolymers (majority alpha) with potential applications
amount of liquor generated after SW was pretreated with in bioplastic materials. In fact, particle sizes of SWT1-C,
sodium hydroxide and bleached with acetic acid- SWT2-C, and SWT2-C-GM indicate similar processability. The
activated sodium chlorite. However, as it has been application of DTG deconvolution is adequate method to
observed, they can be successfully valorized to precipitate quantify lignocellulosic compounds from decomposition
hemicellulose and lignin by-products. Another limitation temperatures which were found highly stable meaning that
is the amount of water to be neutralized after each biomasses are appropriated to be processed with any kind
pretreatment step. of polymers. As a final point, the results highlighted that
The present study was necessary to be performed the HHV value is quite dependent of the aromatic struc-
before using a by-product, the SW, to evaluate the final tures contained in the biomass.
quality of a biomass rich in cellulose and determine the Through that, we will continue studying SWT1-C,
possible applications in the plastic field. In addition, it SWT2-C and SWT2-C-GM biomasses for processing value
was performed with the intention of finding processing added bioplastic with biodegradable and compostable
conditions to start replacing the typical chlorine-based features and therefore, to advance into products fabri-
method with that more environmentally friendly (the cated from renewable biomass for finding better energy
proposed GM) to obtain cellulose. Results are significant efficiency in plastic processes and renewable clean energy
since from the structural, thermal, optical and heat fea- solutions. Then, some perspective related to the future
tures and CC derived from characterization, we can pre- research work are the following proposal:
dict the properties more accurately than previous
reported works with the used analysis and data treat- • To find energy applications for side-streams (H and L)
ment. Then, the next step is to process the pretreated bio- such as ethanol production and some fuel cells.
masses to find the optimal conditions to obtain a product • A method to process a thermoplastic cellulose with
in the bioplastic field. melting features to obtain moldable products. To pro-
cess blends of SWT1-C, SWT2-C and SWT2-C-GM bio-
masses with biodegradable polymers such as
4 | C ONCLUSIONS A ND F UTURE poly(lactic acid) (PLA) or poly(caprolactone) (PCL)
PERSPECTIVES using compatibilizer agents and different amounts of
biomass and to evaluate final properties finding high
The present study demonstrates that SW biomass of two performance applications.
different origins from Mexico is a source of value-added • To study specific energetic consumption to those
biopolymers which can be used as raw materials for dif- blends while comparing with conventional plastic such
ferent green and clean energy solutions. as PVC, HDPE, PET, among others.
FT-IR measurements indicated that from both • To propose a pilot plant to valorize integrally the SW
sources, it is possible to isolate quality cellulose in ade- by-product to obtain mainly hemicellulose, lignin and
quate yield (30.0%–60.0%). The CC of the samples cellulose to further continuing processing materials at
processed by conventional SW pretreatment allowed to nanoscale.
obtain a biomass rich in alpha cellulose comparable with • Future studies should focus on the direction of
that used for the production of commercial products. research in sustainability aspects such as LCA, exe-
Thermal analysis confirms that both SW samples have rgetic and economic analyses as well as combinations
similar thermal stability because similar amounts of (exergoenvironmental and exergoeconomic analyses)
hemicellulose and lignin are removed during the alkaline to provide costs and environmental loads of processes.
and bleaching processes. Lignin was removed between
30.0%–40.0%, but it was difficult to separate some contri- AUTHOR CONTRIBUTIONS
butions of polymorphic cellulose type Iα dissolved in R. Cardenas-Zapata: Conceptualization, Investigation,
NaOH. Particularly, SWT1-C biomass is proposed to be the Methodology, Validation, Investigation; D. Palma-
most stable sample due to the highest content of cellulose Ramírez: Writing—original draft, Resources, Writing—
polymorphic type II and it can be used for reinforced Review & Editing, Formal analysis, Supervision, Funding
ductile polymer (elastomers) during the production of acquisition; A. I. Flores-Vela: Writing—original draft,
bioplastic applications. In contrast, SWT2-C was found to Resources, Writing—Review & Editing, Formal analysis,
be more abundant in alpha cellulose followed by cellu- Supervision, Funding acquisition; M. A. Domínguez
lose type II which can mainly be used for thermoplastic Crespo: Data curation, Writing—original draft,
applications. In addition, the application of GM to cellu- Writing—Review & Editing, Resources; A.M. Torres—
lose isolation (SWT2-C-GM) lead to obtain similar quality Huerta: Data curation, Writing—original draft,
Writing—Review & Editing, Resources; H. Dorantes- 4. Tsang YF, Kumar V, Samadar P, et al. Production of bioplastic
Rosales: Conceptualization, Data curation of SEM analy- through food waste valorization. Environ Int. 2019;127:
sis, Formal analysis, Resources; S. B. Brachetti-Sibaja: 625-644.
5. Lim C, Yusoff S, Ng CG, Lim PE, Ching YC. Bioplastic made
Conceptualization, Data curation of XRD analysis, For-
from seaweed polysaccharides with green production
mal analysis, Resources. All authors have read and methods. J Environ Chem Eng. 2021;9(5):105895.
agreed published version of manuscript. 6. Okolie JA, Mukherjee A, Nanda S, Dalai AK, Kozinski JA.
Next-generation biofuels and platform biochemicals from lig-
A C K N O WL E D G E M E N T nocellulosic biomass. 2021;45(10):14145-14169.
R. Cardenas-Zapata is grateful for his postgraduate fellow- 7. Tursi A. A review on biomass: importance, chemistry, classifi-
ship to CONACYT and BEIFI. Authors are grateful for cation, and conversion. J Biofuel Res J. 2019;6(2):962-979.
8. Kim M, Lee DJ, Jung S, et al. Valorization of peanut wastes
financial support provided by Instituto Politécnico
into a catalyst in production of biodiesel. Int J Energy Res.
Nacional (IPN) through SIP, 2022-0672, 2022-1111,
2022;46(2):1299-1312.
2022-0548, 2022-0668, 2022-0671, 2022-1153, 2022-1155 9. Lu Q, Zhang X, Yuan S, Xie X. Study of Fe-Ni-Mg catalytic
projects as well as SNI-CONACyT. Authors would like to activities for hydrogen-rich gas production from biomass
thank to D. Paez-Torres, B. Audelo-Rebollar, O. U. pyrolysis. Int J Energy Res. 2021;45(5):7193-7203.
Sanchez-Herrera and ROMFER S.A. de C.V. Company for 10. Muchuweni E, Martincigh BS, Nyamori VO. Organic solar
their assistance with practical work and technical support. cells: current perspectives on graphene-based materials for
electrodes, electron acceptors and interfacial layers. Int J
Energy Res. 2021;45(5):6518-6549.
CONFLICT OF INTEREST
11. Kusmayadi A, Leong YK, Yen HW, Huang CY, Dong CD,
Authors declare no conflict of interest. Chang JS. Microalgae-microbial fuel cell (mMFC): an inte-
grated process for electricity generation, wastewater treat-
DATA AVAILABILITY STATEMENT ment, CO2 sequestration and biomass production. Int J
The data that support the findings of this study are avail- Energy Res. 2020;44(12):9254-9265.
able from the corresponding author upon reasonable 12. Luqman M, Ghiat I, Maroof M, Lahlou FZ, Bicer Y, Al-
request. Ansari T. Application of the concept of a renewable energy
based-polygeneration system for sustainable thermal desalina-
tion process—A thermodynamics' perspective. Int J Energy
ORCID
Res. 2020;44(15):12344-12362.
Roberto C ardenas-Zapata https://orcid.org/0000-0002- 13. Tu H, Zhu M, Duan B, Zhang L. Recent progress in high-
7855-2417 strength and robust regenerated cellulose materials. Adv
Diana Palma-Ramírez https://orcid.org/0000-0003- Mater. 2021;33(28):2000682.
1329-1604 14. Norouzi O, Heidari M, di Maria F, Dutta A. Design of a ter-
Abelardo I. Flores-Vela https://orcid.org/0000-0001- nary 3D composite from hydrochar, zeolite and magnetite
7018-0383 powder for direct conversion of biomass to gasoline. Chem
Eng J. 2021;410:128323.
Miguel A. Domínguez-Crespo https://orcid.org/0000-
15. Norouzi O, Pourhosseini SEM, Naderi HR, Di Maria F,
0001-5382-0756
Dutta A. Integrated hybrid architecture of metal and biochar
Aidé M. Torres-Huerta https://orcid.org/0000-0002- for high performance asymmetric supercapacitors. Sci Rep.
8907-2275 2021;11(1):5387.
Héctor Dorantes-Rosales https://orcid.org/0000-0001- 16. Rajesh M, Manikandan R, Park S, et al. Pinecone biomass-
6973-1766 derived activated carbon: the potential electrode material for
Silvia B. Brachetti-Sibaja https://orcid.org/0000-0001- the development of symmetric and asymmetric super-
9942-4628 capacitors. Int J Energy Res. 2020;44(11):8591-8605.
17. Roldan-San Antonio JE, Martín-Hernandez E, Briones R,
Martín M. Process design and scale-up study for the produc-
R EF E RE N C E S tion of polyol-based biopolymers from sawdust. Sustain Prod
1. Abbas A, Yi YM, Saleem F, et al. Multiwall carbon nanotubes Consum. 2021;27:462-470.
derived from plastic packaging waste as a high-performance 18. Bi H, Lin Q, Wang C, Jiang X, Jiang C, Bao L. An experimen-
electrode material for supercapacitors. Int J Energy Res. 2021; tal study of single unconventional biomass pellets: ignition
45(13):19611-19622. characteristics, combustion processes, and artificial neural
2. Shen M, Song B, Zeng G, et al. Are biodegradable plastics a network modeling. Int J Energy Res. 2020;44(4):2952-2965.
promising solution to solve the global plastic pollution? Envi- 19. Mehmood T, Nadeem F, Qamar SA. Bioconversion of agro-
ron Pollut. 2020;263:114469. industrial waste into value-added compounds. In: Inamuddin,
3. Gironi F, Piemonte V. Bioplastics and petroleum-based plas- Khan A, eds. Sustainable Bioconversion of Waste to Value
tics: strengths and weaknesses. Energ Source A. 2011;33(21): Added Products. Bioconversion of agro-industrial waste into
1949-1959. value-added compounds. Cham: Springer; 2021:349-368.
20. Li J, Lawton DJW, Sacripante GG, Thompson MR, their potentials as film forming materials. Carbohydr Polym.
Marway HS. Process intensification of thermoplastic lignocel- 2021;253:117225.
lulose production through high-solids reactive extrusion 36. Rizwan M, Gilani SR, Durrani AI, Naseem S. Cellulose extrac-
enabled by a novel recycle loop. Ind Eng Chem Res. 2021; tion of Alstonia scholaris: a comparative study on efficiency of
60(38):13886-13894. different bleaching reagents for its isolation and characteriza-
21. Chong TY, Law MC, Chan YS. The potentials of corn waste tion. Int J Biol Macromol. 2021;191:964-972.
lignocellulosic fibre as an improved reinforced bioplastic com- 37. Buendia-Kandia F, Brosse N, Petitjean D, et al. Hydrothermal
posites. J Polym Environ. 2021;29(2):363-381. conversion of wood, organosolv, and chlorite pulps. Biomass
22. Mariano APB, Unpaprom Y, Ponnusamy VK, Ramaraj R. Bio- Convers Biorefin. 2020;10(1):1-13.
ethanol production from coconut pulp residue using hydro- 38. Lan W, Liu C-F, Sun R-C. Fractionation of bagasse into cellu-
thermal and postalkaline pretreatment. Int J Energy Res. 2021; lose, hemicelluloses, and lignin with ionic liquid treatment
45(6):8140-8150. followed by alkaline extraction. J Agric Food Chem. 2011;
23. Baig KS, Wu J, Turcotte G. Future prospects of delignification 59(16):8691-8701.
pretreatments for the lignocellulosic materials to produce sec- 39. Zasadowski D, Yang J, Edlund H, Norgren M. Antisolvent
ond generation bioethanol. Int J Energy Res. 2019;43(4):1411- precipitation of water-soluble hemicelluloses from TMP pro-
1427. cess water. Carbohydr Polym. 2014;113:411-419.
24. Cheah WY, Sankaran R, Show PL, et al. Pretreatment 40. Fernandez-Rodríguez J, Robles E, Gordobil O, et al. Lignin
methods for lignocellulosic biofuels production: current valorisation from side-streams produced during agriculture
advances, challenges and future prospects. Biofuel Res J. 2020; waste pulping and TCF bleaching. Chem Eng Trans. 2016;52:
7(1):1115-1127. 187-192.
25. Mirmohamadsadeghi S, Karimi K, Azarbaijani R, et al. Pre- 41. Chen M, Ma Q, Zhu JY, Martin Alonso D, Runge T. GVL pul-
treatment of lignocelluloses for enhanced biogas production: ping facilitates nanocellulose production from woody bio-
a review on influencing mechanisms and the importance of mass. Green Chem. 2019;21(19):5316-5325.
microbial diversity. Renew Sustain Energy Rev. 2021;135: 42. Dixit M, Gupta GK, Usmani Z, Sharma M, Shukla P.
110173. Enhanced bioremediation of pulp effluents through improved
26. Kong F, Wang L, Chen H, Zhao X. Improving storage prop- enzymatic treatment strategies: a greener approach. Renew
erty of wheat bran by steam explosion. Int J Food Sci Technol. Sustain Energy Rev. 2021;152:111664.
2021;56(1):287-292. 43. Bahtiyari MI, _ Benli H. Comparison of ozone-based cold
27. Xu M, Zeng Q, Li H, et al. Contribution of glycerol addition bleaching processes with conventional pretreatment of cotton.
and algal–bacterial cooperation to nutrients recovery: a study Ozone Sci Eng. 2020;42(5):450-460.
on the mechanisms of microalgae-based wastewater remedia- 44. Shi S-C, Liu G-T. Cellulose nanocrystal extraction from rice
tion. J Chem Technol Biotechnol. 2020;95(6):1717-1728. straw using a chlorine-free bleaching process. Cellulose. 2021;
28. Chen H-Z, Liu Z-H. Steam explosion and its combinatorial 28(10):6147-6158.
pretreatment refining technology of plant biomass to bio- 45. Do NHN, Truong BY, Nguyen PTX, le KA, Duong HM, le PK.
based products. Biotechnol J. 2015;10(6):866-885. Composite aerogels of TEMPO-oxidized pineapple leaf pulp
29. Jha A, Kumar A. Biobased technologies for the efficient and chitosan for dyes removal. Sep Purif Technol. 2022;283:
extraction of biopolymers from waste biomass. Bioprocess 120200.
Biosyst Eng. 2019;42(12):1893-1901. 46. Jing S, Zhao Y, Sun RC, Zhong L, Peng X. Facile and high-
30. Zhou Z, Lei F, Li P, Jiang J. Lignocellulosic biomass to yield synthesis of carbon quantum dots from biomass-derived
biofuels and biochemicals: a comprehensive review with a carbons at mild condition. ACS Sustain Chem Eng. 2019;7(8):
focus on ethanol organosolv pretreatment technology. Bio- 7833-7843.
technol Bioeng. 2018;115(11):2683-2702. 47. Özbek HN, Koçak Yanık D, Fadıloglu S, Gögüş F. Effect of
31. Peng X, Nie S, Li X, Huang X, Li Q. Characteristics of the microwave-assisted alkali pre-treatment on fractionation
water- and alkali-soluble hemicelluloses fractionated by of pistachio shell and enzymatic hydrolysis of cellulose-
sequential acidification and graded-ethanol from sweet maize rich residues. J Chem Technol Biotechnol. 2021;96(2):
stems. Molecules. 2019;24(1):212. 521-531.
32. Moghaddam MK, Karimi E. The effect of oxidative bleaching 48. Teran Hilares R, Ramos L, da Silva SS, Dragone G,
treatment on Yucca fiber for potential composite application. Mussatto SI, Santos JC. Hydrodynamic cavitation as a strategy
Cellulose. 2020;27(16):9383-9396. to enhance the efficiency of lignocellulosic biomass pre-
33. Geng W, Narron R, Jiang X, et al. The influence of lignin con- treatment. Crit Rev Biotechnol. 2018;38(4):483-493.
tent and structure on hemicellulose alkaline extraction for 49. Nazari L, Xu C, Ray MB. Resource utilization of
non-wood and hardwood lignocellulosic biomass. Cellulose. agricultural/forestry residues via fractionation into cellulose,
2019;26(5):3219-3230. hemicellulose and lignin. In: Nazari L, Xu C, Ray MB, eds.
34. Yang B, Zhang S, Hu H, Duan C, He Z, Ni Y. Separation of Advanced and Emerging Technologies for Resource Recovery
hemicellulose and cellulose from wood pulp using a from Wastes. Singapore: Springer Singapore; 2021:179-204.
γ-valerolactone (GVL)/water mixture. Sep Purif Technol. 2020; 50. Kumar P, Barrett DM, Delwiche MJ, Stroeve P. Methods for
248:117071. pretreatment of lignocellulosic biomass for efficient hydrolysis
35. Wang T, Zhao Y. Optimization of bleaching process for cellu- and biofuel production. Ind Eng Chem Res. 2009;48(8):3713-
lose extraction from apple and kale pomace and evaluation of 3729.
51. Esteves CV, Sevastyanova O, Östlund S, Brännvall E. Differ- 66. Materials A.S.f.T.a Method of test for alpha-cellulose in wood.
ences and similarities between Kraft and oxygen deli- ASTM D1103-60 2001.
gnification of softwood fibers: effects on chemical and 67. Elma Karakaş D. New bifunctional carbon material of metal-
physical properties. Cellulose. 2021;28(5):3149-3167. free pomegranate peel catalyst and supercapacitor for highly
52. Pattnaik F, Nanda S, Kumar V, Naik S, Dalai AK. Isolation of efficient hydrogen production and energy storage. 2022;46(2):
cellulose fibers from wetland reed grass through an integrated 1789-1802.
subcritical water hydrolysis-pulping-bleaching process. Fuel. 68. Deng H, Yang W, Cai T, et al. Phase-change composites sili-
2022;311:122618. cone rubber/paraffin@SiO2microcapsules with different
53. Sreeraj, PR, Mishra, SK, Singh, PK. Chapter 6 – characteris- core/shell ratio for thermal management. 2021;45(12):18033-
tic features and functions of nanocellulose for its feasible 18047.
application in textile industry. In: Oraon R, Rawtani D, 69. Wei L, McDonald AG, Freitag C, Morrell JJ. Effects of wood
Singh P, Hussain CM, eds. Nanocellulose Materials: Fabri- fiber esterification on properties, weatherability and bio-
cation and Industrial Applications, Netherlands: Elsevier; durability of wood plastic composites. Polym Degrad Stab.
2022:105-122. 2013;98(7):1348-1361.
54. Benyoucef S, Harrache D, Djaroud S, Sail K, Gallart-Mateu D, 70. Zhuang J, Li M, Pu Y, Ragauskas A, Yoo C. Observation of
de la Guardia M. Preparation and characterization of novel potential contaminants in processed biomass using Fourier
microstructure cellulosic sawdust material: application as transform infrared spectroscopy. Appl Sci. 2020;10(12):4345.
potential adsorbent for wastewater treatment. Cellulose. 2020; 71. Biyada S, Merzouki M, Elkarrach K, Benlemlih M. Spectro-
27:8169-8180. scopic characterization of organic matter transformation dur-
55. Gonzalez G, Ehman NV, Aguerre YS, et al. Quality of micro- ing composting of textile solid waste using UV–visible
fibrillated cellulose produced from unbleached pine sawdust spectroscopy, infrared spectroscopy and X-ray diffraction
pulp as an environmentally friendly source. Waste Biomass (XRD). Microchem J. 2020;159:105314.
Valori. 2022;13:1609-1626. 72. Lin B-J, Colin B, Chen WH, Pétrissans A, Rousset P,
56. Fagbemi OD, Andrew JE, Sithole B. Beneficiation of wood Pétrissans M. Thermal degradation and compositional
sawdust into cellulose nanocrystals for application as a bio- changes of wood treated in a semi-industrial scale reactor in
binder in the manufacture of particleboard. Biomass Convers vacuum. J Anal Appl Pyrolysis. 2018;130:8-18.
Biorefin. 2021. https://doi.org/10.1007/s13399-021-02015-6. 73. Boukir A, Fellak S, Doumenq P. Structural characterization of
57. Xu C, Zhang X, Hussein Z, et al. Influence of the structure Argania spinosa Moroccan wooden artifacts during natural
and properties of lignocellulose on the physicochemical char- degradation progress using infrared spectroscopy (ATR-FTIR)
acteristics of lignocellulose-based residues used as an environ- and X-Ray diffraction (XRD). Heliyon. 2019;5(9):e02477.
mentally friendly substrate. Sci Total Environ. 2021;790: 74. Arthanarieswaran VP, Kumaravel A, Saravanakumar SS.
148089. Characterization of new natural cellulosic fiber from acacia
58. Cavali M, Soccol CR, Tavares D, et al. Effect of sequential leucophloea bark. Int J Polym Anal Charact. 2015;20(4):
acid-alkaline treatment on physical and chemical characteris- 367-376.
tics of lignin and cellulose from pine (Pinus spp.) residual 75. Lehto J, Louhelainen J, Kłosi nska T, Drożdżek M, Alén R.
sawdust. Bioresour Technol. 2020;316:123884. Characterization of alkali-extracted wood by FTIR-ATR spec-
59. Trevorah RM, Huynh T, Brkljača R, Othman MZ. Structural troscopy. Biomass Convers Biorefin. 2018;8(4):847-855.
and morphological analysis of cellulose pulp produced from 76. Bayoumi A, Sarg MT, Fahmy TYA, Mohamed NF, el-
the fractionation of Eucalyptus obliqua sawdust using Zawawy WK. The behavior of natural biomass materials as
γ-Valerolactone. ACS Omega. 2021;6(6):4126-4136. drug carriers in releasing loaded gentamicin sulphate. Arab J
60. Ämmälä A, Sirviö JA, Liimatainen H. Energy consumption, Chem. 2020;13(12):8920-8934.
physical properties and reinforcing ability of microfibrillated 77. Traoré M, Kaal J, Martínez Cortizas A. Differentiation
cellulose with high lignin content made from non-delignified between pine woods according to species and growing loca-
spruce and pine sawdust. Ind Crop Prod. 2021;170:113738. tion using FTIR-ATR. Wood Sci Technol. 2018;52(2):487-504.
61. Monção M, Hrůzova K, Rova U, Matsakas L, 78. Latham KG, Matsakas L, Figueira J, Rova U,
Christakopoulos P. Organosolv fractionation of birch sawdust: Christakopoulos P, Jansson S. Examination of how variations
establishing a lignin-first biorefinery. Molecules. 2021;26(21): in lignin properties from Kraft and organosolv extraction
6754. influence the physicochemical characteristics of hydrothermal
62. Clauser NM, Felissia FE, Area MC, Vallejos ME. Design of carbon. J Anal Appl Pyrolysis. 2021;155:105095.
nano and micro fibrillated cellulose production processes 79. Poyraz B, Tozluoglu A, Candan Z, et al. TEMPO-treated CNF
from forest industrial wastes in a multiproduct biorefinery. composites: pulp and matrix effect. Fibers Polym. 2018;19(1):
Chem Eng Res Des. 2021;167:1-14. 195-204.
63. Haile A, Gelebo GG, Tesfaye T, et al. Pulp and paper mill 80. Richard B, Quilès F, Carteret C, Brendel O. Infrared spectros-
wastes: utilizations and prospects for high value-added bioma- copy and multivariate analysis to appraise α-cellulose
terials. Bioresour Bioprocess. 2021;8(1):35. extracted from wood for stable carbon isotope measurements.
64. Materials A.S.f.T.a Standard test method for acid-insoluble lig- Chem Geol. 2014;381:168-179.
nin in wood. ASTM D1106-21 2021. 81. Samim Y. Esterification of cellulose isolated from black poplar
65. Materials A.S.f.T.a Method of test for Holocellulose in wood. (Populus nigra L.) sawdust with octanoyl chloride. Turk J For.
ASTM D1104-56 1956. 2021;22(3):306-310.
82. Akhlamadi G, Goharshadi EK, Saghir SV. Extraction of cellu- 96. Chaa L, Joly N, Lequart V, et al. Isolation, characterization
lose nanocrystals and fabrication of high alumina refractory and valorization of hemicelluloses from Aristida pungens
bricks using pencil chips as a waste biomass source. Ceram leaves as biomaterial. Carbohydr Polym. 2008;74(3):
Int. 2021;47(19):27042-27049. 597-602.
83. John MJ, Dyanti N, Mokhena T, Agbakoba V, Sithole B. 97. Rajeshkumar G, Hariharan GLD, Maran JP, Al-Dhabi NA,
Design and development of cellulosic bionanocomposites Ponmurugan K. Cellulose fiber from date palm petioles as
from forestry waste residues for 3D. Print Appl. 2021;14(13): potential reinforcement for polymer composites: physico-
3462. chemical and structural properties. Polim Compos. 2021;42(8):
84. Souza AG, de Lima GF, Rodrigues RCLB, Cesarino I, 3943-3953.
Leão AL, Rosa DS. A new approach for conversion of eucalyp- 98. Yuan J, Chen Q, Fang C, Zhang S, Liu X, Fei B. Effect of
tus lignocellulosic biomass into cellulose nanostructures: a chemical composition of bamboo fibers on water sorption.
method that can be applied in industry. J Nat Fibers. 2021; Cellulose. 2021;28(11):7273-7282.
18(10):1501-1511. 99. Khaire KC, Sharma K, Thakur A, Moholkar VS, Goyal A.
85. Li M-F, Fan YM, Xu F, Sun RC, Zhang XL. Cold sodium Extraction and characterization of xylan from sugarcane tops
hydroxide/urea based pretreatment of bamboo for bioethanol as a potential commercial substrate. J Biosci Bioeng. 2021;
production: characterization of the cellulose rich fraction. Ind 131(6):647-654.
Crop Prod. 2010;32(3):551-559. 100. Wu Q, Ren M, Zhang X, et al. Comparison of cd(II) adsorption
86. Mohamed MA, Salleh WNW, Jaafar J, Asri SEAM, Ismail AF. properties onto cellulose, hemicellulose and lignin extracted
Physicochemical properties of “green” nanocrystalline cellu- from rice bran. LWT. 2021;144:111230.
lose isolated from recycled newspaper. RSC Adv. 2015;5(38): 101. Sun S-F, Yang HY, Yang J, Wang DW, Shi ZJ. Integrated
29842-29849. treatment of perennial ryegrass: structural characterization of
87. Kamali-Gharamaleki M, Sadeghi B, Rouhani M, Mirjafary Z. hemicelluloses and improvement of enzymatic hydrolysis of
Nano-pistachio hull-OSO3H: synthesis, characterization and cellulose. Carbohydr Polym. 2021;254:117257.
application as an effective and novel nanocatalyst for one-pot 102. Sun S-F, Yang HY, Yang J, Shi ZJ. The effect of alkaline
synthesis of dihydropyrano [3, 2-b] chromene dione deriva- extraction of hemicellulose on cocksfoot grass enzymatic
tives. React Kinet Mech Catal. 2021;132(1):251-260. hydrolysis recalcitrance. Ind Crop Prod. 2022;178:114654.
88. Fernandes C, Melro E, Magalhães S, et al. New deep eutectic 103. Vazquez G, Antorrena G, Gonzalez J, Freire S. FTIR, 1H and
13
solvent assisted extraction of highly pure lignin from mari- C NMR characterization of acetosolv-solubilized pine and
time pine sawdust (Pinus pinaster Ait.). Int J Biol Macromol. eucalyptus Lignins. Holzforschung. 1997;51:158-166.
2021;177:294-305. 104. Shaheen TI, Emam HE. Sono-chemical synthesis of cellulose
89. Md Salim R, Asik J, Sarjadi MS. Chemical functional groups nanocrystals from wood sawdust using acid hydrolysis. Int J
of extractives, cellulose and lignin extracted from native Biol Macromol. 2018;107:1599-1606.
Leucaena leucocephala bark. Wood Sci Technol. 2021;55(2): 105. Oyewo OA, Mutesse B, Leswifi TY, Onyango MS. Highly effi-
295-313. cient removal of nickel and cadmium from water using
90. Macías-Almazan A, Lois-Correa JA, Domínguez-Crespo MA, sawdust-derived cellulose nanocrystals. J Environ Chem Eng.
et al. Influence of operating conditions on proton conductivity 2019;7(4):103251.
of nanocellulose films using two agroindustrial wastes: sugar- 106. Oyewo OA, Adeniyi A, Sithole BB, Onyango MS. Sawdust-
cane bagasse and pinewood sawdust. Carbohydr Polym. 2020; based cellulose nanocrystals incorporated with ZnO
238:116171. nanoparticles as efficient adsorption Media in the Removal of
91. Li Q, Hu C, Li M, et al. Enhancing the multi-functional prop- methylene blue dye. ACS Omega. 2020;5(30):18798-18807.
erties of renewable lignin carbon fibers via defining the 107. Nkalane A, Oyewo OA, Leswifi T, Onyango MS. Application
structure–property relationship using different biomass feed- of coagulant obtained through charge reversal of sawdust-
stocks. Green Chem. 2021;23(10):3725-3739. derived cellulose nanocrystals in the enhancement of water
92. Caputo D, Fusco C, Nacci A, et al. A selective turbidity removal. Mat Res Exp. 2019;6(10):105060.
cellulose/hemicellulose green solvents extraction from buck- 108. Chuayplod P, Aht-Ong D. A study of microcrystalline cellu-
wheat chaff. Carbohydr Polym Technol Appl. 2021;2:100094. lose prepared from parawood (Hevea brasiliensis) sawdust
93. Di B, Li Z, Lei Y, et al. Phenol-enriched hydroxy waste using different acid types. J Met Mater Miner. 2019;
depolymerized lignin by microwave alkali catalysis to prepare 28(2):106-114.
high-adhesive biomass composites. Polim Eng Sci. 2021;61(5): 109. Trisant Prida N, Gunardi I, Sumarno. The influence of hydro-
1463-1475. lysis time in hydrothermal process of cellulose from sengon
94. Magalhães S, Filipe A, Melro E, et al. Lignin extraction from wood sawdust. Macromol Symp. 2020;391(1):2000016.
waste pine sawdust using a biomass derived binary solvent 110. Ruiz Cuilty K, Ballinas-Casarrubias L, Rodríguez de San
system. Polymers. 2021;13(7):1090. Miguel E, de Gyves J, Robles-Venzor JC, Gonzalez-
95. Marciano JS, Ferreira RR, de Souza AG, Barbosa RFS, de Sanchez G. Cellulose recovery from Quercus sp. sawdust
Moura Junior AJ, Rosa DS. Biodegradable gelatin composite using Ethanosolv pretreatment. Biomass Bioener. 2018;111:
hydrogels filled with cellulose for chromium (VI) adsorption 114-124.
from contaminated water. Int J Biol Macromol. 2021;181: 111. Sharma A, Mohanty B. Thermal degradation of mango (Man-
112-124. gifera indica) wood sawdust in a nitrogen environment:
characterization, kinetics, reaction mechanism, and thermo- 127. Shaikh HM, Anis A, Poulose AM, Al-Zahrani SM, Madhar
dynamic analysis. RSC Adv. 2021;11(22):13396-13408. NA, Alhamidi A, Alam MA. Isolation and characterization
112. Varma AK, Mondal P. Pyrolysis of pine needles: effects of pro- of alpha and Nanocrystalline cellulose from date palm
cess parameters on products yield and analysis of products. (Phoenix dactylifera L.) Trunk Mesh. Polymers. 2021;13(11):
J Therm Anal Calorim. 2018;131(3):2057-2072. 1893.
113. Mishra RK, Mohanty K. Pyrolysis kinetics and thermal behav- 128. Zhang S, Zhang F, Jin L, Liu B, Mao Y, Liu Y, Huang
ior of waste sawdust biomass using thermogravimetric analy- J. Preparation of spherical nanocellulose from waste paper
sis. Bioresour Technol. 2018;251:63-74. by aqueous NaOH/thiourea. Cellulose. 2019;26(8):5177-
114. Nyombi A, Williams M, Wessling R. Determination of kinetic 5185.
parameters and thermodynamic properties for ash (Fraxinus) 129. He H, An F, Wang Y, Wu W, Huang Z, Song H. Effects of pre-
wood sawdust slow pyrolysis by thermogravimetric analysis. treatment, NaOH concentration, and extraction temperature
Energ Sources A. 2018;40(22):2660-2670. on the cellulose from Lophatherum gracile Brongn. Int J Biol
115. Van Nguyen Q, Choi YS, Choi SK, Jeon YW, Kwon YS. Macromol. 2021;190:810-818.
Improvement of bio-crude oil properties via co-pyrolysis of 130. Hafemann E, Battisti R, Bresolin D, Marangoni C,
pine sawdust and waste polystyrene foam. J Environ Manage. Machado RAF. Enhancing chlorine-free purification routes of
2019;237:24-29. Rice husk biomass waste to obtain cellulose nanocrystals.
116. Chen H, Zhang W, Wang X, Wang H, Wu Y, Zhong T, Fei Waste Biomass Valori. 2020;11(12):6595-6611.
B. Effect of alkali treatment on wettability and thermal stabil- 131. Pal K, Chowdhury SG, Mondal D, Chattopadhyay D,
ity of individual bamboo fibers. J Wood Sci. 2018;64(4): Bhattacharyya SK, Mukhopadhyay R. Impact of
398-405. α-cellulose as a green filler on physico-mechanical proper-
117. Freda C, Zimbardi F, Nanna F, Viola E. Mathematical tool ties of a solution grade styrene-butadiene rubber based
from corn Stover TGA to determine its composition. Appl Bio- tire-tread compound. Polym Eng Sci. 2021;61(12):
chem Biotechnol. 2012;167(8):2283-2294. 3017-3028.
118. Goenka R, Parthasarathy P, Gupta NK, Biyahut NK, 132. Gupta PK, Uniyal V, Naithani S. Polymorphic transformation
Narayanan S. Kinetic analysis of biomass and comparison of of cellulose I to cellulose II by alkali pretreatment and urea as
its chemical compositions by Thermogravimetry, wet and an additive. Carbohydr Polym. 2013;94(2):843-849.
experimental furnace methods. Waste Biomass Valoriz. 2015; 133. Samayam IP, Hanson BL, Langan P, Schall CA. Ionic-liquid
6(6):989-1002. induced changes in cellulose structure associated with
119. Kosan B, Römhild K, Meister F, Pelenc V, Kühnel S, enhanced biomass hydrolysis. Biomacromolecules. 2011;12(8):
Gerhardt M. Enzymatic pulp modification: an excellent way 3091-3098.
to expand the raw material base for Lyocell applications? Cel- 134. De Figueiredo LP, Ferreira FF. The Rietveld method as a tool
lulose. 2020;27(11):6577-6590. to quantify the amorphous amount of microcrystalline cellu-
120. Chandrasekaran AP, Sivamani S, Ranjithkumar V. Character- lose. J Pharm Sci. 2014;103(5):1394-1399.
ization of combined organic–inorganic acid-pretreated cassava 135. Bhandari K, Adaval A, Bhattacharyya AR, Maulik SR. Synthe-
stem. Int J Environ Sci Technol. 2017;14(6):1291-1296. sis of microcrystalline cellulose from carpenter waste and its
121. Farhat W, Venditti R, Quick A, Taha M, Mignard N, characterizations. J Nat Fibers. 2020;2020:1-15.
Becquart F, Ayoub A. Hemicellulose extraction and character- 136. Verma C, Chhajed M, Gupta P, Roy S, Maji PK. Isolation of
ization for applications in paper coatings and adhesives. Ind cellulose nanocrystals from different waste bio-mass collating
Crop Prod. 2017;107:370-377. their liquid crystal ordering with morphological exploration.
122. Kumar R, Sharma V, Verma N, Diwan PK, Kumar V, Int J Biol Macromol. 2021;175:242-253.
Kumar V. Analysis of writing/printing paper via ther- 137. Kwak HW, Lee H, Park S, Lee ME, Jin HJ. Chemical and
mogravimetric analysis: application in forensic science. Aust J physical reinforcement of hydrophilic gelatin film with di-
Forensic Sci. 2019;51(1):22-39. aldehyde nanocellulose. Int J Biol Macromol. 2020;146:
123. Chen H, Han Q, Venditti RA, Jameel H. Enzymatic hydrolysis 332-342.
of pretreated newspaper having high lignin content for bio- 138. Aniceto JPS, Portugal I, Silva CM. Biomass-based polyols
ethanol production. Bioresources. 2015;10(3):4077-4098. through Oxypropylation reaction. ChemSusChem. 2012;5(8):
124. Anupam K, Sharma AK, Lal PS, Bist V. Physicochemical, 1358-1368.
morphological, and anatomical properties of plant fibers used 139. Roy R, Ray S. Effect of various pretreatments on energy recov-
for pulp and papermaking. In: Ramawat KG, Ahuja MR, eds. ery from waste biomass. Energ Sources Part A. 2019;2019:1-13.
Fiber Plants: Biology, Biotechnology and Applications. Cham: 140. Telmo C, Lousada J. The explained variation by lignin and
Springer International Publishing; 2016:235-248. extractive contents on higher heating value of wood. Biomass
125. Huang Z, Liu C, Feng X, Wu M, Tang Y, Li B. Effect of regen- Bioenerg. 2011;35(5):1663-1667.
eration solvent on the characteristics of regenerated cellulose 141. Demirbas A, Gullu D, Caglar A, Akdeniz F. Estimation of cal-
from lithium bromide trihydrate molten salt. Cellulose. 2020; orific values of fuels from Lignocellulosics. Energ Source.
27(16):9243-9256. 1997;19(8):765-770.
126. Illa MP, Sharma CS, Khandelwal M. Tuning the 142. Shafizadeh F, Sarkanen KV, Tillman DA. Thermal uses and
physiochemical properties of bacterial cellulose: effect of dry- properties of carbohydrates and Lignins. UK: Academic Press,
ing conditions. J Mater Sci. 2019;54(18):12024-12035. Inc. LTD; 2012.
143. Jaya H, Omar MF, Md Akil H, Ahmad ZA, Zulkepli NN. SU PP O R TI N G I N F O RMA TI O N
Effect of alkaline treatment on sawdust reinforced high den- Additional supporting information may be found in the
sity polyethylene composite under wide strain rate. Mater Sci online version of the article at the publisher's website.
Forum. 2016;840:103-107.
144. Yang Y, Cannon FS. Biomass activated carbon derived from
pine sawdust with steam bursting pretreatment; How to cite this article: Cardenas-Zapata R,
perfluorooctanoic acid and methylene blue adsorption. Bio- Palma-Ramírez D, Flores-Vela AI, et al.
resour Technol. 2022;344:126161.
Valorization of sawdust biomass for biopolymer
145. Soltanian S, Aghbashlo M, Almasi F, et al. A critical review of
extraction via green method: Comparison with
the effects of pretreatment methods on the exergetic aspects of
lignocellulosic biofuels. Energ Conver Manage. 2020;212:112792. conventional process. Int J Energy Res. 2022;1‐24.
146. Rosen MA. Environmental sustainability tools in the biofuel doi:10.1002/er.8112
industry. Biofuel Res J. 2018;5(1):751-752.

Valorization of Sawdust Biomass For Biopolymer Extraction Via Green Method: Comparison With Conventional Process

Uploaded by

Copyright:

Available Formats

Valorization of Sawdust Biomass For Biopolymer Extraction Via Green Method: Comparison With Conventional Process

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Valorization of Sawdust Biomass For Biopolymer Extraction Via Green Method: Comparison With Conventional Process

Uploaded by

Copyright:

Available Formats

Received: 29 October 2021 Revised: 30 April 2022 Accepted: 5 May 2022

SPECIAL ISSUE RESEARCH ARTICLE

Valorization of sawdust biomass for biopolymer extraction

Roberto Cardenas-Zapata1 | Diana Palma-Ramírez1 |

important manner to the development of biodegradable thermoplastics. The

1 | INTRODUCTION materials, such as crosslinking agents, chemicals and

4000 3500 3000 2500 2000 1500 1000

Weight loss (%)

Sample CC DTG CC DTG CC DTG CC DTG CC

demonstrating important differences in dependence of evaluation of CC of single-use cups made of cellulose,

F I G U R E 4 X-ray (A) (B)

Type I Alpha Type I Beta Type II Crystallinity (%) Rp factor(%)

(A) (B) F I G U R E 5 Deconvolution of

(A) (B) F I G U R E 6 Deconvolution of

(A) (B) (C)

(D) (E) (F)

(G) (H) (I)

T A B L E 4 High heating value

Abbreviations: –, Undetermined; H = Humidity %; VC % = Volatile carbon %, FC = Fixed carbon %.

You might also like