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GreenChemistryCutting-edge research for a greener sustainable futurewww.rsc.org/greenchem
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CRITICAL REVIEWG. Chatel et al.Heterogeneous catalytic oxidation for lignin valorization into valuable chemicals: what results? What limitations? What trends?
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McCoy, E. Lee, H. Lee, R. Saremi, C. Feit, I. Hardin, S. Sharma, S. Mani and S. Minko, Green Chem., 2017,
DOI: 10.1039/C7GC01662J.
Green Chemistry
COMMUNICATION
This journal is © The Royal Society of Chemistry 20xx J. Name., 2013, 00, 1-3 | 1
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Received 00th January 20xx,
Accepted 00th January 20xx
DOI: 10.1039/x0xx00000x
www.rsc.org/
Environmentally Sound Textile Dyeing Technology with
Nanofibrillated Cellulose
Yunsang Kim,a Lauren Tolbert McCoy,
a Eliza Lee,
a Hansol Lee,
b Raha Saremi,
a Corbin Feit,
a
Ian R.Hardin,a Suraj Sharma,
a Sudhagar Mani
b and Sergiy Minko*
a
We have developed a sustainable dyeing technology with
nanofibrillated cellulose (NFC) fibers that would decrease the
amount of water, salt and alkali used in cotton dyeing by one
order of magnitude, but with comparable dyeing performance to a
conventional exhaust dyeing method.
Current textile dyeing technology is based on wet processes that
generate copious amounts of wastewater during dyeing, printing,
washing, and finishing.1 Since wastewater that contains pollutants
such as dye, salt, alkali, surfactant, and finishing agents needs to be
specially treated before discharging, it is desirable to diminish the
amount of contaminants beforehand.2-4 Among many dyes and
textile systems, reactive dyes are one of the most used synthetic
dyes for cotton fibers. This is because of their wide range of hues,
stability, and their good dry/wet fastness properties.5 However,
high levels of salt (> 20 g/L) are necessary in reactive dyeing to
mitigate the electrostatic repulsive forces between fibers and
reactive dyes. Thus, the high levels of salt used leave a substantial
environmental footprint in the effluent from the process.6 This
becomes an even greater problem as the regulations for the level of
total dissolved solids (TDS) in effluents becomes stringent.7
Approaches to increasing the utilization of reactive dyes, as well as
reducing the use of salt and alkali in cotton dyeing, involve
mercerization,8 surface modification of textile surfaces,8-14 changing
the molecular structure of reactive dyes, and the optimization of
dye auxiliaries.5, 15 Recent approaches for sustainable textile dyeing
technologies include effluent treatment using activated carbon
membranes,16 enzymatic scouring and H2O2 removal, and ultrasonic
wet processing,17 which would lead to a lower power and water
consumptions. So-called waterless dyeing technologies have also
been proposed including ColorZen18 and DyeCoo.19 Although there
have been some improvements in dye utilization, reduction of
chemicals and wastewater in dyeing, several disadvantages such as
toxic and harmful substances, need for extensive capital
expenditure, and cost still hamper the wide application of new
technologies in industrial settings. Thus, there is still a need for the
development of a more environmentally sound dyeing technology
that leads to a significant reduction of economic and environmental
costs.
Cellulose is a molecule originating in biomass. Cellulose is one of
the most abundant natural materials that feature sustainability, low
environmental/health/safety concerns, and biocompatibility.
Nanocellulose (NC) is engineered, nano-structured cellulose, which
is categorized as nanofibrillated cellulose (NFC), nanocrystalline
cellulose (NCC), or bacterial nanocellulose (BNC), depending on a
production method and/or overall size.20, 21 Because of their low
environmental impact, large surface area, and high reactivity arising
from abundant surface hydroxyls, NCs have found many intriguing
applications in transparent films, barrier layers, membranes,
thermal and mechanical reinforcements, substrate material for
electronics and optics, biocomposites, and food packaging.20-24 Due
to strong affinity for cellulosic substrates mainly via hydrogen
bonding, Van der Waals force, and mechanical interlocking,25-29 NFC
has potential as coating and finishing materials for textiles,
especially cotton fibers that are rich in cellulose (c.a. 95%).
Herein, we report an environmentally sound textile dyeing
technology based on NFC that would reduce the use of water and
chemicals in textile dyeing by one order of magnitude. In this study,
NFC hydrogels are produced by high-pressure homogenization with
carboxymethyl cellulose (CMC) as an additive without the addition
of any toxic chemicals. NFC hydrogels bearing reactive dye
molecules are coated and anchored on the surface of cotton fibers
to complete the coloration of cotton fabrics. With only a fraction of
the water, salt, and alkali, NFC-based dyeing achieved comparable
dyeing and colorfastness performance compared to conventional
exhaust dyeing. Substantial reduction in the use of water and dye
auxiliaries in NFC-based dyeing is also expected to decrease
environmental costs, which is suggested by a gate-to-gate life-cycle
assessment. The developed NFC-based dyeing technology is a facile
and scalable approach that would substantially reduce the
environmental footprint of conventional dyeing processes, given
the greatly reduced level of contaminants as well as the
sustainability of NFC as a raw material.
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2 | J. Name., 2012, 00, 1-3 This journal is © The Royal Society of Chemistry 20xx
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NFC hydrogel is produced by a high-pressure homogenization
starting from cellulose pulp sheets. The procedure for a gel
production is shown pictorially in Fig. S1 (See Electronic
Supplementary Information, ESI). The images from transmission
electron microscopy (TEM, Fig. S2a) and atomic force microscopy
(AFM, Fig. S2b) present isolated nano-size cellulose fibers whose
width and length range from 10 to 50 nm and up to several
micrometers, respectively. NFC gel also exhibits a wide range of
viscosity as a function of shear rate (Fig. S2c), which is an important
feature for printing. Due to its nano-dimension, the specific surface
area of NFC fibers is expected to be substantially large. Among
many methods for determining the surface area of solids, the
adsorption of methylene blue in the liquid phase method has been
widely used.30, 31 From the amount of adsorption (Fig. S3c and S3d)
and the footprint of the methylene blue molecule (130 Å2) on a
solid surface,31 the specific surface of cotton and NFC fibers are
determined to be 5.8 m2/g and 430 m2/g, respectively, which is
about two orders of magnitude difference. The greater surface area
of NFC fibers allows for the larger loading capability, particularly of
the reactive dye molecules in this study.
Table 1 The materials needed to dye 1 kg of cotton fabric by
exhaust dyeing and the NFC-based dyeing (1% dye on the weight of
fabric (owf)) methods.
Reactive
dye
Salt
(Na2SO4)
Alkali
(Na2CO3)
Water
Exhaust
dyeing
10 g 1200 g 76 g 19 L
NFC-based
dyeing
10 g 120 g 7.6 g 1.9 L
A conventional exhaust dyeing method utilizes an exhaustion
dyebath with a copious amount of dye solution, whereas NFC-based
dyeing applies the mixture of NFC-dye containing NFC hydrogel,
reactive dye, and dye auxiliaries (salt and alkali) as a viscous slurry
on the surface of a fabric by printing, which is a commonly
practiced method in pigment printing in the textile industries. The
process flow for each method is compared in Fig. S5. The video
footage of the squeegee printing of the NFC-dye slurry on a cotton
fabric can also be found in ESI. The NFC-dye mixture was set to 5%
(by weight) to match a 20:1 liquor ratio for exhaust dyeing. The
weight ratio of NFC-dye mixture to cotton fabric is 2.0. For example,
5.6 g of the NFC-dye mixture (5% in water) was coated on 2.8 g of
cotton fabric, which resulted in ten times higher dye concentration
in NFC gel than in exhaust dyebath (Table S1). Since the amount of
water required was only 10% in the NFC-based dyeing method
compared to an exhaust method, the same 10 % amount of salt and
alkali was needed to perform the NFC-based dyeing. Table 1
compares the materials used by the two dyeing methods, showing
the notable reduction of dye auxiliaries and water used in the NFC-
based dyeing.
Table 2 summarizes the dyeing performance of dyed cotton
fabrics. In addition to exhaust and NFC-based dyeing, exhaust
dyeing with low salt and alkali concentration was also conducted
and compared. In this practice, the amount of salt and alkali was
the same as in NFC-based dyeing, shown in Table S1. First of all, in
dye exhaustion and fixation, NFC-based dyeing performs
comparably to conventional exhaust dyeing. Despite ten times
higher dye concentration than exhaust dyeing (Table S1), NFC-
based dyeing exhibits a similar level of the uptake and fixation of
dye molecules, which is attributed to the much greater surface area
of NFC than that of cotton fibers. Colorfastness properties of NFC-
based dyeing, including dry/wet crocking and laundering, were also
equivalent to those by exhaust dyeing, except for a lower wet
crocking grade. We ascribe the lower wet crocking grade to the
larger surface area of NFC anchored on a cotton fabric that might
lead to an increase in material transfer while subjected to abrasion
in the crocking test. The colorimetric values of dyed fabrics by NFC-
based dyeing were equivalent to the reference dyeing (Table S2).
The overall dyeing performance of the control exhaust dyeing falls
into the range of values for reactive dye systems reported in
literature.8, 32
Table 2 Dyeing performance of colored cotton fabrics by exhaust dyeing, exhaust dyeing with low concentration of dye auxiliaries, and
NFC-based dyeing. Colorfastness properties are shown as gray scales corresponding to colorfastness grades for staining (crocking) and color
change (laundering) in which higher number indicates less color difference in CIELAB units, i.e., gray scale 5 indicates no color difference.
1% dye owf,
20:1 liquor ratio
Exhaust dyeing Exhaust dyeing with a low
concentration of dye
auxiliaries*
NFC-based dyeing
Dye exhaustion 86% 42% 84%
Dye fixation 78 ± 3 % 31 ± 2 % 88 ± 3 %
Color strength (K/S) after wash-
off
5.6 ± 0.1 1.2 ± 0.1 5.7 ± 0.5
Dye concentration in wash-off
(mg/L)**
6.4 mg/L 8.1 mg/L 5.7 mg/L
Colorfastness to crocking
(dry/wet) (AATCC 8-2013)
5 / 4 5 / 4.5 5 / 3.5
Colorfastness to laundering
(AATCC 61-2013, 2A)
4.5 4.5 4.5
Bending length (mm) (ASTM
D1388)
30.3 ± 1.2 n/a 48.8 ± 5.7
* The amount of salt and alkali was as same as in NFC-based dyeing shown in Table S1.
** Estimated by the calibration curve of absorption at 510 nm for Red Reactive 120.
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Fig. 1. Cotton fabrics colored by (a) a conventional exhaust dyeing
method, (b) an exhaust dyeing method with the lower
concentration of salt and alkali, and (c) the NFC-based dyeing
method. Fabrics before (left column) and after (right) the
accelerated laundering test (AATCC 61-2013, 2A) are shown side by
side.
It should be noted that exhaust dyeing used ten times more salt
and alkali than NFC-based dyeing, which inevitably poses economic
and environmental costs in meeting regulatory compliances for
discharging effluent. With a ten times lower concentration of salt
and alkali, exhaust dyeing exhibited very poor performance with
lower color strength and fixation, leading to much lower dye
utilization. Photographs of dyed fabrics by these three methods are
shown in Fig. 1. Even after the accelerated laundering test, which
mimics five cycles of domestic machine laundering at 38±3°C, NFC-
dyed fabrics exhibit a minimal color change that is reflected in the
same gray scale for color change as exhaust dyeing.
Bending stiffness is one of representative, quantitative measures
of the fabric hand. It depends on the bending behavior of a fabric
and measures with the bending length of a fabric under its own
mass.33 As shown in Table 2, the fabric dyed by the NFC-based
method exhibited a greater bending length by 61% compared with
the reference by the exhaust dyeing method. The increase in
stiffness is attributed to the addition of high-modulus NFC to cotton
as well as increased friction between interwoven cotton fibers.
Approaches to reducing stiffness of the fabrics created by NFC-
based dyeing are ongoing, which include the optimization of NFC
thickness and the use of softener that could reduce friction
between cotton fibers.
The effect of NFC-based dyeing was examined by SEM. An
additional NFC layer on the surface of cotton after NFC dyeing is
clearly seen in Fig. 2b compared to neat cotton fabric in Fig. 2a.
Once anchored, the NFC layer did not lose its structural integrity
after wash-off (30 minutes treatment at boil) and even after five
cycles of laundering in a detergent solution with abrasive action by
steel balls, which are shown in Fig. 2c and 2d, respectively. The
cross-sectional image of NFC-coated cotton fabric (Fig. 2f) shows a
skin-like layer on top of cotton fibers, in which the thickness of NFC
layer was estimated to be 5-10 μm. Since the weight increase after
the NFC dyeing on cotton was 10% (ratio of cotton fabric to dry NC
was 10) and the average thickness of cotton fabric was 200 μm, the
5-10 μm thick NC layer seems reasonable, given the double-sided
coating and the compression of the NFC layer upon printing.
Fig. 2 Top-surface SEM images of (a) neat cotton and (b) NFC-coated cotton fabrics before wash-off, (c) after wash-off, and (d) after
accelerated laundering test. Cross-sectional SEM images of (e) neat cotton and (f) NFC-coated cotton fabrics after laundering test with
arrows pointing at the NFC layer.
a
b
c
a b c
d e f
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The adhesion between cellulosic fibers (NFC and cotton fibers)
was further examined by washing a bilayer consisting of NFC fibrils
deposited on a cellulose model film. The bilayer film was subjected
to washing in a detergent solution at 50°C with mechanical
agitation to test the durability of NFC layer on a cellulose film. As
compared in Fig. S6a and S6b, washing did not remove NFC fibers
on a cellulose film, which indicates strong affinity between the
cellulose in the film and the cellulosic fibers. It is worthwhile to note
that the adhesion between NFC and a cotton fabric would be more
complicated than between NFC and a flat model film due to the
complex morphology of cotton fibers. The possible mechanisms
ofadhesion include intermolecular hydrogen bonds,25, 29 mechanical
interlocking, adsorption, and diffusion of NFC fibers on cotton
fibers.28
To assess the environmental impacts of NFC-based dyeing, a life
cycle impact assessment (LCIA) was performed by using BEES
impact assessment method in the SimaPro package. The gate-to-
gate LCA system boundary for exhaust and NFC-based dyeing
methods are compared in Fig. 3. In this study, LCIA was conducted
for producing one kg of dyed cotton fabric using an exhaust dyeing
and the NFC-based dyeing methods (see Table S3 for detailed data).
Among all environmental impacts, eutrophication is an important
attribute to measure the environmental impacts of products on
water bodies such as rivers, lakes etc. This was calculated based on
g N equivalent emission. The total eutrophication potential for the
exhaust dyeing scenario was 18.93 g N eq., which was four-fold
higher than that of the NFC-based dyeing method (4.31 g N eq.).
The lower eutrophication potential in NFC-based dyeing was due to
the significantly reduced amount of (10 times less) dye auxiliaries,
especially sodium sulfate, compared with a conventional exhaust
method.
Fig. 3 Gate-to-gate LCA system boundary for manufacturing dyed cotton fabric using exhaust and NFC-based dyeing methods.
Water usage (or intake) was also investigated, which corresponds
to the amount of water used for the process from cradle to gate.
We assumed that water used for rinsing in NFC-based dyeing
passed through a nanofilter based on a granular activated carbon
(GAC) treatment method (see Fig. S7) to remove unfixed dye
molecules and reuse until the concentrations of salt and alkali
reached the same concentrations of the effluent from exhaust
dyeing approach. The reusability of wastewater from NFC-based
dyeing in the washing step seems feasible because of the
significantly lower concentrations of alkali and salts. The total water
amount used during the life-cycle of one kg of dyed cotton fabric
was estimated to be 6,306 L for exhaust dyeing and 936 L for NFC-
based dyeing, respectively, which shows substantial reduction by a
factor of 6. Furthermore, if the rinsing stage of textile dyeing can
be completely eliminated by the NFC-based dyeing method, the
new technology could have an indispensable impact on water
footprints for the textiles industry, specifically fabrics and clothes.
NFC-based dyeing impacts could surpass exhaust dyeing in all
environmental areas of concern such as global warming,
acidification, ecotoxicity, smog, natural resource depletion, and
ozone depletion, as shown in Fig. S8.
Acknowledgements
The authors thank Walmart Foundation (Grant number: 7230155)
and Elsevier Foundation for financial support.
Conclusions
In summary, a sustainable textile dyeing technology has been developed using NFC fibers. This technology capitalizes on the large surface area of NFCs and their strong affinity to cotton fibers. NFC-based dyeing achieved a dyeing performance comparable to conventional exhaust dyeing with the reduction of salt and alkali by one order of magnitude. A gate-to-gate life-cycle assessment conducted based on experimental data for NFC-dyeing indicates a substantial reduction in eutrophication potential and wastewater effluent load, which would save significant environmental costs for textile dyeing processes. The sustainability and the facile processing of a NFC hydrogel suggest NFC as a novel and potentially “green” material in textile dyeing and finishing applications.
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Journal Name COMMUNICATION
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9. H. Wang and D. M. Lewis, Coloration Technology, 2002, 118, 159-168.
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