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GreenChemistryCutting-edge research for a greener sustainable futurewww.rsc.org/greenchem

ISSN 1463-9262

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

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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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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.

Notes and references

1. A. K. Roy Choudhury, in Roadmap to Sustainable Textiles and

Clothing, ed. S. S. Muthu, Springer Singapore, Singapore, 2014, pp. 1-39.

2. Industrial Effluent Guidelines: Part 410 - Textile Mills Point

Source Category, Industrial Effluent Guidelines: Part 410 - Textile Mills Point Source Category, United States Environmental Protection Agency, 1982.

3. T. Robinson, G. McMullan, R. Marchant and P. Nigam, Bioresource Technology, 2001, 77, 247-255.

4. C. Allègre, P. Moulin, M. Maisseu and F. Charbit, Journal of

Membrane Science, 2006, 269, 15-34. 5. D. M. Lewis, Coloration Technology, 2014, 130, 382-412. 6. Cotton: science and technology, edited by Y.-L. Hsieh, CRC Press,

2007. 7. Chapter 95.10.: Treatment requirements for new and expanding

mass loadings of Total Dissolved Solids (TDS), Department of Environmental Protection, Commonwealth of Pennsylvania, 2011.

8. S. Fu, D. Hinks, P. Hauser and M. Ankeny, Cellulose, 2013, 20, 3101-3110.

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9. H. Wang and D. M. Lewis, Coloration Technology, 2002, 118, 159-168.

10. Y. Kitkulnumchai, A. Ajavakom and M. Sukwattanasinitt, Cellulose, 2008, 15, 599-608.

11. N. S. E. Ahmed and R. M. El-Shishtawy, Journal of Materials

Science, 2010, 45, 1143-1153. 12. A. Patiño, C. Canal, C. Rodríguez, G. Caballero, A. Navarro and J.

M. Canal, Cellulose, 2011, 18, 1073-1083. 13. S. Ali, M. A. Mughal, U. Shoukat, M. A. Baloch and S. H. Kim,

Carbohydrate Polymers, 2015, 117, 271-278. 14. L. Fang, X. Zhang, J. Ma, D. Sun, B. Zhang and J. Luan, RSC

Advances, 2015, 5, 45654-45661. 15. D. M. Lewis, in Kirk-Othmer Encyclopedia of Chemical

Technology, eds. W. John and I. Sons, John Wiley & Sons, Inc., Hoboken, NJ, USA, 2004.

16. R. Kant, Natural Science, 2012, 04, 22-26. 17. A. Hasanbeigi and L. Price, Journal of Cleaner Production, 2015,

95, 30-44. 18. ColorZen: How it Works/the Benefits,

http://www.colorzen.com/, (accessed 2017). 19. DyeCoo: CO2 Dyeing Technology, http://www.dyecoo.com/,

(accessed 2017). 20. R. J. Moon, A. Martini, J. Nairn, J. Simonsen and J. Youngblood,

Chemical Society Reviews, 2011, 40, 3941. 21. D. Klemm, F. Kramer, S. Moritz, T. Lindström, M. Ankerfors, D.

Gray and A. Dorris, Angewandte Chemie International Edition, 2011, 50, 5438-5466.

22. L. A. Berglund and T. Peijs, MRS Bulletin, 2010, 35, 201-207. 23. A. Dufresne, Materials Today, 2013, 16, 220-227. 24. H. Wei, K. Rodriguez, S. Renneckar and P. J. Vikesland,

Environmental Science: Nano, 2014, 1, 302. 25. T. Kondo and C. Sawatari, Polymer, 1996, 37, 393-399. 26. K. L. Kato and R. E. Cameron, Cellulose, 1999, 6, 23-40. 27. J. M. B. Fernandes Diniz, M. H. Gil and J. A. A. M. Castro, Wood

Science and Technology, 2004, 37, 489-494. 28. D. J. Gardner, G. S. Oporto, R. Mills and M. A. S. A. Samir,

Journal of Adhesion Science and Technology, 2008, 22, 545-567. 29. R. Sinko, X. Qin and S. Keten, MRS Bulletin, 2015, 40, 340-348. 30. C. Kaewprasit, E. Hequet, N. Abidi and J. P. Gourlot, The Journal

of Cotton Science, 1998, 2, 164-173. 31. J. C. Santamarina, K. A. Klein, Y. H. Wang and E. Prencke,

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Vippola and M. Rissanen, Coloration Technology, 2015, 131, 396-402.

33. F. T. Peirce, Journal of the Textile Institute Transactions, 1930, 21, T377-T416.

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