Resources, Conservation & Recycling 149 (2019) 510–520

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Resources, Conservation & Recycling

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Full length article

Sustainable industrial technology for recovery of cellulose from banknote T

production waste and reprocessing into cellulose nanocrystals
⁎
Samy Yousefa,e, , Mohamed Hamdyb, Maksym Tatariantsc, Simona Tuckuted,
Samy Zein El-Abdenb, Linas Kliucininkasc, Arunas Baltusnikasd
a
Department of Production Engineering, Faculty of Mechanical Engineering and Design, Kaunas University of Technology, LT-51424, Kaunas, Lithuania
b
Department of Production Engineering and Design, Faculty of Engineering, Minia University, Minia, Egypt
c
Department of Environmental Technology, Faculty of Chemical Technology, Kaunas University of Technology, LT-50254, Kaunas, Lithuania
d
Lithuanian Energy Institute, Breslaujos 3, LT-44403, Kaunas, Lithuania
e
Department of Production Engineering and Printing Technology, Akhbar Elyom Academy 6th of October, Egypt

A R T I C LE I N FO A B S T R A C T

Keywords: Banknote printing is the industry that has a deep influence on financial operations on market, reflecting the
Banknote economic performance of governments. Therefore, it is surrounded by a great secrecy even when dealing with
Banknote waste production waste and end-of-life products, which are utilized very carefully by controlled combustion or in-
Recycling cineration after crushing using special techniques designed to ensure that the waste does not come into pos-
Cotton recovery
session by third parties. This waste contains significant amounts of cotton, percentage of which sometimes can
Cellulose nanocrystals
reach up to 100% of the weight of banknote paper. It is clear that disposal of such waste by simply incinerating it
Sustainability
is contrary to the principles of sustainability and preservation of resources. In order to achieve these principles,
this research aims to develop a new strategy called “Banknote for Banknote (BFB)” to recover and refine cotton
from Banknote waste and later reuse it in the production of banknote paper or reprocess it into cellulose na-
nocrystals suitable for use in many advanced applications through a sustainable technology. The experiments
were performed only on the Banknote Production Waste (BPW) (which is estimated as ˜3% of the total volume of
Banknote production) because the end-of-life banknotes are usually contaminated with many substances during
the circulation. Some of them can become hazardous to the extent of being contaminated with drugs (e.g.
cocaine, etc.); that requires many additional analyses and special treatment. In the developed technology BPW
was treated by using five sequential processes that were selected based on the banknote design, structure, need
to reach minimum gas emissions and high recovery rate. The technology began from crushing treatment at the
Central Bank for safety reasons, then leaching process was used to dissolve the heavy metals from the ink layer
(Al, Fe, Ni, etc.) and separate other pigment metal elements (Si, Ti, etc.) in the form of suspended particles, while
the dissolution and bleaching stages were employed to dissolve the remaining organic components and purify
the cotton substrate. Finally, acid hydrolysis was used to prepare Cellulose nanocrystals with average size 75 nm
from the purified cotton. Although the experiments were conducted on Egyptian Banknote, the advanced
technology is applicable to all types of cotton based-banknotes with high profitability.

1. Introduction
Banknote printing is one of the oldest, most sensitive, complex and
expensive global industries. For many hundreds of years humanity has
been dealing with gold and silver coins as means of exchange, until, by
the end of the 8th century, paper money (banknotes) appeared as an
alternative to the metallic money in China and slowly started gaining
popularity due to lower weight and ease of handling and carrying in
large quantities. By the beginning of the 19th century, banknotes were
already used all over the world and thus became a part of daily life until
present times. Banknote printing industry therefore can be classified as
one of the oldest ones (Sifat and Mohamad, 2017; Goldberg, 2009).
Banknotes are one of the most secured international commodities,
which are of great importance to practically all the countries of the
world as any currency counterfeiting destabilizes and negatively affects
the economy of said countries (Willis, 2009; Zhu et al., 2015). Although

⁎
Corresponding author at: Department of Production Engineering, Faculty of Mechanical Engineering and Design, Kaunas University of Technology, LT-51424,
Kaunas, Lithuania.
E-mail address: ahmed.saed@ktu.lt (S. Yousef).

https://doi.org/10.1016/j.resconrec.2019.06.026
Received 15 March 2019; Received in revised form 19 May 2019; Accepted 20 June 2019
0921-3449/ © 2019 Elsevier B.V. All rights reserved.
S. Yousef, et al.
the appearance of the banknotes differs from country to country, from
region to region, expressing proudness of historical heritage or illus-
trating national symbols etc., the design of banknote is always char-
acterized by complexity to avoid unsanctioned duplication (Baek et al.,
2018; Badovinac et al., 2010; Shukla, 2017; Bartzsch et al., 2013; Ruiz
et al., 2017). Interestingly, composition and individual components of
typical banknotes are almost identical throughout the world and
banknote production stages are highly similar as well. Banknote paper
can be classified as a durable cloth able to resist accidental washing,
resistant to fading and folding multiple times.
Banknote’s structure is composed of many layers: substrate from
pure cotton or mixed with linen (up to 25%) produced using twin-screw
processing that ensures consistent quality and can achieve the right
“look-and-feel” that people expect. Also, the twin-screw process sim-
plifies inclusion of watermarks, security threads or chemical tracers at
the papermaking phase to make better protected banknotes (Griffin
et al., 2018; Takalo et al., 2014; Soukup et al., 2009). It’s worth men-
tioning that until now there is no global standard specifications for
banknote printing paper and each country or region has its own cur-
rency printing standards. For example, to increase the durability of the
banknotes, in 1988 Australia switched to polymer substrate (Menzies,
2004). Once the initial problems of polymer substrate (resistance to
various destructive factors, such as solar radiation) were solved and
production technology with improved banknote protection was devel-
oped (Lim and Murukeshan, 2017), more than 30 countries decided to
switch to such polymer banknotes (Downham et al., 2017). Many stu-
dies proved the economic effectiveness of polymer substrate; with
printing cost reduced by ˜20%, polymer banknotes show higher peel
strength, may yield greater durability and ensure increased lifetime in
intensive use during their circulation (Varenberg and Tsipenyuk, 2014;
Luján-Ornelas et al., 2018; Van Hove, 2015). However, a large number
of countries around the world is not ready to implement polymer
banknotes due to the high cost of new banknote production lines. Usage
of polymer as a raw material requires many new material inputs and
changes in the manufacturing lines to produce not only the new sub-
strate, but to add new security features, e.g. new security watermarks
(Hardwick et al., 2001; Khanduja, 2017; García-Lamont et al., 2012).
Thus, cotton-based banknotes still remain relevant. Banknote produc-
tion process involves a number of steps before the banknote printing
can begin as illustrated in Fig. 1. During the traditional printing process
banknotes pass through three main stages to obtain the final product,
beginning from offset printing followed by intaglio printing, and let-
terpress printing.
All these stages must be followed by a strict inspection to determine
printing defects, resulting in a relatively big amount of rejected bank-
notes. Many of these defects are found in the thickness of ink layers that
greatly affects performance of the final banknote (Bank of Thailand,
2015). Unfortunately, there is no statistics detailing the exact quantity
of banknote waste generated worldwide, however according to the in-
formation provided by Central Bank of Egypt (CBE) (one of the leading
banks in printing of banknotes in Africa and Middle East) during the
printing of Banknotes in Egypt the rejection rate reaches 3% from the
total number of printed banknotes. Although banknote has proven to be
more practical than coins (Bouhdaoui and Van Hove, 2017; Aitken
et al., 2017), by the end of its lifespan it becomes a burden on the
governments as it has to be completely and safely disposed of. Although
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Resources, Conservation & Recycling 149 (2019) 510–520
paper money has been used for nearly two centuries, very few studies
have been concerned with its recycling due to the strict security system
existing within the banknote production process. As a result, incinera-
tion remains the most used process for disposal of end-of-life banknotes
well as of banknote production waste (BPW). Such disposal approach,
naturally, leads to negative environmental impact – such conclusion
can be drawn from the waste management hierarchy, where incinera-
tion is just one stage above the least recommended waste management
approach (disposal) (Gharfalkar et al., 2015).
There is no classification of waste banknotes in literature, however,
according to their structure (cotton- or linen-based), similar to the
structure of many textiles and paper, it is safe to assume that waste
banknotes can be characterized as cellulose-rich municipal solid waste
(Sebastian et al., 2019; Jeswani and Azapagic, 2016). Most of this
cellulose-based feedstock is contaminated by a number of heavy metals
from dyes, inks, etc., making actual recycling of banknotes quite chal-
lenging as the products of recycling would be contaminated as well. If
this contamination problem was overcome, the base cotton would be
suitable for use as a feedstock to produce biogas, ethanol, etc. using
hydrolysis and fermentation process (Christopher et al., 2017;
Hamawand et al., 2016). Digesting in trifluoroacetic acid (TFA) can be
an alternative solution to treat the banknote waste and directly trans-
form it into bioplastics or convert these digestion products into fuel
molecules. During this treatment, cellulose fraction of the banknote is
dissolved and TFA diesters penetrates into cellulose microfibrils with
some TFA monoesters forming with glucosyl residues of the cellulose
chains (Bayer et al., 2014; Shiga et al., 2017). However, this process
must be conducted in a special ambient at water freezing temperature;
additional concerns are related to the high cost of reagents, their re-
covery and regeneration costs at a commercial scale.
Paper recycling process requires removal of the residual inks en-
trapped in the paper. Presently, chemical deinking process is widely
used to tackle this issue (Petzold and Schwarz, 2015). Some researches
work on biological deinking process that is considered a prospective
alternative to chemical deinking since it allows to avoid the generation
of toxic effluents produced after traditional chemical deinking. In ad-
dition, enzymes used in biological treatment can be much more effi-
cient in separation of certain inks, for example in treatment of Mixed
Office Waste (MOW) papers printed by laser printer and xerox (Saxena
and Singh Chauhan, 2017). The new approach utilizes microbial en-
zymes, which are considered safer than chemicals, however, that pro-
cess still remains under study (Nathan et al., 2018).
Working with similar heavy metal-contaminated textile waste,
Hasanzadeh et al. (2018) applied chemical pre-treatment to recover
purified cotton and produce biogas from it (Hasanzadeh et al., 2018).
Unfortunately, the value of the generated fuel-gas products was very
low when compared with original value of cotton. Life-cycle of cotton-
based textile in not entirely sustainable in this case because the ob-
tained fuel-gas can be used as a source of energy only once before
leaving the loop, whereas cotton, recovered as a raw material, could be
used multiple times. Properly treated banknote waste could become an
alternative source of low-price cotton with sufficient quality to manu-
facture new cotton-demanding products. Introduction of such alter-
native cotton source can decrease demand for virgin cotton and thus
address the issue of water shortage in agricultural lands specializing in
cotton production (Rehman et al., 2019). In this framework, Yehia et al.
Fig. 1. Typical Banknote production process.
S. Yousef, et al.
(2018) used multiple techniques to extract cotton from banknotes in-
cluding soaking with chemicals, screening to separate the detached ink
particles from the soaking step, pulping at high temperature, screening
to separate large nylon pieces and small ink particles, flotation to se-
parate large ink particles and small pieces of nylon, and bleaching as
the final step to increase the whiteness of the product (Yehia et al.,
2018). Although the goal was achieved, the results lacked much pre-
cision and detailed analysis, which are necessary to establish recovered
cotton as a new secondary raw material. In order to treat these issues in
a systematic and profitable way, this research aims to establish a new
strategy called “Banknote for Banknote (BFB)” through development of
integrated, eco-friendly, and sustainable technology for cotton re-
covery, refining. To increase the value of the purified cotton, acid hy-
drolysis was used to prepare Cellulose Nanocrystals (CNCs) from the
purified cotton; such nanocrystals are suitable for use in many ad-
vanced products related to biomedical, hydrogel applications, etc.
(Maciel et al., 2019).
2. Experimental
2.1. Banknote production waste (BPW) selection and pre-treatment
Banknote waste can be divided into types: Banknote Production
Waste (BPW) and end-of-life banknotes. According to the literature, the
end-of-life banknotes are quite often contaminated by various sub-
stances and hazardous microorganisms as a result of continuous cir-
culation. Accordingly, such waste requires special handling and a
number of additional analyses prior to recycling (Carter et al., 2003;
Zarayneh et al., 2018). To avoid these problems, the samples were
taken only from BPW, provided by Central Bank of Egypt (CBE). Sample
diversity factor was taken into account to increase the accuracy of the
final results. Four samples of banknotes with low (1 EP and 5 EP) and
high (100 EP and 200 EP) nominal values were selected. Samples were
given specific codes as illustrated in Fig. 2. Each sample had two se-
curity threads: Holographic Security Thread needed for visual inspec-
tion and magnetic thread for reading by ATMs as shown in Fig. 2.
Size reduction pre-treatment of the selected BPW samples was
started at CBE for security reasons. The samples were crushed into small
pieces (6 × 6 mm max.) in currency disintegration systems for bank-
note printing works CDs-P at optimum crushing conditions using spe-
cial algorithms designed for these banknote series to ensure that they
cannot be reused again. Ink color and size of the crushed samples were
investigated by color imaging using USB Microscope with scale 500 μm
and Metallographic photographies are shown in Fig. 2. As illustrated,
the banknotes were saturated by various inks with different colors,
while the banknote pieces had different size, thickness and structure.
2.2. Morphology and chemical Analysis of the selected samples
Scanning Electron Microscope (SEM) and Energy Dispersive
Spectrometry (EDS) were used to analyze the morphology of the cru-
shed BPW samples. Tungsten (W) grid holder was used during the in-
spection process in order to avoid any measurement overlap between
the metals in the checked samples and holder. Fig. 3 shows the results
of SEM-Mapping analysis performed on the samples. As shown, cotton
fibers had different size and distribution in each sample and were
coated by ink layer. Mapping analysis of the samples showed that their
surface was contaminated by multiple metals including heavy metals
such as Al, Fe, Cr, Ni, etc. There was a large variation in the metal
concentration distribution in mapping images due to the highly variable
nature of ink layer.
2.3. Treatment of the samples and nanocellulose production
The main treatment in the proposed technology is composed of five
sequential processes. Fig. 4 shows the layout of the technology
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Resources, Conservation & Recycling 149 (2019) 510–520
beginning from pre-treatment of the collected banknotes (based on the
conditions listed before), heavy metal leaching and precipitation, se-
paration of ink, polymer, and organic components by float-sink se-
paration, centrifugal separation, and solvent treatment. Finally,
bleaching and chemical reduction are used to respectively purify the
recovered cotton paper and produce the nanocellulose particles. All
these processes and selection of the optimum treatment conditions are
explained in details in the following sections. Since the leached solu-
tions contained more than 11 different metals (as shown in the results
section) additional research that is already out of scope of one article is
needed for their recovery, the current work was instead focused on the
extraction of cotton, polymer threads and reprocessing of cotton into
nanocellulose. The authors also suggest some ways to extract the metals
based on the methods found on the literature.
2.3.1. Ink separation and precipitation
Intaglio inks are widely used in banknote printing and consist of two
main fractions: metallic pigments and organic compounds (ink vehicle)
(Kyrychok et al., 2014). Leaching using nitric acid (HNO3) is widely
used in extraction of metals from different wastes, including E-waste,
solar cell, etc. with high performance in terms of recovery rate and
sustainability (Tatariants et al., 2018b; Yousef et al., 2019a; Tatariants
et al., 2018a). Therefore, leaching process (using HNO3 with con-
centration 60% to avoid cellulose nitration or formation of knecht
compound between nitric Acid and cellulose (Gert et al., 2000)) was
employed in the present research to solubilize metals. Preliminary
leaching was conducted on 1 g 200 EP sample with various concentra-
tions of HNO3 (1, 2, and 2 M) at low-constant temperature 70 °C to
avoid cotton yellowing and decrease the emissions of toxic gases. The
results showed that 2 M HNO3 were sufficient to leach the heavy metals
from the BPW substrate in 8 min.
The main leaching experiments for all samples were conducted
based on the optimum leaching conditions; the leaching time was in the
range 7–10 min. USB Microscope was used to examine the surface
morphology of the original and leached samples with scale 500 μm as
shown in the results section. Finally, heavy metals were recovered from
the leached solutions in form of precipitate by adjusting pH (1.5 to 14)
through addition of NaOH, HCl, H2SO4, etc. followed by filtration
process based on the optimum values obtained by Zhang et al. (2016)
(Zhang et al., 2016). Leaching process can separate heavy metals from
intaglio inks in the form of solution, while other pigment elements (e.g.
Ti, etc.) can be separated in the form of suspended particles with lower
density. Therefore, float-sink separation and filtration were used to
separate the particles from cotton and polymer fraction.
2.3.2. Recovery and purification of cotton paper from polymer
Centrifuge separation was employed to separate the polymer
threads from cotton paper. It was noted that the separated paper was
contaminated with organic components originating from intaglio inks.
Therefore, a dissolution process using DMSO as an eco-friendly solvent
was used to remove any unwanted organic components. The dissolution
process was performed based on the optimum results obtained by
Yousef et al. (2019), 3g:10 mL at 50 °C for 2 h. (Yousef et al., 2019b).
After that, the bleaching process using sodium hypochlorite (the
chlorine content is about 1.5% from the weight of cotton) and diluted
hydrochloric acid (˜2% from the weight of cotton) was employed to
remove the remaining impurities under soundwave treatment for 2 h. at
40 °C (Zhou et al., 2016).
2.3.3. Cotton paper purification and nanocellulose particles production
Based on the literature data, sulfuric acid gave the highest crystal-
linity of nanocrystals compared with other acids including phosphoric
acid, hydrochloric acid and mixture of acetic/nitric acids due to the
higher tendency to promote the breakage of the hydrogen bonds in
crystalline regions of cellulose (Börjesson and Westman, 2015).
Therefore, acid hydrolysis process was performed using sulfuric acid
S. Yousef, et al.
Fig. 2. Images and Metallographic photographies of the selected banknote samples.
(64%) with four experiments with different reaction duration (1, 1.5, 2,
2.5 h.) under ultrasound treatment at temperature 60 °C and solid to
liquid ratio 1 g (cotton)/20 ml (HNO3), resulting in production of four
Cellulose nanocrystal (CNCs) suspensions (Pires et al., 2019).
3. Characterizations
To better understand the mechanism of banknote waste separation,
USB 8 LED light digital microscope microscope was used in this re-
search. Observation began from inspecting the outer surface of the
original untreated samples to determine the common and distin-
guishing sample features. These observations were supported by
Scanning Electron Microscope (SEM, Zeiss EVO MA10) and Energy-
Dispersive X-ray Spectroscopy (EDS, Bruker XFlash® 630). Also, SEM-
EDS was used to analyze and observe separated ink particles and re-
covered cotton paper. Chemical structure of the prepared CNCs was
analyzed by Fourier-Transform Infrared spectroscopy (FTIR, Vertex70
spectrometer, ATR mode, spectral range 3800-800 cm−1, 4 scans/
sample) and X-ray crystallography (XRD, Bruker D8 Advance).
Thermogravimetric Analysis (TGA, PerkinElmer Pyris Diamond TG/
DTA 6300) and Derivative Thermogravimetric Analysis (DTG) were
used to study the thermal behavior the recovered cotton and its de-
composition under nitrogen atmosphere (20 mL/min), heating rate
10 °C/min. Inductively Coupled Plasma-Optical Emission Spectroscopy
(ICP-OES, Varian 715-ES) measurements were used to determine the
chemical composition of the ink layer. Morphology and purification
degree of the synthesized CNCs were examined using High-Resolution
Transmission Electron Microscope (HRTEM: Model JEM- 2100).
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Resources, Conservation & Recycling 149 (2019) 510–520
4. Results and discussions
4.1. Separation mechanism
Fig. 5 shows the metallographic photographies of the untreated
samples with scale 500 μm. As shown, the distinguishing features can
be classified into five categories: intaglio printed ancient Egyptian-
themed images Fig. 5A–D), intaglio printed Islamic-themed images
Fig. 5E-H), micro lettering Fig. 5 I), optically variable printing Fig. 5J,
K), and mix of micro lettering, see-trough features and intaglio printed
images as shown in Fig. 5L). Once the banknote waste was exposed to
leaching treatment, most of these features were eliminated after
breakage of Van-der Waals forces, ionic, covalent bonding, and polar
interactions, etc. depending on the types of dyes and dyeing substrates
Fig. 5M) (Kaufmann and Ravoo, 2010).
By increasing the treatment time all metals dissolved in the leaching
solution or separated as suspensions and cotton paper became clean as
shown in Fig. 5N). Contamination by organic components was removed
and paper was purified by dissolution and bleaching processes, re-
spectively Fig. 5O, P). Besides optical USB microscope, SEM was used to
determine the delamination morphology during each treatment step
and to study the formation of cellulose nanocrystals. Results show that
mechanical pre-treatment caused cracking and formation of many
notches on the outer surface of banknote waste Fig. 5Q). These damage
features began to increase in size under the effect of leaching treatment
Fig. 5R), followed by removal of all organic components from the
substrate after solvent and bleach treatments; at this stage cotton paper
became completely clean Fig. 5R). Acid hydrolysis process facilitated
the decomposition of clean cotton fiber and started to produce cellulose
S. Yousef, et al. Resources, Conservation & Recycling 149 (2019) 510–520

Fig. 3. SEM-Mapping analysis of the crushed BPW samples.

nanocrystal precursor (Sadeghifar et al., 2011). All recovered layers and
components, including cotton, ink, and polymer are discussed in details
in the following sections.
4.2. Analysis of the leached solutions and suspended particles
4.2.1. Concentration of metals in the leached solutions
Inductively Coupled Plasma-Optical Emission Spectroscopy mea-
surements were used to precisely determine the concentrations of
elements in the solution leached from the selected samples, after that
the average percentage of each element was calculated. The ICP ana-
lysis was done for 20 mL of BPW, digested by aqua regia under mi-
crowave treatment. The results showed that the samples were mainly
composed of eleven metals – Pb, Cu, Al, Zn, Ni, Ti, Fe, Cr, Mg, Ca, Si,
with varying average weight percentage in range 0.12–72.72% as in-
dicated in Table 1. Such banknote waste, containing many metals, can
be used as a new source for secondary raw materials to face the
shortage in natural sources. In the literature, a variety of methods have

Fig. 4. Waste banknote separation flowchart.

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Fig. 5. Metallographic-SEM micrographs of the untreated and treated BPW during the different treatment stages and images of cellulose nanocrystals.

been reported to recover these metals through adjusting the pH of the
leached solution followed by precipitation, thus achieving the sustain-
ability concept (Zhou et al., 2015). Also, the ICP analysis indicated the
strong presence of heavy metals (e.g. Al, Cu, Ni, Pb, Zn, Cr, etc.),
therefore a conclusion can be drawn that disposal of BPW by in-
cineration or landfilling can lead to environmental problems due to the
accumulation of these heavy metals in soil causing acidification and
negatively affecting plants, animals and fish (Wang et al., 2018).
4.2.2. Analysis of the suspended particles
SEM-EDS mapping was used to examine the morphology and che-
mical composition of the suspended particles after filtration process.
Fig. 6A–F) shows the SEM-EDS images and mapping analysis of the
recovered particles. As shown in the SEM micrograph, the surface
morphology of all samples was almost identical, samples were in the
shape of micro-size powder. At the same time, EDS mapping revealed
that the recovered particles were mainly composed of the following
metals: Si, Al, Ti, S, and Na as indicated in Fig. 6G). Metal elements are
typically used in inks for coloring and improving the overall appearance

Table 1
Weight composition of the crushed BPW samples.
Sample code Element (mg/L)

Pb Cu Al Zn Ni Ti Fe Cr Mg Ca Si

1 EP 0.53 4.14 20,97 1.70 0.58 0.32 5.28 0.10 9.63 164.9 11.40
5 EP 0.31 4.21 1.95 8.51 5.75 0.25 4.30 — 4.88 121.2 12.84
100 EP — 0.65 25.69 8.99 — 0.32 1.68 — 9.55 127.5 12.29
200 EP — 0.45 5.08 5.05 3.54 0.64 2.01 0.10 5.10 81.6 7.02
Average (mg/L) 0.21 2.36 13.42 6.06 2.47 0.38 3.32 0.05 7.29 123.80 10.89
Average wt.% 0.12 1.39 7.88 3.56 1.45 0.22 1.95 0.03 4.28 72.72 6.39

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Fig. 6. A–C) SEM micrograph of the suspended particles separated from 1 EP, 5 EP, 100 EP, and 200 EP respectively, E, F) EDS mapping analysis, and G) EDS analysis
and materials count in the separated ink particles.

Fig. 7. SEM micrograph of the recovered

cotton fibers at A) 500, B) 200, C) 100, and D)
10 μm.

Fig. 8. (A) SEM micrograph, (B) FTIR spectra, and (B) visual image of the recovered cotton paper.

Fig. 9. A, B) TGA and DTG curves of the recovered cotton fibers from the treated samples.

of dry ink, while Carbon and Oxygen are a major component of any
organic compounds (e.g. ink binders, resins or other additives). The
EDS mapping may lead to a conclusion that the extracted particles are
printing inks (Wang et al., 2018).
4.3. Analysis of the recovered cotton paper
4.3.1. Morphology of the recovered fiber
Fig. 7 shows the SEM morphological analysis of the recovered
cotton after purification with scale 10–500 μm. As shown, the covered
cotton fibers were covered by inks before the treatment became clear as
a result of applied solvent and bleaching treatment. It was clear that the

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Fig. 10. TEM images of the prepared Cellulose nanocrystals.
Fig. 11. XRD pattern of the synthesized cellulose nanocrystals.
Fig. 12. FTIR spectra of the synthesized cellulose nanocrystals.
treated fibers (average thread size 150 nm) did not have significant
changes in the fibril morphology compared to what was observed at the
beginning of the pretreatment; these results are similar to the results
found in the literature (Liu et al., 2019).
4.3.2. Spectroscopic analysis of the recovered cotton paper
The chemical structure of the fiber samples (before and after the
Fig. 13. FTIR spectra of the recovered A) Hologram security thread and B) Magnetic security thread.
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Resources, Conservation & Recycling 149 (2019) 510–520
treatment) was investigated by FTIR spectroscopy. SEM image of the
purified cotton paper, FTIR spectra, and photographies and are pre-
sented in the Fig. 8.
It can be seen that all cotton samples had practically the same cel-
lulose-characteristic FTIR vibrational bands, i.e. OeH stretch, CH bend
and CeO stretch vibrations at 3400 cm−1, 2927 cm−1 and 1043 cm−1,
respectively. Also, SeO bond stretching was detected at 902 cm−1 due
to the sulfate groups present on the surface of the treated fibers. This
means that leaching, dissolution, and bleaching treatment successfully
removed all dyes and contaminating materials from the samples and the
recovered fiber was composed of high purity cotton; these data corre-
spond to the results in the literature (Fan et al., 2012). Regarding the
peak at 1639 cm−1, it is associated with the OeH stretch and corre-
sponds to adsorbed water in cellulose. The absorbance vibrational band
at 1160 cm−1 was attributed to CeOeC asymmetric stretching vibra-
tions associated with cellulose I and cellulose II (this part are explained
in details in Section 4.4) and is more accentuated for the nanocrystal-
line cellulose what means the cellulose nanocrystals started to form (as
shown in SEM micrograph (Fig. 8A)) (Gaspar et al., 2014).
4.3.3. Thermal analysis of the recovered cotton paper
Fig. 9A-B shows TGA and DTG curves of the recovered cotton from
each of BPW samples. As shown in TGA curves, the samples displayed
similar thermal degradation profiles with average total weight loss (wt.
%). The degradation process had four characteristic stages; the first
stage, located between 113 and 224 °C, had a 4.6 wt.% weight loss due
to water and solvent evaporation. The second stage, located between
225 and 292 °C, had a 9.7 wt.% weight loss due to the decomposition of
organic residue remaining from ink. The third stage, which represented
the primary decomposition and was located between 293 and 402 °C,
had a massive 55.6 wt.% weight loss due to cellulose decomposition.
The last degradation stage is attributed to char decomposition and its
devolatilization. DTG curves showed that the decomposition maximum
was located in the range 345–356 °C. These results are similar to the
results obtained by Miranda et al. (2007), suggesting that the developed
approach can be applied for liberation of cotton paper with high purity
and sufficient thermal properties from banknote waste.
S. Yousef, et al.
Table 2
Recycling rate and yield of the developed strategy.
Process Material recovery and synthesis rate (g)
Ink (2.55 wt.%)
Initial weight 1.02
Leaching and float-sink separation 0.73
Centrifugation ——
Dissolution and bleaching ——
CNCs synthesis ——
Recycling rate and yield (%) 71.5%
Table 3
GHGE from the developed strategy.
Recovered material/Energy Kg or kWh/t of BPW Average (kgCO2-eq/ton or 1000 kW h) (Yousef et al., 2018; Agarwal and Jeffries, 2013;
EEA, 2014)
Metallic particles + security threads 67 −18,300
Cotton paper 915 −1,500
Cellulose nanoparticles 888 −48,000
Input energy 1200(25,000) +1472
CO2-eq reduction by the developed approach (kgCO2-eq/t)
4.4. Analysis of synthesized cellulose nanocrystals
Fig. 10 shows HRTEM images of the synthesized CNCs with scale
200 and 100 nm. As illustrated in Fig. 10A, the obtained particles had
high yield and were nano-sized with transparent single layers (nano-
crystals). These particles had spherical and hexagonal shapes without
any undesirable fragments as shown in Fig. 10B, C. The synthesized
layers had clear surfaces with a high degree of flatness, uniform
thickness, average size 70 nm, sharp and straight edges. Dark areas in
the images represent Cellulose nanocrystals aggregating in clusters
(Wulandari et al., 2016). XRD patterns of the synthesized CNCs are
shown in the Fig. 11. As shown in the figure, the sample exhibited peaks
around 14.45°-16.26° and 22.5° which represent typical cellulose-I
structure (the bonds between each cellulose molecule are particularly
strong, which makes cellulose very hard to break down). The cellulose
crystals exhibit characteristic assignments of 110, and 200 planes, re-
spectively (Wulandari et al., 2016).
Finally, Fig. 12 shows FTIR spectra of synthesized CNCs; as a result
of FTIR analysis, FTIR spectra of CNCs having absorbance peaks in the
3400–3320 cm−1 regions are attributed to the stretching and bending
vibrations of the OH groups of cellulose, respectively. The peaks around
2900–2820 cm−1 correspond to CH stretching which is little analyzed,
because cellulose, hemicelluloses, and lignin have similar peak shapes
in this band. Another band at 1642 cm−1 is corresponding to adsorbed
water in cellulose. The peak observed at 1400 cm−1 were attributed to
the symmetric bending of CH2 and were also related to cellulose I, the
band at 1340–1380 cm−1 corresponded to the bending vibrations of the
CeH and CeO groups of the polysaccharides. The absorbance peaks
observed in the 1160 cm−1 range were attributed to CeOeC asym-
metric stretching vibrations associated with cellulose I and cellulose II.
The main difference between these is the crystalline structure, which
changes from cellulose I to II mainly through the way the hydrogen
bonds are organized between cellulose chains. In fact, cellulose II is
more stable than I. The FTIR results are in agreement with various re-
ported values, confirming the obtained particles were high-purity Cel-
lulose nanocrystals (Kumar et al., 2014; Aguayo et al., 2018).
4.5. Analysis of the separated security threads
The chemical structure of the hologram and magnetic security
thread were examined by FTIR as shown in Fig. 13. FTIR spectra ana-
lysis of of the recovered magnetic and hologram security thread from
Resources, Conservation & Recycling 149 (2019) 510–520
Security threads (5.35 wt.%) Cotton paper (92.1 wt.%) Cellulose nanocrystals
2.14 36.84 1
—— ——— ——
1.96 ——— ———
—— 36.62 ———
—— ——— 0.97
91.6% 99.4% 97%
kgCO2-eq /t of WPCBs
−1,230
−1,373
−42,625
+1200(36,800)
−1400(-7060)
the treated samples had the similar peaks. As shown in the FTIR spectra
analysis, the recovered hologram spectra contains several characteristic
peaks at 1700, 1336, 1242, 1155, 1136, 1056, 1010, 918, 821 cm−1,
which are characteristic to the nylon plastic film of the recovered ho-
logram (Itrić and Modrić, 2017). While the FTIR spectra analysis of the
recovered magnetic thread can be identified by several characteristic
peaks at 892, 1052, 1217, 1400–1500, 1718, and 2316 cm−1. The
presence of these peaks indicated that the extracted was made primarily
from chrome (Itrić et al., 2019).
4.6. Assessment of the developed strategy
4.6.1. Recycling rate and yield
Table 2 shows the recycling rate and yield of material recovery from
the BPW samples that was calculated based on the initial and final
masses of recovered fractions. The calculation was performed on 40 g of
BPW (10 g from each series) and was based on the data reported by the
Egyptian Central Bank, where blank (cotton paper), ink, and two se-
curity threads represent 92.1, 2.55, and 5.35 wt.%, respectively from
the total banknote weight. The calculation illustrates that the developed
strategy had a very good performance in recycling of cotton paper
(99.4%) and security threads (91.6%); high efficiency was also
achieved during the production of Cellulose Nanocrystals (97%). As for
the losses, they mostly occurred during filtration, centrifugation, and
washing steps. As a result, recycling rate of ink was low (71.6 wt.%),
especially compared to the other recovered and synthesized compo-
nents due to the fact that some fraction of ink still remained dissolved in
the leaching solution after all extraction steps and this matter is cur-
rently under research by our research group to determine the accurate
percentage.
4.6.2. Greenhouse gas emissions
Finally, Greenhouse Gas Emissions (GHGE) of the developed
strategy was evaluated and calculated based on the same approach
developed by Turner et al. (2015) (Turner et al., 2015), particularly
based on the correction factor (CO2 emissions), amount of each re-
covered or synthesized material, and energy consumption during the
treatment as shown in Table 3. The GGE analysis shows that a sig-
nificant reduction in greenhouse gas emissions can be achieved (-1,400
CO2-eq./ton) (Cotton recovery scenario) and (-7,060 CO2-eq/ton) (CNCs
synthesis scenario).
Finally, the developed strategy achieved promising results in terms
518
S. Yousef, et al.
of recycling rate (> 99% for cotton) and reprocessing the recovered
cotton into cellulose nanocrystals as high added value products with
average size 75 nm and yield 97%. Also, the significant reduction in
GHGE was shown, demonstrating that the developed technology has a
great potential in closing the Circular Economy loop of banknote waste.
5. Conclusions
In this research, the authors developed a new industrial technology
to recover cotton paper from the banknote production waste. The de-
veloped technology is composed of three combined treatments:
leaching, dissolution, and bleaching. The treatments are used to dis-
solve and separate metal and organic components from ink layer (in the
form of suspension or solution) and purify the recovered cotton paper
with recycling rate > 99%. To extend the scope of the developed
strategy and link it to other advanced applications, high purity cellulose
nanocrystals with average size 75 nm were synthesized from the re-
covered cotton using acid hydrolysis with yield 97%. Other components
of banknote waste such as magnetic and hologram security threads
were completely separated with recycling rates 71.5% and 91.6% re-
spectively. According to the developed strategy, more than 915 kg of
material from 1 ton of banknote waste (this value depends on the
chemical composition of feedstock) could be recycled, potentially re-
ducing carbon footprint by −1400 kg of CO2-eq/ton of waste or by
−7060 kg of CO2-eq/ton in (CNCs synthesis scenario). Based on that the
developed strategy can be a promising approach for banknote waste
recycling with high outputs and multiple advantages over currently
worldwide used incineration and landfilling.
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