Journal of Cleaner Production 285 (2021) 124819

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Journal of Cleaner Production

journal homepage: www.elsevier.com/locate/jclepro

Review

Waterless processing of sheep wool fiber in textile industry with

supercritical CO2: Potential and challenges
Faisal Aboelksim Salem Allafi, Md Sohrab Hossain*, Mohd Omar Ab Kadir,
Marwan Abdul Hakim Shaah, Japareng Lalung, Mardiana Idayu Ahmad**
School of Industrial Technology, Universiti Sains Malaysia, 11800, USM, Penang, Malaysia

a r t i c l e i n f o a b s t r a c t

Article history: Raw sheep wool contains various impurities such as wax, suint, dirt, and microorganisms. Water-based
Received 7 March 2020 cleaning process of sheep wool requires toxic volatile organic compounds that generate a significant
Received in revised form portion of toxic effluents. Supercritical CO2 (scCO2) is a waterless technology that has been utilized for
21 October 2020
sterilization, extraction, cleaning, and drying in various manufacturing sectors. The application of the
Accepted 22 October 2020
scCO2 technology in sheep wool processing is cleaner, as it avoids the generation of toxic effluents. scCO2
Available online 26 October 2020
is a promising technology that can be simultaneously utilized in sheep wool processing for sterilization,
Handling editor: Prof. Jiri Jaromir Kleme
s extraction of lanolin, and cleaning and drying. Therefore, the present study was conducted to evaluate
the potential and limitations of the use of the scCO2 technology for sheep wool processing. Moreover, the
Keywords: properties of sheep wool, the impurities associated with sheep wool fiber, and treatment technology are
Cleaner production discussed.
Waterless technology © 2020 Elsevier Ltd. All rights reserved.
Sheep wool
Supercritical CO2
Wool wax

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2. Sheep wool . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.1. Production, properties, and structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.2. Utilization of sheep wool fiber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.3. Impurities and biological hazards of sheep wool fiber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
3. Sheep wool fiber processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
3.1. Pulsed electrohydraulic discharge (PED) for wool fiber cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
3.2. Ultrasonic-assisted industrial wool scouring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.3. Solvent wool scouring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.4. Detergent wool scouring with an alkaline builder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3.5. Limitations of the existing sheep wool processing process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
4. Supercritical carbon dioxide technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
4.1. Supercritical carbon dioxide as an extraction technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
4.2. Supercritical carbon dioxide as a sterilization technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
4.3. Supercritical carbon dioxide as a cleaning and drying technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
4.4. Potential and challenges of scCO2 technology in sheep wool processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
5. Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Declaration of competing interest . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

* Corresponding author.
** Corresponding author.
E-mail addresses: sohrab@usm.my (M.S. Hossain), mardianaidayu@usm.my
(M.I. Ahmad).

https://doi.org/10.1016/j.jclepro.2020.124819
0959-6526/© 2020 Elsevier Ltd. All rights reserved.
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

1. Introduction extensively utilized in various industrial fields for the extraction

and separation of bioactive compounds (Hossain et al., 2016a;
Wool, an excellent natural protein fiber derived from animals, Vardanega et al., 2019), the sterilization of biomaterials to remove
e.g. sheep, has been widely utilized in the production of clothing biological hazards (Hossain et al., 2016b; Soares et al., 2019), and
materials and technical textiles in the medical, aerospace, auto- the cleaning of the surfaces of fabric materials to remove dirt and
motive, and decoration fields. It is a major raw material in the fabric other impurities (Aslanidou et al., 2016). In the scCO2 technology,
industry. The demand for wool fabric materials is increasing due to fluid CO2, which is a gas at ambient temperature, is used as the
their high quality and excellent mechanical properties, such as solvent. Therefore, the scCO2 technology does not produce any
good flexibility, high heat retention, high hygroscopicity, high stain residue after treatment. It offers numerous advantages as a cleaner
and static resistances, tender luster, high igniting temperature, and sterilization technology, such as easy separation, shorter processing
soft handling (Niu et al., 2012; Patnaik et al., 2015). Sheep wool is a time, environment-friendliness, waterless nature, high solubility,
keratin fiber. The chemical characteristics of sheep wool are asso- and treatment of heat-sensitive materials without causing damage
ciated with its semi-crystallized protein polymer structure, which (Hossain et al., 2016b). The implementation of the scCO2 technol-
consists of various types of amino acids linked through peptide ogy in the textile industry for treating wool and fabric materials has
bonds. However, raw sheep wool is a dirty natural fiber because it been studied (Long et al., 2013; Zheng et al., 2016). Thus, the scCO2
contains high levels of impurities, including wax, grease, suint, technology could be utilized as an effective alternative technology
mineral soil, dead skin, dust, vegetable matter (VM), and dags for conventional steam-based treatment. Therefore, the present
(Bertini et al., 2013). The impurities on the surface of raw wool fiber study was conducted to summarize the existing methods of sheep
need to be removed through cleaning processes prior to its use as a wool processing and their impact on sheep wool properties and
textile material. In the textile industry, wool fibers are subjected to structure. Subsequently, the implementation of the scCO2 tech-
a series of water-based treatment processes such as scouring, nology as a waterless alternative for conventional steam-based
washing, bleaching, fulling, carbonization, and functional finishing technology was assessed. Finally, the potential and limitations of
(Abecia et al., 2005; Patnaik et al., 2015). These processes involve the use of the scCO2 technology for sheep wool processing were
the use of large volumes of water and chemicals, which conse- also discussed.
quently generate huge volumes of toxic effluents from wet-
chemical treatment processes. 2. Sheep wool
The high dependence on water-based treatment is a major
environmental concern in the textile industry due to the associated 2.1. Production, properties, and structure
generation of significant amounts of wastewater with pollutants
(Holkar et al., 2016). The wastewater generated during sheep wool Wool is a natural fiber whose specifications are determined by
processing poses serious environmental and economic concerns, as several production variables. According to the statistics reported by
effective treatment is required to remove impurities prior to the the International Sheep Wool Organization, the worldwide pro-
discharge or recycling of water (Holkar et al., 2016; Poole and Cord- duction of clean sheep wool was estimated to be approximately
Ruwisch, 2004). Due to the detrimental impact of existing sheep 1.155 million kg in 2018 (IWTO, 2019). Generally, sheep wool is
wool processing techniques, the annual production of wool in the collected by trimming wool from sheep once a year during summer
textile industry has reduced to 75% in European sheep farms or spring. Australia produced the highest amount of clean sheep
(Sabatini et al., 2019). Therefore, scientists and environmentalists wool, i.e., 23.4% of the total worldwide production of sheep wool in
are seeking alternatives for conventional water-based treatment 2018. Other major sheep-wool-producing countries are China
technologies in sheep wool processing. Over the years, numerous (15.5%), Russia (11.4%), New Zealand (9.1%), Argentina (2.3%), South
technologies have been implemented for processing sheep wool to Africa (2.2%), the UK (2.2%), and Uruguay (1.6%). Clean sheep wool
minimize the environmental and economic impacts (Pavlikova, can be categorized according to the average diameter of the wool
2020; Poole and Cord-Ruwisch, 2004). fiber into fine wool (24.5 mm), medium wool (24.6e32.5 mm), and
The handling and processing of raw sheep wool may pose po- coarse wool (>32.5 mm) fibers. The types of wool obtained from
tential hazards to personnel handling sheep wool. This is because various types of sheep and their characteristics are shown in
sheep wool fiber is highly susceptible to microbial contamination, Table 1. It was observed that the category of sheep wool depends on
starting from its time on the sheep body to the various stages of its the type of sheep. The sources of fine sheep wool are Delaine Me-
processing. The potential development of pathological diseases due rino sheep, Rambouillet sheep, and Deboillet sheep. Fine sheep
to microorganisms has been identified in sheep (Giannitti et al., wool has the shortest staple length and the highest spinning count.
2018). However, certain microorganisms may not be pathological Wool is considered a lavish natural fiber owing to its low weight,
to sheep, but they can rapidly multiply and stain wool fibers with dirt resistance, durability, and water repellency. Wool can absorb
mildew under favorable conditions. This results in loss of strength approximately 30% of its own weight in water, which can also be
and leads to deterioration. The activity of various microbes can released subsequently (Patnaik et al., 2015). Although the sheep
inhibit the utilization of wool. Hence, wool must often be sterilized wool is water repellent but able to absorb moisture. This is because
against pathogenic organisms and other microbes that can easily of the cuticle and cortical cell components of sheep wool fiber. The
damage it. Bacteriological studies are required to ensure the ster- cuticle cells of sheep wool coated with waxy materials, which
ilization of these fibers, to mitigate the effect of these microor- makes sheep wool water repellent. Wherein, the cortical cells of
ganisms. However, most of these organisms exist as spores and are sheep wool contain high sulfur proteins that absorbs the water
highly resistant to conventional water-based treatment methods. molecule. This property makes wool breathable and comfortable to
Supercritical carbon dioxide (scCO2) technology has been wear. It helps regulate body temperature by absorbing sweat and
2
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

Table 1
Sheep wool from various types of sheep and their characteristics (Source: Encyclopædia Britannica).

Type of wool Type of sheep Fiber diameter (mm) Staple length (mm) Spinning count (s) Mature Body weight (lb)

Ram Ewe

Fine sheep wool Delaine Merino 22e17 2.5e4 64e80 190e240 125e160
Rambouillet 24e19 2.5e4 60e80 200e300 140e180
Deboillet 22e18 3e5 64e80 220e275 125e160
Medium sheep wool Targhee 25e21 3e5 58e64 200e300 140e200
Finnsheep 31e24 3e6 48e60 160e200 120e160
Columbia 30e23 4e6 50e62 250e350 160e240
Dorset polled 33e26 3e4.5 46e58 225e275 150e200
Montadale 30e25 3e5 56e58 200e275 160e180
Corriedale 31e25 3.5e6 50e58 220e275 150e200
Cheviot 33e27 2.5e4 46e56 160e200 120e160
Shropshire 33e25 3e4 46e58 225e290 170e200
Southdown 30e25 2e3 50e58 180e230 120e180
Suffolk 33e26 2e3.5 46e58 275e400 200e300
Oxford 34e28 3e5 46e54 225e325 150e200
Coarse sheep wool Border leicester 38e30 5e10 36e48 225e300 150e225
Lincoln 41e34 8e15 36e46 240e300 200e250
Romney 39e32 5e8 36e48 200e275 150e200

releasing it as vapor, thereby preventing the clammy, cold feeling
experienced when some synthetic materials are worn during hot
weather. The ability of wool to retain moisture makes it resistant to
static electricity; hence, wool garments have a minimal chance of
sparking or clinging to the body (Kim and Kim, 2019). The chemical
structure of wool fiber is shown in Fig. 1.
Wool contains keratin, which is strengthened by disulfide bonds
from sulfur-containing amino acids. The non-protein fraction con-
sists of an outer lipid hydrophobic layer, which is known as lanolin
or wool wax (Fiore et al., 2019; Sabatini et al., 2018). The utilization
of wool on floors and car seats minimizes shock risks upon contact
with grounded objects because of its resistance to wear and tear
due to its mechanical and chemical properties (Bharath et al., 2016).
Wool is a biological polymer characterized by the cuticle, cell-
membrane complex, and cortex (Aluigi et al., 2008). Ninety
percent of the fiber by weight is composed of the cortex. Wool is
applied as a filler to produce mortar or plastic, which makes it a
renewable resource (Fiore et al., 2019). Wool fibers are hydrophilic
in nature. Fiber swells when it adsorbs moisture, resulting in an
increase in weight and size, which also affects its mechanical and
electrical properties (Memon et al., 2018).
Sheep wool has a diameter in the range of 16e40 mm; however,
unlike synthetic fibers, sheep wool has no specific thickness (Del-
Rey et al., 2017). Sheep wool contains 60% animal protein fibers,
15% moisture, 10% fat, 10% sheep sweat, and 5% impurities and is
known to be highly hygroscopic (Zach et al., 2012). Fabrics are bulky
compared with other textiles because they crimp and retain air,
which makes them good insulators. They help retain warmth in
cold weather. However, their insulation capability functions in both
ways. For instance, the Bedouins and Tuaregs use clothes made of
wool to keep the heat out, as it does not cling to their skin, allowing
proper air circulation. Fibers are more resistant to tension
compared with cotton and rayon; fibers can resist breakage even
when bent 20,000 times, whereas cotton and rayon can break
when bent just 3000 and 75 times, respectively (Yan 2016). Fibers
can be elongated by approximately 25%e30% and still return to a
natural shape. Fibers have a higher ignition point than cotton and
some synthetics. Even when burnt, they do not melt or drip like
synthetic materials. They have the self-extinguishing property
when the flame source is extinguished. They generate fewer toxic
gases when burned compared with synthetic materials, and they
are often recommended for high-safety environments such as
aircraft and trains. Their capability to protect from UV is much
higher than that of cotton and synthetic materials.
3
The presence of both crystalline and amorphous regions in wool
fibers makes them one of the most advanced complex and com-
posite structures in nature. Fig. 2 shows the physical structure of
sheep wool fiber. Sheep wool has a complex physical structure
consisting of a membrane, cortical cell, cortex, micro fibril, matrix,
twisted molecular chain, and helical coil (Erdogan et al., 2020).
Further, sheep wool is coated with the waxy material, lanolin.
Therefore, lanolin needs to be removed during the processing of
sheep wool. Notably, each wool component has a specific compo-
sition (physical and chemical), which plays a significant role in the
wool system. Changes in the physical structure due to activities
such as unscalling and peeling off may affect the morphology of the
wool fiber. Consequently, the cuticle cells might enhance the sur-
face area by weakening the structural bonds within the fiber
(Kuzmanova et al., 2018). The cortex is surrounded by cuticle scales,
which are rich in cysteine, a sulfur-containing amino acid whose
disulfide bond confers both chemical and mechanical stability to
wool. Even though the cuticle scales are known for their hydro-
phobicity, the propensity of the cortex to absorb 30% by weight in
moisture indicates hygroscopic characteristics. A combination of
these properties provides a unique wool surface (each component
possesses desirable properties such as high moisture absorbency
and chemical resistance). A wool fiber can be reverse engineered
into its major subcomponents by altering its chemical and physical
structures (Caven and Bechtold, 2017).
2.2. Utilization of sheep wool fiber
Sheep wool has received considerable attention for use as an
apparel fiber and interior fabric because of its good technical
properties. The utilization of sheep wool in various industrial ap-
plications is presented in Table 2. Sheep wool is mainly utilized as a
textile material for producing garments, warm clothes, carpets, and
curtains. However, the technical application of wool has attracted
scant attention compared with that of other synthetic fibers. Suc-
cessful technical utilization of wool fiber requires a high-value
application that can exploit its natural properties or modify it to
achieve a particular target performance. The sustainability and
biodegradability of wool fiber make it attractive for use as an ideal
material for various technical applications. Sheep wool, as a natural
fiber, has been utilized in civil engineering for the thermal and
acoustic insulation of facades and roofs or as reinforcement in
composites with polymeric, earthen, or cementations matrices
(Zagarella et al., 2014). Sheep wool has been employed as a soft mat
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al.
Fig. 1. Chemical structure of sheep wool (Rippon 1992).
for the thermal insulation of pitched roofs (Wulfhorst and Gries,
2012). There are two categories of sheep wool insulation products
in the building market. They are soft mats composed of 100% sheep
wool having a thickness of 4e6 cm, mainly used for the insulation
of pitched roofs, and semi-rigid panels composed of 70%e80%
sheep wool and 20%e30% polyester having a thickness of 5e12 cm
(Zach et al., 2012). They are applicable on walls because of the
stiffness achieved through the partial fusion of polyester fibers.
Wool fiber mainly contains a protein called keratin, which can
be used as a reinforcement. The insolubility and the resistance of
sheep wool are attributed to the disulfide bridges formed in the
sheep wool structure by cysteine. Keratin does not soluble in hot
and cold hot water and it does not break down into soluble ele-
ments, but it dissolves in dialkyl sulfoxides (Alston et al., 2019).
Besides, the sheep wool contains resilience and excellent elonga-
tion characteristics (Saxena et al., 2011). The tensile strength of
wool decreases with increasing temperature and time in a heat
n
treatment system utilizing argon or nitrogen (Li et al., 2019). Gala
and Marín et al., (2010) utilized the sheep wool fiber as a rein-
forcement in soil-alginate composite to enhance bonding within
soil particles. Zagarella et al. (2014) isolated a biocomposite
4
Journal of Cleaner Production 285 (2021) 124819
concrete using lime and sheep wool fibers (20e40 wt%) by
following granulometrics and a layered envelope system. It was
found that the thermal conductivity of the biocomposite concrete
was increased with the percentage sheep wool content. The study
reported that the sheep wool has the potential to be used in the
energy efficiency of a building.
Sheep wool shows a sufficiently good acoustical performance
for its use as a noise barrier, as a sound absorber in acoustic rooms,
or as a vibration insulator (Borlea et al., 2020; Korjenic et al., 2015).
The absorption coefficient of sheep wool panels were determined
to be 0.84 at 2000 Hz (Borlea et al., 2019). Borlea et al. (2020) re-
ported that the sheep wool panels could be utilized to improve
cavity absorber or vibration insulator maximum 10 dB and to
improve the transmission loss on plasterboard walls by maximum
6 dB. Wool fibers are a self-extinguishing material and it burns
slowly with a slight sputtering in the presence of a flame (Zach
et al., 2012). Besides, wool fibers are more hygroscopic and it can
absorb moisture in vapor form up to 20e35 wt% without causing a
damp feeling (Korjenic et al., 2015). The moisture absorption
capability of sheep wool fibers are higher than the glass wool fiber
(0.2%) or polystyrene foam (0.03%e0.1%) (Borlea et al., 2019).
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

Fig. 2. Physical structure of the sheep wool fiber.

Table 2
Utilization of sheep wool in various industrial application.

Applications Role References

Textile materials To produce warm clothes, carpet and curtains Laitala et al. (2018)
Civil engineering materials Thermal and acoustic insulations of facade and roof insulations Korjenic et al. (2015).
Reinforcement material Enhance mechanical and thermal properties of polymeric, earthen or cementitious matrices dinaru et al. (2016)
Gra
Acoustical material Adsobe sound, noise barrier and as a vibration insulator Borlea et al. (2020)
Del Rey et al. (2017)
Catalyst Enhance mass transfer, physical and chemical stability McNeil et al. (2017)
Geotextile Steep slopes protection of soil from erosion Broda et al. (2018)
Soil nutrient Cube nutrients for soil fertilization Abdallah et al. (2019)

2.3. Impurities and biological hazards of sheep wool fiber
Raw wool is often contaminated with impurities based on
certain factors such as the sheep breed, husbandry method, and
region in which the sheep are raised. Wool fiber contaminants can
be generally divided into the following four groups (IWTO, 2019;
Long et al., 2013; Millington and Rippon, 2017; Zhang et al., 2005):
i Water-soluble material, commonly called suint (soluble con-
taminants such as potassium salts from perspiration and feces);
ii Dirt from both organic and inorganic sources;
iii VM
iv Wool wax (oxidized and unoxidized forms)
Wool grease, suint, and dirt are the major contaminants in sheep
wool (Millington and Rippon, 2017). Wool grease is a wax produced
by the sebaceous glands in sheepskin, whereas suint is produced by
sweat glands. Both types of waxes are more precisely defined based
on their solubilities in water and organic solvents. Suint is mainly
composed of potassium salts of organic acids, with potassium ac-
counting for approximately 90% of the cations present or 25%e27%
of the dry weight of suint (Millington and Rippon, 2017). VM can
also be found in raw wool as a contaminant. In the case of heavy VM
contamination, carbonization may be required to remove it. Ex-
amples of VM include burrs, seeds, twigs, and straws. Copper
pollution was observed to affect the mineral metabolism of sheep
wool (Chi et al., 2019). Cadmium and Pb are known heavy metals in
sheep wool, as observed in the study of Tuncer (2019).
Sheep wool fiber is continually exposed to microbial contami-
nation starting from its time on the sheep body to the various
stages of its processing. Some of these microorganisms are
responsible for most of the pathological diseases in sheep.

5
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al.
However, certain microorganisms may not be pathological to
sheep, but under favorable conditions, they can rapidly multiply
and stain wool fibers with mildew, causing them to lose strength
and deteriorate easily. The activity of various microbes can hamper
the utilization of wool; hence, wool must often be sterilized to
eliminate pathogenic organisms and other microbes that can easily
cause damage to it. Moreover, organisms such as gram-positive
bacilli, gram-negative pleomorphic rods, coccobacilli, and cocci
can be found in the fleece of sheep, although their counts may vary.
The common resident floras in the fleece are Pseudomonas, Proteus,
Staphylococcus, and Bacillus. Mycotic dermatitis or “lumpy wool” is
caused by the bacterium Dermatophilus congolensis (Saleh et al.,
2019). It is often encountered in humid areas where humidity
keeps the wool from drying. The action of Mycobacterium avium ss.
Paratuberculosis can result in wool breakage. Wattiau et al. (2008)
detected Bacillus anthrax spores in a wool fiber processing factory.
B. anthrax is an infectious human pathogen. Thus, the presence of
microorganisms in sheep wool must be considered before selecting
a technology for sheep wool processing to ensure complete inac-
tivation of the pathogen to protect the wool fiber from damage and
prevent the exposure of the infectious pathogen.
3. Sheep wool fiber processing
During the production of fabric, sheep wool undergoes several
processing steps, such as shearing, classing, scouring, carding,
combining, and spinning into a yarn (Millington and Rippon, 2017).
Fig. 3 shows the process of sheep wool processing for producing
clean fabrics. Sheep are generally sheared once a year. After
shearing, the fleece is separated manually from shorter wool,
leaves, twigs, and undesirable parts of the fleece. The folded and
rolled fleece is classified according to the diameter, length,
strength, and color of the individual fibers. Subsequently, sheep
wool undergoes scouring to remove lanolin and other VM present
in the wool. The clean sheep wool from different batches is blended
in size and color. The blended and scoured wool contains tufts of
tangled fibers. Consequently, the fiber undergoes carding to pro-
duce smooth fibers. Generally, carding is performed by brushing
with a carding machine over a series of rolling drums with varying
drum sizes and rotation speeds. After carding, the wool is twisted
into ropes by spinning. Generally, shorter fibers are used to make
woolen yarns and longer fibers are used to make worsted yarns.
Fig. 3. Existing sheep processing method for produce clean sheep wool.
6
Journal of Cleaner Production 285 (2021) 124819
Subsequently, the yarned wool undergoes aqueous dying to pro-
duce colorful textile products.
Scouring is the most important step in sheep wool processing.
Generally, raw sheep wool is greasy because it contains lanolin,
sweat salts, dirt, dung, dust, and other VM. It is essential to remove
the extraneous materials to utilize sheep wool as a textile fiber;
consequently, wool scouring is essential (Li et al., 2017; Long et al.,
2013). Although the term “wool scouring” refers to the process of
wool washing and drying, in reality, there are several other steps
involved in this process, such as opening, blending, mechanical
cleaning, baling, sampling, and testing. In addition, several types of
chemical treatments may be used in conjunction with the scouring
process (Li et al., 2017). Table 3 shows the various scouring methods
used in sheep wool processing and their limitations.
The scouring process cleans wool by eliminating lanolin in a hot
water bath using alkali or soap. However, some advanced scouring
processes have been reported in the literature as follows:
i. Pulsed electrohydraulic discharge wool scouring;
ii. Ultrasonic-assisted industrial wool scouring;
iii. Solvent wool scouring;
iv. Detergent wool scouring with alkaline builders.
3.1. Pulsed electrohydraulic discharge (PED) for wool fiber cleaning
Pulsed electrohydraulic discharge (PED) is an environmentally-
safe wool cleaning technology based on the electrohydraulic effect.
It involves several complex phenomena in the discharge of high
voltage through a liquid. PED technologies have been shown to
involve several mechanisms, such as ultraviolet radiation, shock-
waves, and radical reactions (Anpilov et al., 2001; Li et al., 2012).
Raw wool samples are scoured in the experimental PED system
and treated in water without adjusting the pH. In a study conducted
by Zhang et al. (2016), the output voltage was set to 14.8 kV, where
each sample was treated 3, 9, and 18 times. Detergent/chemicals
and water heating were not employed during the scouring process.
After the scouring process, it was observed that the wool became
white in color owing to the elimination of certain impurities and
contaminants. The conductivity of the liquid can be increased by
increasing the number of treatments. However, there are certain
drawbacks of the PED process (Zhang et al., 2016), including slight
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

Table 3
Various scouring methods for sheep wool processing.

Method of treatment Limitations References

Pulsed electrohydraulic discharge Damage to the scales and fiber strength. Zhang et al. (2016)
Generate wastewater with high chemical oxygen demand and turbidity
Ultrasonic-assisted industrial wool scouring High energy consumption Li et al., (2017)
Enzymatic treatment with subtilizing and subtilizing Hydrolytic attack to the fibre surface Mojsov (2017)
Enzyme diffuses causes fiber strength loss.
Alkaline wool scouring High cost due to the depreciation Bhavsar et al., (2017)
Excessive damage to keratin structure.
Soap scouring Fiber loss of flexibility Gutarowska et al. (2017)
Carbonizing Decreased tensile strength of carbonized fibre Czaplicki and Strzelecki, (2019)
Extensive fibre damage
Oxidation with H2O2 Damage fiber and weekend the fiber strength Long et al. (2013)

Superheated water hydrolytic damage to the cuticle and cortical cell Zhang, et al.(2016)
loss of fiber surface integrity
High pressure water Decreased the tenacity and elongation at break of wool fibres Zheng et al., 2016

damage to the scales, generation of wastewater with turbidity and
COD values, longer treatment times, and a decrease in fiber
strength caused by the removal of scale.
3.2. Ultrasonic-assisted industrial wool scouring
Ultrasonic irradiation can be used to improve the process of raw
wool scouring in an effective and environment-friendly manner (Li
et al., 2012; Pan et al., 2018). This can be achieved in several ways,
such as lowering the cleaning temperature in the baths to reduce
the required energy for scouring, and significantly reducing the
amount of chemicals/detergent required for cleaning such that the
toxicity of the effluents can be reduced. Li et al. (2012) reported the
utilization of wool with the following specifications: 175 kg net
weight, 18e20 mm mean diameter, 0.3% VM, 18% coefficient of
variation, and 64.5% scouring yield with ultrasound frequency. The
process was performed using an ultrasonic frequency of 80 kHz,
and each panel had a maximum power of 3300 W adjustable from
0 to 100%. The volume of the bath was 600 L, and the maximum
power density of 12e13 W/L was maintained in the bath
throughout the process. Ultrasonic radiation was only introduced
into one scouring bath (bowl 2) because industrial trials have
shown that the use of one ultrasonic bath can significantly improve
the removal of dirt and grease. Ultrasound scouring has the
advantage of low cost and low energy consumption. It also has the
potential to utilize maximum power. However, residual ash content
and insufficient reduction in the toxicity of the effluents produced
by the cleaning process are known limitations of ultrasonic scour-
ing (Pan et al., 2018).
3.3. Solvent wool scouring
This method has been applied to remove oily dirt from fabrics
and to induce stress relaxation to individual fibers (Barba Albanell
pez-Mesas et al., 2005). The solvent used in solvent
et al., 2018; Lo
scouring is trichloroethane added with some special inhibitors;
these inhibitors are suitable for repeated use in solvent scouring
and they do not have adverse effects on the scoured fabrics (Hong
2018). The grey fabric is passed through three solvent baths for the
removal of oil-soluble soil. After the solvent is removed by vacuum
squeeze, the fabric enters a hot water bath. At this stage, the solvent
remaining on the fabric is instantaneously vaporized and removed
as bubbles. Water-soluble soil is also removed. After hot water is
squeezed out by the mangle, the fabric is sent to a cold water bath,
which prevents the setting of creases, and then, the fabric is folded
by a swaying fall. The fabric is scoured in three baths. The fabric
passes from the first bath to the third bath while the solvent flows
7
in the opposite direction from the third bath to the first bath to
form a multi-stage countercurrent extraction system. The total
volume of solvent held in solvent scouring is 2.5 m3. For example, if
the machine is driven 6 h/day, the solvent consumed is 66 kg/day
(Hassan and Shao, 2016). The advantages of using scouring ma-
chines include producing quality fabrics excellent in color, texture,
and uniformity of scouring, although the fixed cost is generally high
because of the cost attributed to depreciation.
3.4. Detergent wool scouring with an alkaline builder
Soap is the main detergent used for wool scouring; it is used in
combination with an alkaline builder, which is usually soda ash
(Brani
sa et al., 2019; Senthil Kumar and Grace Pavithra, 2019).
Synthetic detergents were developed because of their ability to
react with calcium and magnesium ions in hard water to form
insoluble salts. The most common ones used today in the scouring
industry are the non-ionic types (Brani
sa et al., 2019). So far, syn-
thetic detergents, which are nonyl or octylphenol ethoxylates, have
been commonly used; however, their non-biodegradability and the
associated environmental concerns have hampered their applica-
tion in scouring processes. Consequently, the more biodegradable
fatty alcohol ethoxylates have increasingly been used, with soda
ash being the most commonly employed builder. Wool scouring is
often aimed at stabilizing the emulsified wool grease and dirt and
preventing their re-deposition on the wool (Brani
sa et al., 2019).
Moreover, the typical bowl temperatures used during scouring
with a neutral non-ionic detergent depend on the detergent used.
The temperature is often within 50e65  C. However, lower tem-
peratures are used when using alkaline scouring conditions (usu-
ally less than 55  C).
The quantity of detergent used depends on the wool type being
scoured; however, it is often <9 L/ton greasy weight and <3 L/ton
greasy weight for wool and crossbred wools, respectively. More
detergent must be added to the second and third hot scouring
bowls to achieve the greatest effect of the countercurrent flowback
system; however, this approach must be altered when scouring
wools, especially when the detergent foams excessively in the later
scouring bowls (Senthil Kumar and Grace Pavithra, 2019). The type
of wool determines the rate of its scouring process. For instance, the
scouring throughput of relatively clean crossbred wool can be
approximately twice that of a low-yielding type. However, due to
the presence of multivalent metal ions, hardness can occur. In areas
affected by hard water, it may be necessary to install a softening
plant to overcome this challenge. Furthermore, the presence of
metal ions can cause severe dying problems through interaction
with the dye.
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

3.5. Limitations of the existing sheep wool processing process

The main contaminants of sheep wool are grease (wax), suint

(sweating salts), and dirt. Wax is a complex mixture of organic
compounds, including ester, which is a stable solid or semi-solid
formed around the wool fiber with a melting point of approxi-
mately 43  C (Zakaria El-Sayed et al., 2018). Generally, wax is an
organic compound insoluble in water; therefore, its removal during
scouring requires additional chemicals or detergents. Suint is dried
sweat, which mainly consists of potassium salts of organic com-
pounds (Cholewinska et al., 2020). The VM present in sheep wool is
not soluble in water and is difficult to remove using an existing
scouring process. It is effectively removed by carbonization.
Table 4 shows the advantages and limitation of various sheep
wool processing technologies. The main objective of wool scouring Fig. 4. Phase diagram of the fluid CO2 in solid, liquid, gas and supercritical state.
is to produce clean wool by eliminating impurities with minimal
environmental impact (Sabatini et al., 2018). Although numerous
approaches have been adopted to improve the sheep wool scouring microorganisms, which are difficult to treat with biological
process, fiber entanglement and the generation of wastewater wastewater treatment and disposal processes. In recent years, the
remain the biggest challenges. As a protein fiber, sheep wool is wool processing industry has focused more on minimizing waste-
weaker than a stable fiber. During scouring, sheep wool experi- water generation than on mitigating wool entanglement due to
ences various adverse experimental conditions, including me- strict environmental legislations. Thus, it is necessary to find an
chanical pressing, temperature, pH, and the addition of chemicals, alternative for existing water-based treatment processes.
which lead to the loss of fiber strength and fiber damage. The
tensile strength of wool decreases when wool is wet during 4. Supercritical carbon dioxide technology
scouring because the hydrogen bonds of the keratin chain in wool
are disassociated in the presence of water. However, wool fibers The scCO2 technology has been viewed as an effective method
may gain reversible strength loss when disulfate bonds are reduced for the extraction and separation of lipids, sterilization of heat-
in wool during the wet scouring process (Long et al., 2013; Lo pez- sensitive materials, and cleaning and drying of textiles and fabric
Mesas et al., 2005). In the chemical scouring process, wool fiber materials. Due to the rising environmental concerns associated
can be damaged, as the protein chain of wool fiber can be ionized, with the discharge of toxic pollutants to the environment and
producing smaller charged molecules. Sheep wool fiber can greenhouse gas emissions, the scCO2 technology has been
degrade thermally when exposed to a relatively mild temperature. increasingly implemented. Supercritical carbon dioxide refers to
The generation of wastewater from wool scouring has caused the physical condition of fluid carbon dioxide in the supercritical
environmental concerns because of the extremely high pollution state. This phenomenon can be further described with a phase di-
load associated with the existing steam-based scouring process of agram of scCO2 fluids, as presented in Fig. 4. The critical tempera-
greasy wool. The effluent generated during the wool scouring ture and pressure of CO2 are 31.1  C and 7.38 MPa, respectively.
process contains greasy materials, pesticides, parasites, and Beyond this point, CO2 is neither a gas nor a liquid, and it can be

Table 4
Advantages and disadvantages of scCO2 technology and existing water-based sheep wool processing technology.

Technology Advantages Disadvantages References

Conventional Water Effective in removing wool fat and dirt from sheep Requires the use of solvent with water. Bhavsar et al.,(2017); Gutarowska
based technology wool. Generates toxic effluent that must be treated prior to et al. (2017); Zhang et al. (2016)
Produce good quality of scoured wool discharge.
Less tangled wool with a high degree of white. Minimize wool fiber strength.
Require further processing technology for separating
lanolin from wool and drying the wool.
Microwave radiation Shorter treatment time. Expensive equipment. Aydin (2008); Xu et al., 2006
No chemicals required. Not suitable for scaling up.
Easy handling. Difficult to reaction monitoring.
Excellent reproducibility. Decomposition of lipid matter on the surface of the
plasma-treated fibers.
Require further processing technology for separating
lanolin from wool and drying the wool.
Plasma Shorter treatment process Requires chemicals. Czaplicki and Ruszkowski (2014); Haji
low chemical consumption High capital investment for plasma equipment and and Naebe (2020).
No wool damage. vacuum pump.
Good reproducibility. Wastewater generation.
Reducing water consumption and energy to dry Require further processing technology for separating
the treated wool. lanolin from wool and drying the wool.
scCO2 Waterless technology. High capital investment for the equipment setting Jones et al. (1997); Long et al. (2013);
It does not require any toxic chemical. up.  pez-Mesas et al., 2005
Lo
No wool damage. Requires co-solvent for extracting polar organic
No generation of toxic effluent. compounds.
Sheep wool cleaning, extraction of lanolin and
drying can be carried out simultaneously.
Green technology.

8
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al.
best described as an intermediate between these two extremes
(Hossain et al., 2013; Scognamiglio et al., 2017). The advantage of
the scCO2 technology is that CO2, which is used as a solvent, is a gas
at ambient temperature; therefore, it does not require an additional
separation technology to separate the end product. In addition, CO2
is non-toxic, non-flammable, easy to handle, environment-friendly,
abundant, recyclable, and inexpensive (Hossain et al, 2011, 2015).
Moreover, the wide range of solubilities of organic compounds in
scCO2 makes this technology preferable for advanced applications
in various industrial fields.
4.1. Supercritical carbon dioxide as an extraction technology
The scCO2 technology has been extensively utilized for the
extraction and separation of lipids (Alhattab et al., 2019) and an-
tioxidants (Goyeneche et al., 2018), decaffeination of coffee or tea
(Bermejo et al., 2016), and separation of lecithin from oil (Teberikler
et al., 2001). It has also been applied for the extraction and sepa-
ration of waxes from plants, as shown in Table 5. Distinct properties
such as the low viscosity, high diffusivity, and low surface tension of
scCO2 make it an ideal solvent for the extraction of wax materials
(Hossain et al., 2015). Another advantage of using scCO2 as a solvent
for extraction is that the solubility, viscosity, diffusivity, and surface
tension of scCO2 are tunable. These properties of scCO2 can be
tuned to enhance the strength of the fluids in the interaction of the
matrices by varying the pressure and temperature during extrac-
tion (Hossain et al., 2016a). In addition, this technology produces a
solvent-free extract, which makes it an ideal extraction technology
in the food, pharmaceutical, and cosmetics industries.
Al Bulushi et al. (2018) extracted waxes from date palm leaves
using scCO2. The study reported that the scCO2 technology is a
clean and efficient method for the extraction of wax materials from
date palm leaves. In addition, the extraction time and treatment
cost of scCO2 were considerably lower than those of conventional
Soxhlet extraction methods for wax extraction from date palm
leaves. With a shorter extraction time, Attard et al. (2018) utilized
scCO2 for the extraction of waxes and the fractionation of canna-
bidiol from hemp wastes. The study reported that the scCO2 tech-
nology is suitable for the fractionation of cannabidiol from hemp
waste due to the relatively low extraction temperature of scCO2.
The scCO2 technology has been implemented as a downstream
processing of miscanthus for the extraction of lipophilic com-
pounds, including waxes. It was observed that the release of sugar
increased by approximately 20% with the addition of scCO2 in the
downstream processing of miscanthus. Athukorala and Mazza
(2010) observed that the scCO2 technology is suitable for the
extraction of triticale wax, as compared with Soxhlet extraction
with hexane. Sin et al. (2014) extracted various wax esters from
wheat straw using scCO2 at the pressures of 7.5e40 MPa and
Table 5
Supercritical CO2 extraction of waxes from various plant matrices.
a
Matrix Parameters
Pressure MPa Temperature (oC)
Food waste 35 50
Date palm leaves 40 100
Hemp 35 50
wool 66 150
Triticale straw 40 70
Wheat straw 40 100
Rice bran 28 70
Peppermint leaves 30 70
Old corrugated containers 30 100
Apple peel 35 50
a
Optimal experimental conditions of scCO2.
9
Journal of Cleaner Production 285 (2021) 124819
temperatures of 32e100  C.
4.2. Supercritical carbon dioxide as a sterilization technology
Sterilization refers to the process of eliminating, killing, and
inactivating all types of microorganisms present in materials, such
as viruses, bacteria, fungi, and other unicellular eukaryotes
(Hossain et al., 2013). It provides materials free from live microor-
ganisms; therefore, the materials do not pose any threat of infec-
tion. The scCO2 technology is viewed as a terminal sterilization
method that can be operated at low temperature and moderate
pressure. scCO2 refers to a supercritical state of carbon dioxide gas
when it is exposed to a higher temperature and pressure relative to
its critical point (Hossain et al., 2016b). CO2 behaves as a normal gas
under standard temperature and pressure conditions, but beyond a
temperature and pressure of 31.1  C and 7.4 MPa, respectively, it
assumes a supercritical phase with associated changes in proper-
ties, appearing neither as a gas nor as a liquid (Hossain et al., 2011;
Mohd Omar et al., 2018). Pressurized gas sterilization was first
investigated by Fraser in 1951 (Fraser, 1951), before further exam-
ination of the treatment of microorganisms with fast depressur-
ization of high-pressure gases using nitrogen gas. Several Japanese
scholars explored high-pressure gas treatment in the 1980 as an
alternative method for sterilizing biological products and heat-
sensitive compounds, and food preservation. In 1987, Kamihira
et al. (1987) utilized scCO2 for the inactivation of a group of mi-
croorganisms including Bacillus subtilis, Staphylococcus aureus,
Aspergillus niger, Baker’s yeast, and Escherichia coli. Subsequently,
scCO2 has been widely applied for the sterilization of food (Mohd
Omar et al., 2018), pharmaceutical products (Long et al., 2019),
medical devices (Ribeiro et al., 2020), healthcare waste (Hossain
et al., 2013), and biodegradable plastics (Scognamiglio et al., 2017).
The potential advantage of scCO2 sterilization is that it sterilizes
heat-sensitive materials without causing damage. Table 6 shows
the application of the scCO2 technology for the sterilization of
various heat-sensitive materials. Various parameters such as pres-
sure, temperature, sterilization time, CO2 flow rate, and the addi-
tion of chemical additives or modifiers influence the efficiency of
scCO2 sterilization (Ribeiro et al., 2020). Among these parameters,
pressure and temperature have the highest influence on the inac-
tivation of microorganisms (Hossain et al., 2015). Scognamiglio
et al. (2017) utilized scCO2 for the sterilization of a poly-
saccharidic membrane for surgical utilization at 27 MPa and 40  C
for 60 min with the addition of a small amount of H2O2
(200e1000 ppm) as an additive. The mechanical test analyses of
the sterilized membrane showed that scCO2 sterilization was highly
effective. Moreover, biological characterization revealed that the
sterilized membrane was biocompatible in vitro. Thus, the study
pointed out that the scCO2 technology is a safe and effective
References
Time (min)
60 Yu et al. (2019)
120 Al Bulushi et al., 2018
240 Attard et al. (2018)
60 Jones et al. (1997)
90 Athukorala, and Mazza (2010)
e Sin et al. (2014)
García et al. (1996)
Roy et al. (1996)
60 Stauffer et al. (2002)
90 Li et al. (2015)
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

Table 6
Sterilization of various materials for the inactivation of microorganism using scCO2.
a
Materials Parameters Target microbes References

Pressure Time Temperature

(MPa) (min) (oC)

Polysaccharide membranes 27 180 40 NA Scognamiglio et al.,

2017
Cellulose membranes 30 30 40 Bacterial lipopolysaccharides Pigaleva, et al., 2019
Endotoxins
Biofilm 30 120 60 Bacillus cereus spores Park et al. 2013
Baker’s yeast 20 120 35 Escherichia coli Kamihira 1987
Staphylococcus aureus
Aspergillus niger
Solid food matrices 12 60 40 Salmonella enterica Galvanin et al., 2014
Escherichia coli
Listeria monocytogenes
Ancient paper 15 60 40 Aspergillus niger Teixeira et al., 2018
Aspergillus flavus
Eurotium amstelodami
Wheat grains 10 11 44 Penicillium oxalicum spores Park et al., 2012
Foods 11.4 120 40 Escherichia coli Melo Silva et al.
(2013)
Biomaterials 10 180 60 Bacillus atrophaeus White et al. 2006
Bacillus stearothermophilus spore
Apple cider 7.6 20 42 Escherichia coli K12 Yuk et al., 2010
Physiological saline phosphate-buffered 25 30 55 Salmonella enterica Kim et al (2007)
saline
Apple juice 35 5 36 Escherichia coli ~ o et al 2014
Ortun
Saccharomyces cerevisiae
Apple juice 10 40 70 Alicyclobacillus acidoterrestris spores Bae et al. 2009
Metal surfaces 30 120 60 Bacillus subtilis Da Silva et al., (2016)
Geobacillus stearothermophilus
Vegetative foodborne pathogens 10 120 75 Pseudomonas aeruginosa Aeromonas hydrophila Salmonella Furukawa et al 2009
enteritidis
Salmonella typhimurium,
Yersinia enterocolitica,
E. coli O157:H7
Staphylococcus aureus
Listeria monocytogenes
Food industry 20 120 33 Listeria monocytogenes Soares et al. 2013
Pears 10 45 55 Saccharomyces cerevisiae Valverde et al. 2010
Cocoa seed 30 20 80 Aspergillus niger Calvo et al. 2007
Aspergillus ochraceus
Paprika 10 45 95 Enterobacteriaceae Calvo and Torres
E. coli and S. aureus (2010)
Apple juice 15 30 55 Lactobacillus casei cells Silva et al. (2018)
Corticosteroid powders 20 30 55 Staphylococcus epidermidis Bacillus pumilus Zani et al 2013
Bacillus subtilis
a
Optimal experimental conditions of scCO2.

method for the sterilization of polysaccharide-based medical de-
vices. Aslanidou et al. (2016) successfully disinfected an Aspergillus-
niger-contaminated textile using the scCO2 sterilization technology
at 15 MPa and 40  C with 5 wt% of Ca(OH)2. Hossain et al. (2016b)
sterilized clinical solid waste materials using scCO2 and an auto-
clave. It was observed that scCO2 completely inactivated the
pathogenic bacteria present in the solid waste. The regrowth ana-
lyses of bacteria showed the regrowth of bacteria from autoclaved
clinical solid waste after 48 h of sterilization. However, no regrowth
was observed from the scCO2-sterilized clinical waste. This is
because scCO2 inactivates the bacteria physicochemically. Physi-
cally, the scCO2 pressure breaks and punctures the cell wall.
Chemically, scCO2 extracts the cytoplasmic materials of the
bacteria.
4.3. Supercritical carbon dioxide as a cleaning and drying
technology
Cleaning technology significantly influences product quality in
the manufacturing industry. Generally, the cleaning process is uti-
lized in the manufacturing industry to remove impurities and dirt
from the surface of processing materials. Existing cleaning pro-
cesses can be classified into dry or wet processes, and they require
the use of volatile organic compounds (VOCs) or detergents at high
temperatures. However, these cleaning processes are challenging
from an environmental perspective, as they generate hazardous
residues and polluted wastewater (Aslanidou et al., 2016;
Michelino et al., 2018). The scCO2 technology has been utilized as a
precision cleaning and drying method for many industrial products
to remove dirt, including carbon nanotubes, polymers, metals, and
glass surfaces as well as silicon wafers (Aslanidou et al., 2016; Liu
et al, 2015, 2016). The tunable properties of CO2 in the supercriti-
cal state, such as its liquid-like density and gas-like viscosity, make
scCO2 an established cleaning technology in various industrial
fields. Owing to the very low surface tension of scCO2, which en-
sures the high wettability of materials, this technology is an
effective precision cleaning technology. Table 7 shows the appli-
cation of scCO2 as a cleaning and drying technology for various
industrial materials.
In scCO2 cleaning, CO2 is used as a solvent, instead of volatile
organic solvents or detergents. This minimizes the generation of
VOC-contaminated wastewater, hazardous air pollutants, and

10
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al. Journal of Cleaner Production 285 (2021) 124819

Table 7
Cleaning and drying various manufacturing materials using scCO2.
a
Materials Purpose Parameters References

Pressure (MPa) Temperature (oC) Time (min)

Textile Removal of soil 34 40 120 Aslanidou et al. (2013)

Remanufacturing materials Removal of carbonaceous deposits, oil and grease 30 90 40 Liu et al. (2014)
Archeological artifacts Removal of organic material 20.4 40 30 Rowe et al. (2013)
Contaminated sand Removal of Cesium 29 80 6 Leybros et al. (2016)
Flax rove Removal of gum 20 50 90 Zhang et al. (2019)
Oxidized copper Removal of the post-etch residues 14 55 7 Ventosa et al., 2008
Textiles Removal of sand, carbon black and clay 4.5 10 30 Van Roosmalen et al., 2003
Grey cotton Removal of impurities 13 50 60 Liu et al. (2016)
Remanufacturing metals Cleaning metals surface 25 75 40 Liu et al. (2015a)
Air filters Removal of dioctylphthalate 20 40 120 Ito et al. (2004)
Glass Removal of polymeric photoresist films from glass surfaces 12.4 50 4 Wang et al. (2008)
Microfiltration membrane Removal of soybean oil 30 40 139 Krzysztoforski et al. (2018)
Drilling mud Removal of contaminants 18 60 110 Khanpour et al. (2014)
Soil Removal of pesticides 21.5 40 120 Castelo-Grande et al., 2005
Printing inks Cleaning engraved rollers 15 40 60 Della Porta et al., 2006
Diesel engine valve Cleaning carbonaceous deposits 25 65 30 Liu et al. (2015b)
Textile Removal of soils 15 40 60 Aslanidou et al. (2016)
a
Optimal experimental conditions of scCO2.

substances causing ozone depletion. However, the cleaning effi-
ciency of scCO2 depends on the diffusion coefficient, density, sol-
ubility, and polarity of the contaminates present in sheep wool (Hu
and Deng, 2016). As CO2 is a non-polar molecule, its dipole moment
is zero. Therefore, scCO2 has a strong dissolving capacity for organic
compounds such as grease, oil, and ester (Attard et al., 2016). The
scCO2 technology has also been utilized as a drying technology for
food (Brown et al., 2008), pharmaceutical products (Bensebia et al.,
2016), and aerogels (Wang et al., 2016). The potential advantage of
scCO2 drying is that the dried products appear natural, as this
process does not alter the shape and color of the product. In
addition, the process is considered a mild drying process. It can be
performed at a low temperature and moderate pressure in an
oxygen-free environment; therefore, it does not degrade the ma-
terial quality and avoids destruction due to thermal stress (Wang
et al., 2016). During the scCO2 drying process, water is gently
removed from the materials and the texture and structure of the
materials are maintained during rehydration. The fluid CO2 in the
supercritical state rehydrates the water without interacting with
the internal surface of the materials, thereby preventing shrinkage
or collapse. Brown et al. (2008) utilized scCO2 to remove moisture
from a carrot at a pressure of 20 MPa by varying the temperature
and adding ethanol as a solvent. The study reported that carrot
dried under scCO2 had favorable rehydrated properties. Michelino
et al. (2018) observed that the application of the scCO2 drying
technology did not affect the color and appearance of treated
coriander leaves. Zambon et al. (2018) applied the scCO2 technology
as a drying agent for the decontamination and drying of herbs at
the pressure of 10 MPa and temperatures of 40  C and 50  C for a
drying time of 150 min. The study reported that the scCO2 tech-
nology is a promising green method for both the decontamination
and drying of herbs in a single step with relevant effects on cost and
safety.
4.4. Potential and challenges of scCO2 technology in sheep wool
processing
Sheep wool is widely used as a warm clothing material in the
textile industry and as a technical material in various industrial
fields owing to its high quality and excellent properties. However,
the fabrication of sheep wool involves effective water-based
washing, scouring, bleaching, drying, and functional finishing
processes to remove dirt, suint, wax, and other impurities (Kan
et al., 1998; Xu et al., 2006). This conventional treatment process
requires numerous chemicals and a large amount of water, result-
ing in the generation of toxic effluents. Therefore, the conventional
water-based sheep wool treatment process poses serious envi-
ronmental and economic concerns. Consequently, numerous
alternative technologies, such as corona charge (Xu et al., 2006),
microwave (Xue, 2016) Xue, and plasma (Kan et al., 1998) have been
applied in wool fiber processing. However, these technologies have
only improved the surface morphology of wool fiber, and they
require additional treatment processes for the cleaning and drying
of sheep wool fiber.
The scCO2 technology has been introduced in the textile in-
dustry for the extraction and separation of wool wax from raw wool
and wool wax waste, as shown in Table 5. Jones et al. (1997)
examined the solubility of wool during the extraction of lanolin
from raw sheep wool using scCO2. The study reported that
approximately 98% of wool wax acids and wool wax esters were
dissolved in scCO2 at 65 MPa and 150  C. The treated sheep wool
fiber was odorless and pale in color, which revealed that scCO2
effectively removed the wax materials from the sheep wool. Lo  pez-
Mesas et al. (2005) applied the scCO2 technology for the extraction
of wool wax from wool scouring waste. The purpose of this study
was to determine the possibility of using the scCO2 technology as
an alternative to the conventional Soxhlet extraction technology.
The study reported that the scCO2 technology completely extracted
lipids and other impurities present in the wool wax waste with a
shorter extraction time (45 min) than the solvent extraction
method (4 h). Long et al. (2013) determined the effects of scCO2 on
the chemical and crystal structures of wool fiber. It was observed
that scCO2 influences the re-crystallization of the polymer chain in
wool fiber and the rearrangement of the chemical structure due to
the strong affinity of hydrogen bonds within the macromolecular
chain of wool fiber. In addition, analyses of the thermal properties
of scCO2-treated wool fiber revealed that the treatment enhanced
the thermal properties of wool fiber.
Thus, the scCO2 technology has the potential to be utilized in the
sheep wool processing and textile industries as an alternative to
conventional water-based sheep wool processing. The adoption of
the scCO2 technology in sheep wool fiber processing can have
numerous advantages, including cleaner production of wool tex-
tiles with a waterless treatment process to avoid the generation of
toxic effluents. Existing sheep wool processing methods require
multiple processing steps, including wool scouring for removing

11
F.A. Salem Allafi, M.S. Hossain, M.O. Ab Kadir et al.
Fig. 5. Implementation of the scCO2 technology in sheep wool processing.
lanolin, wool cleaning to remove suint and dirt, and wool drying to
remove moisture. Sheep wool processing steps such as the sterili-
zation of sheep wool, extraction of lanolin/wax, and cleaning and
drying of sheep wool can be conducted simultaneously with the
application of the scCO2 technology, as shown in Fig. 5. The
implementation of the scCO2 technology in sheep wool processing
has the following advantages:
 No generation of toxic effluents
 Extraction of lanolin as a byproduct for cosmetic applications
 Enhanced dyeability
 Avoiding multiple processing steps
 Obtaining high-quality sheep wool with lower processing cost
 Time and energy saving
 Avoiding the use of toxic VOCs
 It is a green technology.
However, there are some limitations to the utilization of scCO2
in sheep wool processing. The major limitation of the use of scCO2
in sheep wool processing is the cost associated with high-pressure
technology (Luo et al., 2018). Besides, this processing technology
operates at high pressure (10e40 MPa) and moderate temperature
(35  Ce80  C), which results in high investment cost that stand the
way industrial implementation (Luo et al., 2018; Zhang et al., 2019).
In addition, the solubility of polar compounds and high-molecular-
weight compounds in scCO2 is poor (Long et al., 2013). Although,
the fluid CO2 is an excellent solvent for non-polar compounds, but
the low dielectric constant of CO2 makes difficult to extract ionic
and polar compounds. As sheep wool contains potassium organic
salts, it requires the addition of polar organic solvents such as
ethanol, hydrogen peroxide, and ether as a co-solvent, or chemical
additives to enhance the solubility. The solubility of the scCO2 can
be easily altered by tuning the pressure and temperature in the
presence of small amount chemical modifier (Schmidt et al., 2003).
Another limitation of the application of the scCO2 in sheep wool
processing is the frequently clean up the vent and separation vessel.
Since sheep wool contains dirt and waxy materials, it may clog to
the vent if it is not clean up regularly.
5. Conclusions
The present review was conducted to determine the potential
and challenges of the use of scCO2 technology in sheep wool pro-
cessing. Increasing environmental awareness, legislation, and
worldwide concerns related to the generation of toxic effluents
from the sheep wool manufacturing industry, there is an urgent
12
Journal of Cleaner Production 285 (2021) 124819
need for a waterless technology for cleaner sheep wool production.
Currently, steam-based technology in sheep wool processing re-
quires a series of water-based treatment processes and chemicals,
which consequently generates significant amounts of toxic efflu-
ents. The scCO2, as a waterless technology, has been extensively
utilized in the sterilization, extraction cleaning, and drying tech-
nology for processing various solid matrices. Thus, scCO2 technol-
ogy has considerable potential for use in sheep wool processing.
The scCO2 technology can be simultaneously utilized in sheep wool
processing to sterilize microorganisms, extract lanolin, and clean
and dry the sheep wool. It produces clean and pesticide-free sheep
wool fibers without generating toxic effluents. However, the chal-
lenges of using scCO2 technology are the equipment price and polar
organic compounds in sheep wool. Thus, further laboratory studies
are required to optimize the experimental conditions of scCO2 and
determine suitable co-solvents to enhance the solubility of fluid
CO2.
Declaration of competing interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
Acknowledgement
Authors would like to acknowledge to Ministry of Education
MoE, Malaysia for providing Fundamental Research Grant Scheme
FRGS, Grant N)-203/PTEKIND/6711817, as a financial support.
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