Journal of Cleaner Production 365 (2022) 132795

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Journal of Cleaner Production

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

Zero-waste strategy by means of valorization of bread waste

Jong-Min Jung a, 1, Jee Young Kim b, 1, Jung-Hun Kim a, Shin Myung Kim b, Sungyup Jung a,
Hocheol Song c, Eilhann E. Kwon a, *, Yoon-E Choi b, **
a
Department of Earth Resources and Environmental Engineering, Hanyang University, Seoul, 04763, Republic of Korea
b
Division of Environmental Science and Ecological Engineering, Korea University, Seoul, 02841, Republic of Korea
c
Department of Environment and Energy, Sejong University, Seoul, 05006, Republic of Korea

A R T I C L E I N F O A B S T R A C T

Handling editor: Prof. Jiri Jaromir Klemeš To impose the zero-waste strategy through the diverse valorization route, this study used bread waste (BW) as the
model compound. To realize these grand technical challenges, BW was enzymatically hydrolyzed to obtain a
Keywords: monomer sugar compound (glucose), and glucose was used as the carbon substrate in heterotrophic cultivation
Circular economy of Euglena gracilis (E. gracilis). Cultivation of E. gracilis using cultivation medium derived from BW was evaluated
Zero-waste
from a perspective of an economic viability. In addition, the more production of the target compound (para­
Biorefinery
mylon, β-1,3-glucan) stemmed from E. gracilis was achieved (1.93 g L− 1d− 1; 24% higher productivity than that of
Carbon dioxide
Euglena gracilis control). To approach zero waste disposal, bread waste residue (BWR) derived from enzymatic hydrolysis of BW
Catalytic pyrolysis was valorized into syngas. To offer a greener pyrolysis platform for BWR, CO2 was used as a raw material. Here in
this study, the mechanistic functionality of CO2 was disclosed. In detail, CO2 reacted with volatile matters (VMs)
evolved from BWR, thereby resulting in CO2 reduction. Simultaneously, reduced CO2 also led to oxidation of
VMs. Such consecutive gas-phase-reactions (GPRs) played a critical role to enhance CO formation. Lastly, the
identified GPRs induced by CO2 were tried to expedite the reaction kinetics in the presence of 5 wt% of Ni/SiO2
catalyst. As a result, the molar concentrations of H2 and CO in gaseous pyrolytic products derived from catalytic
pyrolysis in CO2 environment were 2- and 6-times higher, respectively, than that from pyrolysis without catalyst
in N2 environment.

1. Introduction
The massive generation of food waste (FW) has been regarded as
problematic because considerable energy, time, labor, and others are
required for their disposal/management (Sabater et al., 2020). The Food
and Agriculture Organization (FAO) reported that 1.6 billion tons of FW
(vegetable oil, fruit, meat, bread, and dairy product) were generated in
2013, and such amount were equivalent to one third of annual/global
food consumption (Ananno et al., 2020; Bottani et al., 2019). Indeed, the
pecuniary loss from FW accounted for US$ 2.6 trillion (Vimala Ebenezer
et al., 2020). The landfilling of FW has been broadly practiced because
they are biodegradable (De Clercq et al., 2017). 76 wt% of FW in the US
were landfilled in 2015 (Muhammad and Rosentrater, 2020). The US
government has tried to adopt the more sustainable disposal methods
that progressively discourage the landfilling of FW. Large quantity of
methane (CH4, greenhouse gas (GHG)) and leachate are discharged from
a single landfill site (Lohila et al., 2007). Anaerobic digestion has been
also practiced to valorize FW (De Clercq et al., 2017). Nonetheless,
anaerobic digestion of FW involves substantial carbon loss by means of
the uncontrollable microbial activities (respiration, cell growth, etc.)
(Ward et al., 2008). It is also of great importance to seek an environ­
mentally benign disposal platform for FW, while maximizing an eco­
nomic viability. To compromise these grand challenges, it could be a
viable option to use FW as the carbon substrates in microalgae
cultivation.
Microalgae-based biorefinery has gained considerable attention
because diverse chemicals and biofuels could be produced from micro­
algae (Chew et al., 2017). Microalgae are generally autotrophic, but
some species are heterotrophic (Hu et al., 2018). Microalgae grown in
the heterotrophic conditions show faster growth rate and higher cell

* Corresponding author.
** Corresponding author.
E-mail addresses: ek2148@hanyang.ac.kr (E.E. Kwon), yechoi@korea.ac.kr (Y.-E. Choi).
1
Co-first authors: The first two authors equally contributed to this work.

https://doi.org/10.1016/j.jclepro.2022.132795
Received 4 February 2022; Received in revised form 2 June 2022; Accepted 18 June 2022
Available online 21 June 2022
0959-6526/© 2022 Elsevier Ltd. All rights reserved.
J.-M. Jung et al.
density in reference to the autotrophic ones (Jung, J.-M. et al., 2021).
The critical economic constraint in microalgae cultivation from the
heterotrophic conditions is the high cost of sugar (glucose) (Sharma
et al., 2011). FWs are comprised of 30–60% of carbohydrate, 5–10% of
protein, and 5% of lipid (Oh et al., 2017). Carbohydrates in FW can be
turned into depolymerized monomer (glucose) by a means of enzymatic
hydrolysis (Sánchez and Cardona, 2008). As such, the use of glucose
derived from FW for microalgae cultivation could be promising. Moon
et al. reported that 46 wt% of glucose from dried FW was obtained via
enzymatic hydrolysis (Moon et al., 2009). Pleissner et al. took advantage
of an enzymatic hydrolysate (glucose from FW) as a nutrient in het­
erotrophic cultivation of microalgae (Pleissner et al., 2013). Nonethe­
less, some compounds/materials in FW (fiber, protein, and fat) remained
even after enzymatic hydrolysis (Zhang et al., 2013).
Among the diverse pathways to valorize the carbonaceous materials
(such as FW), pyrolysis could be also one of the viable options to turn all
carbons in wastes into value-added chemicals and fuels (Zhao et al.,
2010). During the pyrolysis process, the carbonaceous materials are
thermally degraded, and all carbons in solid waste are reassigned into
the three phased pyrogenic products (syngas, oil, and char) in the anoxic
condition (Kim et al., 2020). Biocrude (oil) is one of the main products
from pyrolysis of biomass (Guedes et al., 2018). However, the direct use
of biocrude as fuel could be not be readily realized due to the high
content of oxygen and the high acidity (Gerçel, 2002). A rigorous step
for a series of separation/purification could be also required to obtain
specific compounds from biocrude (Maqbool et al., 2019). The separa­
tion/purification processes could be one of the main constraints to
deteriorate an economic viability in line with the direct use of biocrude
as chemicals/fuels (Cui et al., 2020). As such, conversion of biocrude to
syngas (H2 and CO) could offer a new chance to resolve all noted
problems with the direct use of biocrude. More preferably, a pyrolysis
platform could be more sustainable if CO2 was used as a raw feedstock
(Lee et al., 2017).
Here, in this study, bread waste (BW) were used as a model com­
pound of FW to seek a strategic example for FW disposal/valorization.
Note that one-tenth of bread globally produced (10 million tons bread
per year) become FW (Pietrzak and Kawa-Rygielska, 2015). To valorize
BW into chemicals/fuels, the biological (enzymatic hydrolysis and
microalgae cultivation) and thermo-chemical (catalytic pyrolysis) pro­
cesses were studied in this work. For example, glucose was obtained
from BW by means of enzymatic hydrolysis, and glucose was used as
carbon substrate in heterotrophic cultivation of microalga, Euglena
gracilis to produce value-added chemical, such as paramylon
(conglomerate of β-1,3-glucan). Paramylon is being used in medicines,
cosmetics, etc. (Kim, D.H. et al., 2021). The residue after enzymatic
hydrolysis of BW was turned into syngas as an attempt to realize the
concept of zero-waste. To approach a greener disposal platform, this
study adopted CO2 as a raw material in pyrolysis of the bread waste
residue (BWR). To enhance the usability of CO2 in syngas formation, this
study also scrutinized the synergistic functional effectiveness of a cata­
lyst (5 wt% Ni/SiO2) and CO2 on pyrolysis of BWR.
2. Materials and methods
2.1. Materials
BW was obtained from a local bakery in Seoul, and it was dried in a
convection oven (80 ◦ C) for 1 d. E. gracilis was obtained from culture
collection of autotrophic organisms at the Institute of Botany of the
Academy of Sciences of the Czech Republic. Malic acid was purchased
from Tokyo Chemical Industry (TCI, Japan). Yeast extract was obtained
from BD Biosciences (USA). Sodium phosphate buffer pH 7.6 (0.1 M)
was purchased from Biosesang (Korea). Urea and nickel nitrate hexa­
hydrate (≥97.0%) was purchased from Daejung Chemical (Korea). N2
and CO2 were obtained from Green gas (Korea). TN(CA)-L and COD-M
kits were purchased from HUMAS (Korea).
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Journal of Cleaner Production 365 (2022) 132795
Table 1
Elemental analysis of BWR.
Elemental composition, [wt.%]
Carbon Hydrogen Oxygen Nitrogen Sulfur
46.1 6.9 40.8 3.9 0.3
2.2. Enzymatic hydrolysis of BW
To depolymerize carbohydrate in BW into glucose, amyloglucosidase
was used. 3.75 g of dried BW in 100 mL of distilled water was autoclaved
at 121 ◦ C for 30 min. The mixture of BW and water were incubated with
1 U mL− 1 enzyme (amyloglucosidase) in a shaker (200 rpm) for 30 min.
Hydrolysate was filtered with a 0.2 μm filter to separate glucose and
solid residue (bread waste residue: BWR). The quantity of glucose was
determined using high-performance liquid chromatography (HPLC,
Shimadzu LC-2030C NT) equipped with a refractive index detector
(RID) (Kim, D.H. et al., 2021). The solution was diluted with distilled
water to make initial glucose concentration 20 g L− 1 to be used as a
carbon substrate in cultivation of E. gracilis. The residue (BWR) after
enzymatic hydrolysis of BW was collected. It was rinsed with distilled
water and dried at 80 ◦ C for 2 d. The dried BWR sample was used as a
raw material for the pyrolysis test.
2.3. Microalgae cultivation and paramylon analysis
E. gracilis was maintained in modified Hutner medium (MHM) (Kim,
J.Y. et al., 2019), before the glucose solution (20 g L− 1) was used as the
carbon substrate. For the sources of N/P, yeast extract (10 g L− 1) was
added to the glucose solution, and this solution was referred to as bread
waste medium (BWM) in this study. E. gracilis was cultivated in a 5-L
bioreactor (medium volume: 2.5 L), and the cultivation temperature
was 28 ◦ C. The initial cell density was 106 cells mL− 1. The concentration
of dissolved oxygen (DO) was adjusted above 40% by controlling the
agitation speed and the aeration rate. The pH value (≤4.5) of the me­
dium was maintained using a buffer solution (1 M H3PO4). The reactor
was covered with cloths to offer the heterotrophic condition. Total ni­
trogen (TN) and chemical oxygen demand (COD) of MHM and BWM
were determined using HUMAS kits. The medium was diluted 50-fold to
adjust the concentration within the detection limit of HUMAS kit. Par­
amylon was extracted from E. gracilis using a trypsin solution (1 g L− 1 in
0.1 M sodium phosphate buffer pH 7.6) (Grimm et al., 2015). The har­
vested cells of E. gracilis were rinsed with ethanol and distilled water.
The trypsin solution was added to the sample and incubated at 37 ◦ C 12
h. After incubation, the supernatant was removed, and urea solution
(500 g L− 1) was added to the solid pellet. The urea solution was sorted
out by centrifugation, and the pellet was rinsed with water. The
extracted pallet (paramylon) was dried at 80 ◦ C for 24 h and gravi­
metrically quantified.
2.4. Characterization of BWR
Elemental analysis (Elementar Analysensysteme, GmbH, Germany)
of BWR was carried out to determine the contents of carbon, hydrogen,
oxygen, nitrogen, and sulfur (Table 1). The thermal behaviors of BWR
were characterized using a thermo-gravimetric analysis (TGA) instru­
ment (STA 449 F5 Jupiter, Netzsch, Germany). N2 and CO2 were used as
the purge gases (100 mL min− 1). 10.0 ± 0.1 mg of the BWR sample was
heated from 35 to 900 ◦ C at a constant heating rate (10 ◦ C min− 1).
2.5. Preparation and characterization of Ni/SiO2 catalyst
5 wt% of Ni/SiO2 catalyst was prepared by the incipient wetness
impregnation method (Kim, J.-H. et al., 2021). 25.5 g of nickel precursor
(nickel nitrate hexahydrate) was dissolved in 54.5 g of deionized water
to make a nickel precursor solution. 100 g of silica support was dried at
J.-M. Jung et al. Journal of Cleaner Production 365 (2022) 132795

Table 2 MS, Agilent 7890B/ALMSCO Bench TOF-dx).

Bread waste (BW) generation in many countries.
Country/city Amount of BW Percentage of BW in Reference 3. Results and discussion
(tons yr− 1) total FW (%)

United 292,000 – Narisetty et al. (2021) 3.1. Status of bread waste (BW) generation
Kingdom
Sweden 80,410 12.0–17.0 Brancoli et al. (2019) Global bread consumption was 129 million tons in 2016, and its
Portugal 7.9 Dias-Ferreira et al.
–
market size was equivalent to 349.4 billion US dollars. Due to a short
(2015)
Norway – 27.0 Hanssen et al. (2016) shelf-life and overproduction of bread, ~10 wt% of produced bread
Finland – 13.0 Katajajuuri et al. were generally being discarded (Mena et al., 2011). In the UK, the
(2014) largest consumer of bread in Europe, nearly 0.3 million tons of bread are
Netherlands – 22.0 van Dooren et al. annually wasted (Narisetty et al., 2021). Indeed, a mass portion of BW in
(2019)
FW accounted for 27 wt% (Norway case), which inferred that a large
Hong Kong ≤400 – Han et al. (2015)
New Zealand – 23.0 Goodman-Smith et al. amount of BW is generated globally (Table 2). Disposal of BW without
(2020) their valorizations could be the loss of resources. As noted earlier, the
Saudi Arabia – 18.7 Alruqaie and Alharbi current management options for FW (landfilling and anaerobic diges­
(2012)
tion) could trigger the diverse environmental/economic burdens
South Korea – 2.2 Adelodun et al.
(2021) (Melikoglu et al., 2013).
The main ingredient of bread is wheat flour, which contains a large
amount of carbohydrate (30–50 wt%) that consists of a number of
105 ◦ C. The precursor solution was slowly added to silica support. The glucose monomers linked by glycosidic bonds (Świeca et al., 2017).
impregnated sample was calcined under air at 600 ◦ C for 5 h. Subse­ Given that carbohydrate is depolymerized into glucose through enzy­
quently, reduction of the calcined sample was performed at 510 ◦ C for 4 matic hydrolysis (Azevedo et al., 2003), glucose recovery from BW could
h using 20 vol% H2 (balanced under N2). X-ray diffractometer (XRD, be desirable. Enzymatic hydrolyzation to obtain glucose from BW could
D8-Advance, Bruker-AXS) was used to confirm the crystal structure of be a viable option from a perspective of cost/energy analyses (Zhang
Ni/SiO2 catalyst. et al., 2020). Enzymes are purchased from the commercialized com­
panies such as Novozymes® in affordable cost (Han et al., 2015; Lam
2.6. Pyrolysis of BWR et al., 2014). Given that enzymatic extraction is generally practiced from
the mild conditions (not required high pressure or temperature), energy
Pyrolysis of BWR was done using a horizontal quartz tube (22 mm cost could not be a critical constraint to lower an economic viability
inner diameter × 3 mm thickness × 1,200 mm length) and tubular (Sánchez and Cardona, 2008). Thus, the use of glucose as the carbon
furnace (FT-400, DAIHAN Scientific, Korea). 1.00 g (±0.01) of BWR was substrate in cultivation of E. gracilis could be the desired end use/ex­
loaded in the center of the quartz tube, covered by external tubular ample of BW. Under the heterotrophic circumstance, E. gracilis files up
furnace. For 1-stage pyrolysis, the furnace was heated from 35 to 720 ◦ C paramylon (a conglomerate of β-1,3-glucan) (Kim et al., 2020; Watanabe
(a heating rate of 10 ◦ C min− 1). Either N2 or CO2 was used as a flow gas et al., 2013). Fig. 1 demonstrates the strategic valorization pathways of
(200 mL min− 1). For 2-stage pyrolysis, additional tubular furnace was BW in this study. As noted earlier, glucose was converted from BW via
consecutively installed next to the existing tubular furnace. Both tubular enzymatic hydrolysis. E. gracilis was cultivated heterotrophically to
furnaces operated separately: 1) first heating zone (35–720 ◦ C at 10 ◦ C produce paramylon. BWR valorization was realized via the catalytic
min− 1) and 2) second heating zone (600 ◦ C). Catalytic pyrolysis pyrolysis process. Lastly, a more greener pyrolysis platform for BWR was
employed 5 wt% Ni/SiO2 catalyst in the second heating zone. sought by adopting CO2 as a raw material.

2.7. Product analysis 3.2. Heterotrophic cultivation of E. gracilis using BW

The concentration of the gaseous pyrogenic products from the py­
rolysis reactors were quantified using an online micro gas chromatog­
raphy (micro-GC, INFICON 3000A). The condensable liquid pyrogenic
products were collected in the three cold traps that were filled with
dichloromethane (≥99.8%) at − 10 ◦ C. The major chemical species in the
liquid pyrogenic products (biocrude) were qualitatively determined
using gas chromatography/time-of-flight mass spectrometer (GC/TOF-
Glucose derived from enzymatic hydrolysis of BWs could be used in
cultivation of E. gracilis, but other nutritional elements are required for
cell proliferation and paramylon production (Jung, J.-M. et al., 2021).
As such, yeast extract was intentionally added in hydrolysates stemmed
from BW (designed to bread waste medium: BWM). Yeast extract con­
tains amino acids, vitamins, and trace elements (Vieira et al., 2016). The
concentrations of total nitrogen (TN) and chemical oxygen demand

Fig. 1. Schematic diagram of the study.

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J.-M. Jung et al. Journal of Cleaner Production 365 (2022) 132795

Table 3 Mass of BWR decreased as the TGA test temperature increased. The
Characteristics of modified Hutner medium (MHM) and bread waste medium major mass change of BWR was occurred from 200 to 500 ◦ C. In detail,
(BWM). ~83 wt% of BWR was thermally degraded from 200 to 500 ◦ C. In the
Total nitrogen, [TN, mg L− 1] Chemical oxygen demand, [COD, mg L− 1] DTG curve at ≤ 500 ◦ C, the trends in the thermolysis of BWR were
MHM 1598 ± 30 32981 ± 890
distinctive at 320 and 395 ◦ C. Based on the study by Ria Aniza et al.
BWM 1228 ± 10 45068 ± 691 (2021), the thermolytic rate of carbohydrate and protein became the
highest at 318 and 400 ◦ C, respectively. The thermolytic rate of fat be­
comes the highest at 400 ◦ C (Jung, J.-M. et al., 2021), and the mass
(COD) of BWM were given in Table 3. TN/COD of BWM were compa­ change of fat was realized by means of bond scission of fatty acid from a
rable to those of modified Hutner medium (MHM), which signifies that glyceride backbone of fat (Jung, J.-M. et al., 2021). As such, it was
BWM could be suitable for heterotrophic cultivation of E. gracilis. concluded that the mass change at ≤ 500 ◦ C could be ascribed to the
Heterotrophic cultivation of E. gracilis was done in a 5-L bioreactor thermolyses of carbohydrate, protein, and fat. The functional effec­
using MHM/BWM. The yields of dried E. gracilis and paramylon (Fig. 2 tiveness of CO2 on the thermolysis of BWR was not observed from the
(a)) in MHM for 3 d were 3.23 and 1.56 g L− 1 d− 1, respectively. The entire temperature range in Fig. 3. The residual masses of BWR from the
yields of dried E. gracilis and paramylon in BWM for 3 d were 3.04 and two atmospheric conditions (N2 and CO2) were 17.39 and 17.10 wt%,
1.93 g L− 1 d− 1, respectively. As depicted in Fig. 2(a), the yield of
E. gracilis from both the media was not much different. Nevertheless, the
yield of paramylon from BWM in reference to MHM was 24% higher,
which was in good agreement with the study done by other authors (Kim
et al., 2020). For example, E. gracilis was cultured to obtain paramylon
using FW (brewer’s spent grain and corn steep liquor) (Kim et al., 2020).
However, the yield of paramylon was 0.45 g L− 1 d− 1, which was not
comparable to our result (1.93 g L− 1 d− 1). Therefore, it was concluded
that BWM could be an affordable cultivation medium to heterotrophi­
cally cultivate E. gracilis.
When E. gracilis was grown in MHM/BWM, TN/COD were decreasing
(Fig. 2(b)–(c)). This infers that E. gracilis consumed nutrients in the
culture media. However, the concentrations of TN/COD were not
changed after 3 d of cultivation. This suggests that the growth of
E. gracilis was saturated. The residual sugar (glucose) in MHM/BWM was
also reduced (Fig. 2(d)). Glucose in BWM was nearly depleted from
cultivation of E. gracilis, while 63% of glucose was consumed from
cultivation of E. gracilis in MHM. The concentration of RS was constant
(≥7.5 g L− 1) after 4 d in MHM. Considering that glucose is a main
building block of paramylon, the high yield of paramylon from culti­
vation of E. gracilis in BWM could be reasonable. Such observation was in
good agreement with the previous study (Kim, D.H. et al., 2021).

3.3. Characterization of bread waste residue (BWR)

The thermolysis of BWR over the temperature variations was char­

acterized. In pyrolysis of a carbonaceous material, an inert gas (such as
N2) was used to provide the oxygen-free environment. However, as a
strategic means to offer a greener pyrolysis platform, this study partic­
ularly used CO2 as a raw material. In an effort to seek the functional role
of CO2, the TGA tests of BWR were done from the two atmospheric
conditions (N2 and CO2). The mass changes of BWR from N2 and CO2
Fig. 3. Mass changes of BWR and their thermolytic rates (differential ther­
over the temperature variations were shown in Fig. 3. Also, the thermal
mogram, DTG) from the two atmospheric conditions (N2/CO2).
degradation rates of BWR from N2/CO2 were incorporated in Fig. 3.

Fig. 2. Heterotrophic cultivation of E. gracilis in MHM and BWM. (a) the yields of dried E. gracilis and paramylon, (b) the concentrations of total nitrogen (TN), (c)
chemical oxygen demand (COD), and (d) residual sugar (RS).

4
J.-M. Jung et al.
Fig. 4. Molar concentrations of the major gaseous pyrogenic products (H2, CH4, CO, C2H6, and C2H4) from pyrolyses of BWR under the two atmospheric envi­
ronments (N2 and CO2).
respectively. As such, it was inferred that the Boudouard reaction
(C(s)+CO2(g) ⇌ 2CO(g)) (Hunt et al., 2013) was not realized from a series
of the TGA tests of BWR. Note that the Boudouard reaction is thermo­
dynamically spontaneous at ≥ 710 ◦ C (Lahijani et al., 2015). No
occurrence of the expected Boudouard reaction could be ascribed to the
slow reaction kinetics of CO2 with BWR.
The similar trends in the thermolyses of BWR experimentally proved
no occurrence of the direct (heterogeneous) interactions/reactions be­
tween the BWR sample and CO2. Given that a TGA apparatus only offers
information on the mass change of a solid sample over the temperature
variations, any direct interactions/reactions between the BWR sample
and CO2 result in alteration of the trends in the thermal degradation of
BWR. Such difference was not observed from a series of the TGA tests
under N2 and CO2 conditions (Fig. 3). Indeed, the gas-phase-reactions
(GPRs) between pyrolysates (derived from the thermolysis of BWR)
and CO2 could not be delineated from the TGA test.
3.4. One-stage pyrolysis of BWR
To seek occurrence of the GPRs (that were not caught from a series of
the TGA tests of BWR), pyrolyses of BWR were carried out from 35 to
720 ◦ C under N2/CO2. It was presumed that the GPRs induced by CO2
could alter the compositional matrix of the pyrogenic products. To this
end, the major gaseous pyrogenic products stemmed from BWR under
the two atmospheric conditions were scrutinized in Fig. 4.
The trends in evolutions of the major pyrogenic products in Fig. 4
were in good agreement with the thermolytic behaviors characterized
Fig. 5. (a) Chromatograms and (b) the relative peak areas of the main constituents in BWR biocrude from the two atmospheric environments.
5
Journal of Cleaner Production 365 (2022) 132795
from a series of the TGA tests of BWR. In detail, the thermolytic rates of
BWR (Fig. 3) from the two environments became noticeably retarded at
≥ 500 ◦ C. These retarded thermolytic rates of BWR at 500 ◦ C could be
attributed to carbonization and depletion of volatile matters (VMs)
(Kwon et al., 2019). Carbonization (char formation) is achieved by
means of dehydrogenation/deoxygenation (Jung et al., 2020b). How­
ever, the main reaction mechanism for carbonization is dehydrogena­
tion. The reaction kinetics for dehydrogenation is proportional to the
reaction temperature (Cho et al., 2019), and such feature is well re­
flected in Fig. 4.
The overall trends in evolutions of the major gaseous pyrogenic
products (Fig. 4) from the two gas environments were fairly similar.
These similar evolution trends infer that the functional role of CO2 by
means of the GPRs was negligible. Nonetheless, the functional role of
CO2 by means of the GPRs was marginally shown from the concentration
profiles of CO in Fig. 4. For example, the formation of CO was enhanced
at ≥ 480 ◦ C from the CO2 atmosphere. The enhanced formation of CO
was in good agreement with the previous studies done by the authors
(Kim et al., 2017). In pyrolysis of lignocellulosic biomass, CO2 played a
critical role to enhance the formation of CO by means of the GPRs be­
tween VMs (derived from the thermolysis of biomass) and CO2 at ≥
480 ◦ C (Jung et al., 2020c). Specifically, the functional role of CO2 was
realized through CO2 reduction into CO while simultaneously oxidizing
VMs (Lee et al., 2020). In detail, the chemical reaction between CO2 and
carbon on gas phase VMs derived from pyrolysis of BW resulted in
additional CO formation under CO2 condition. Nonetheless, CO
enhancement at ≥ 480 ◦ C from the CO2 atmosphere was not substantial
J.-M. Jung et al.
Fig. 6. Molar concentrations of the major gaseous pyrogenic products (H2, CH4, CO, C2H6, and C2H4) from 1-/2-stage pyrolyses of BWR under the CO2.
in a sense that most VMs in BWR were nearly depleted at ≤ 500 ◦ C (refer
to the TGA test result in Fig. 4). In other words, a chance for occurrence
of the GPRs between VMs and CO2 could be very scanty. As well re­
flected in Fig. 4, the concentration levels of the major gaseous pyrogenic
products were not substantial. This suggests that most carbons in BWR
should be assigned into biocrude (oil) rather than gaseous pyrolysates
(refer the TGA results in Fig. 3). Conclusively, the main constituents in
BWR biocrude obtained from the two atmospheric conditions must be
identical in that the GPRs induced by CO2 in Fig. 4 were insignificant. To
confirm this, the compositional matrixes of BWR biocrudes from the two
atmospheric conditions were visualized with the representative chro­
matograms in Fig. 5(a). The mass portions specified the chemical
structures of BWR oils from the two atmospheric conditions were also
given in Fig. 5(b). Specific identification of each constituent (in BWR
biocrude) with its peak area was summarized in Table S1.
As evidenced in Fig. 5, the main compositional matrixes of BWR
biocrudes obtained from the two atmospheric environments were fairly
similar. Such similarities imply that the expected GPRs induced by CO2
was not effective in pyrolysis of BWR. Nonetheless, all experimental
findings from Fig. 5 and Table 3 were in good agreement with all claims
given from a series of the TGA tests of BWR in Fig. 3. As claimed earlier,
the distinctive DTG peaks at 320 and 395 ◦ C could be mainly ascribed to
the thermolyses of carbohydrate, protein, and fat in BWR. Such
compositional features were well highlighted in the compositional ma­
trixes of BWR oils. Fatty acids and N-contained (hetero-)hydrocarbons
(HCs) were the main chemical species in BWR biocrude. Given that
amino acid is a monomer of protein (Gorissen et al., 2018), N-contained
HCs in BWR biocrude could be originated from the thermolyses of
protein in BWR (Kim, J.-H. et al., 2020). The large amount of aliphatic
Fig. 7. Molar concentrations of the major gaseous pyrogenic products (H2, CH4, CO, C2H6, and C2H4) from catalytic pyrolyses of BWR over 5 wt% Ni/SiO2 BWR
under the two atmospheric environments (N2 and CO2).
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Journal of Cleaner Production 365 (2022) 132795
HCs in BWR biocrude could be stemmed from the thermolysis of fat
(fatty acids) in BWR biocrude (Kim, J.-H. et al., 2019). The high content
of fatty acids and hetero-HCs could deteriorate the value of BWR bio­
crude as fuel (Kim, J.-H. et al., 2019; Kim, J.-H. et al., 2020). The direct
use of BWR biocrude for fuel is not be free from the environmental
burdens from the formation of the fuel-bounded NOx (Han et al., 2019).
Moreover, oxygenated/acidic HCs could not be desirable in the fuel
properties (Kim, S. et al., 2019). Rigorous separation/purification/up­
grading/deoxygenation steps are required to use BWR biocrude for
practical fuel (Kim, S. et al., 2019), which could be one of the critical
constraints to lower an economic viability. Thus, it could be beneficial to
produce more syngas rather than biocrude. To this end, it could be
required to shift carbon in BWR biocrude into syngas.
3.5. Catalytic pyrolysis of BWR using 5 wt% Ni/SiO2
To seek a way to shift more carbon in biocrude into syngas by means
of the GPRs induced by CO2, the experimental setup was modified. To
promote the GPRs, pyrolysates (evolved from BWR) were further pyro­
lyzed at 600 ◦ C (i.e., 2-stage pyrolysis). The major gaseous pyrogenic
products from 1-/2-stage pyrolyses of BWR under the CO2 condition
were compared in Fig. 6. The concentration profiles of the major gaseous
pyrogenic products from 2-stage pyrolysis of BWR under the N2 condi­
tion were not shown in a sense that the trends in evolutions of the major
gaseous pyrogenic products from 1-stage pyrolysis of BWR from the CO2
environment were not much different.
The enhanced formation of CO could be developed through the GPRs
in 2-stage pyrolysis of BWR. This could be a key clue to confirm carbon
distribution shift from biocrude to CO by means of the GPRs induced by
J.-M. Jung et al. Journal of Cleaner Production 365 (2022) 132795

Table 4
Compositional matrix and peak areas of BWR biocrudes from the different pyrolysis setups: 1-stage, 2-stage, and catalytic pyrolyses.
Group Chemical name (formula) 1-stage 2-stage Catalytic Catalytic

CO2 (Peak area) N2 (Peak area)

Aliphatic
HCs 1-propene (C3H6) 3,443 26,841 27,808 34,299
1-butene (C4H8) 3,550 27,319 28,493 32,642
1,3-butadiene (C4H6) 2,621 32,744 30,965 36,446
2-methyl-1-butene (C5H10) 3,898 5,895 8,883 11,799
heptane (C7H16) 1,334 2,246 1,042 1,728
decane (C10H22) 1,123 1,427 512 1,106
1-decene (C10H20) 586 1,069 401 645
undecane (C11H24) 1,378 470 172 226
dodecane (C12H26) 973 450 113 269
tridecane (C13H28) 1,590 – – –
tetradecane (C14H30) 1,295 – – –
pentadecane (C15H32) 3,893 – – –
hexadecane (C16H34) 899 – – –
heptadecane (C17H36) 1,530 – – –
8-heptadecane (C17H34) 2,730 – – –
Fatty Acids lauric acid (C12H24O2) 9,678 – – –
myristic acid (C14H28O2) 6,075 – – –
palmitic acid (C16H32O2) 29,168 – – –
stearic acid (C18H36O2) 6,648 – – –
oleic acid (C18H34O2) 26,041 – – –
N–HCs 2-propenenitrile (C3H3N) – 6,262 4,882 6,134
3-hydroxypropanenitrile (C3H5NO) 1,931 8,298 5,783 7,734
2-nitropropane (C3H7NO2) 702 – 2,591 2,983
2-pyrrolidinone (C4H7NO) 1,725 – – –
2,5-pyrrolidinedione (C4H5NO2) 1,149 405 1,147 1,605
4-methylpentanenitrile (C6H11N) 793 702 147 320
hexanamide (C6H13NO) 1,680 – – –
heptanamide (C7H15NO) 1,243 – – –
octanamide (C8H17NO) 5,228 – – –
dodecanitrile (C12H23N) 1,210 – – –
heptadecanenitrile (C17H33N) 7,317 – – –
stearonitrile (C18H35N) 2,629 – – –
oleonitrile (C18H33N) 7,623 – – –
Aromatic
HCs benzene (C6H6) 586 26,373 22,546 25,465
toluene (C7H8) 10,288 28,085 22,744 27,114
xylene (C8H10) 1,251 5,574 2,480 3,101
styrene (C8H8) 1,264 7,569 7,016 6,730
ethylbenzene (C8H10) – 1,928 1,640 1,952
2-propenylbenzene (C9H10) – 1,256 894 1,082
ethyl toluene (C9H12) – 2,159 1,527 1,846
indane (C9H10) – 1,006 797 797
1-methyl-2-propylbenzene (C10H14) – 1,302 970 1,069
azulene (C10H8) – 1,998 2,217 2,277
Phenolic compounds phenol (C6H6O) 3,059 2,275 1,461 1,678
4-methylphenol (C7H8O) 4,490 2,268 285 873
N–HCs pyrrole (C4H5N) 519 3,509 3,794 4,984
pyridine (C5H5N) 1,028 2,640 1,308 2,092
4-methylpyridine (C6H7N) 548 1,453 1,119 1,368
indole (C8H7N) 1,741 1,031 1,038 1,749

CO2. The overall concentrations of the major gaseous products (except pyrolysis of BWR could be also a reason for delineating the enhanced
for CO) also were substantially enhanced from 2-stage pyrolysis of BWR. formation of CO.
This clarifies that the enhanced formation of CO could not be solely Under the circumstance of the same energy input, it is of great
explained by means of the GPRs induced by CO2. Specifically, enhanced importance to expedite the reaction rates for the GPRs induced by CO2
thermal cracking induced by additional thermal energy in 2-stage rather than thermal cracking for the more generation of syngas from
pyrolysis of BWR. In an effort to compromise this grand challenge,
catalytic pyrolysis of BWR over 5 wt% Ni/SiO2 under the CO2 envi­
Table 5 ronment was done. The major gaseous pyrogenic products from catalytic
Mass balance of three phase products from the different pyrolysis setups: 1- pyrolyses of BWR under the two atmospheric environments were
stage, 2-stage, and catalytic pyrolyses. compared in Fig. 7. For a comparison purpose, the highest concentration
Products Yield (wt.%) of each gaseous component from 2-stage pyrolysis of BWR from the CO2
1-stage 2-stage Catalytic Catalytic
environment was marked with a dotted line as a reference in Fig. 7.
Under the presence of 5 wt% Ni/SiO2, the concentration of CO from
CO2 N2
the CO2 atmosphere was noticeably enhanced. The reverse water-gas-
Solid (char) 17 16 16 17 shift (rWGS) reaction could offer a chance to enhance the formation of
Liquid (biocrude) 75 41 7 10
a CO (Jung, S. et al., 2021). Nonetheless, rWGS could not be the main
Gas (syngas and others) 8 33 77 73
mechanistic pathway for the enhanced generation of CO in a sense that
a
Calculated: Gas yield = 100% – Solid yield – Liquid yield.

7
J.-M. Jung et al.
enhance formation of CO cannot be delineated by stoichiometry of rWGS
(González-Castaño et al., 2021). It is noted that 1 mol of H2 turns into 1
mol of CO by means of rWGS (González-Castaño et al., 2021). Thus, it
was concluded that the enhanced generation of CO from the CO2 con­
dition in Fig. 7 could be elucidated by the catalytically enhanced GPRs.
Such observation is of great importance since that the greener disposal
platform for BWR (biomass) could be achieved by means of transferring
CO2 into CO.
As the results of GPRs and catalytic pyrolysis, the formations of
gaseous products were significantly improved (Table 5). The catalytic
pyrolysis under CO2 condition led to conversion of more than two thirds
of solid BW into syngas and flammable HCs that are main components in
natural gases.
The GPRs induced by CO2 (in Fig. 7) offer the several implications in
the thermal treatment of biological waste. First, CO2 could be used as a
resource. Second, the GPRs induced by CO2 offers a new strategic chance
to enhance the more generation of syngas by means of shifting carbon
distribution from long-chained/large HCs into syngas. Third, the GPRs
induced by CO2 could greatly reduce a chance for coke deposition on the
catalyst surface by means of the enhanced formation of CO (i.e., scav­
enging carbon by CO2) (Jung et al., 2020a). Such carbon scavenging
feature could be of great importance in that the GPRs induced by CO2
offer a chance to make a more reliable catalytic platform for biomass
valorization (Jung et al., 2020a). In an effort to confirm the noted
functional effectiveness of CO2 in line with the GPRs, the compositional
matrixes from the different pyrolysis tests of BWR were qualitatively
compared in Table 4. The functional effectiveness of CO2 is well high­
lighted in Table 4. For example, CO2 served a critical role for scavenging
(consuming) carbons in biocrudes. Therefore, the compositional ma­
trixes of biocrudes from the CO2 environment exhibited the less
diversity.
4. Conclusions
In this study, the hybridized biological/chemical processes were
introduced to offer an innovative strategy for food waste disposal. In
addition, the concept of zero-waste in disposal of bread waste (BW) was
experimentally practiced. In detail, diverse routes for valorization of BW
were sought. First, carbon in BW was depolymerized into a monomeric
sugar (glucose), and glucose was used for the main nutrient in hetero­
trophic cultivation of E. gracilis. From a perspective of an economic
viability, the yield of value-added chemical (paramylon) from the two
culture media (HMM and BWM) was compared. This study experimen­
tally proved that the more sugar in BWM was assimilated into para­
mylon, and such production yield delineated the real value of FW as a
raw material for chemical synthesis by means of the biological pathway.
To achieve zero-waste disposal, solid residue of bread waste (BWR)
obtained after enzymatic hydrolysis of BW was upgraded into syngas. To
provide more sustainable pyrolysis platform for BWR, CO2 was utilized
as a reaction medium. In detail, CO2 and VMs derived from pyrolysis of
BWR resulted in additional CO formation through the GPRs. Lastly, the
identified GPRs induced by CO2 were tried to expedite the reaction ki­
netics in the presence of 5 wt% of Ni/SiO2 catalyst.
CRediT authorship contribution statement
Jong-Min Jung: Investigation, Formal analysis, Writing – original
draft, Data curation. Jee Young Kim: Investigation, Formal analysis,
Writing – original draft, Data curation. Jung-Hun Kim: Investigation,
Formal analysis. Shin Myung Kim: Formal analysis, Data curation.
Sungyup Jung: Formal analysis, Data curation, Writing – review &
editing. Hocheol Song: Formal analysis, Data curation, Investigation,
Resources. Eilhann E. Kwon: Conceptualization, Supervision, Investi­
gation, Resources, Writing – review & editing. Yoon-E Choi: Concep­
tualization, Supervision, Investigation, Resources, Writing – review &
editing.
8
Journal of Cleaner Production 365 (2022) 132795
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.
None.
Acknowledgments
This research was supported by NRF (National Research Foundation
of Korea) grant funded by the Korean Government (MSIT;
2019R1A2C2087449 and 2020R1A2C1010748).
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.jclepro.2022.132795.
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