Catalytic pyrolysis of Abandoned Fishing Nets using Activated Carbon Derived from Wasted Clamshell with in-situ and ex-situ Catalyst Configuration
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Environ. Eng. Res. 2023; 28(3): 220162 pISSN 1226-1025
https://doi.org/10.4491/eer.2022.162 eISSN 2005-968X
Research
Catalytic pyrolysis of Abandoned Fishing Nets using Activated
Carbon Derived from Wasted Clamshell with in-situ and ex-situ
Catalyst Configuration
Soosan Kim1, Seonho Lee2, Hee Sue Lee2, Wooyoung Yang2, and Jechan Lee2,3
1
Energy Systems Research Center, Ajou University, Suwon, 16499, Republic of Korea
2
Department of Global Smart City, Sungkyunkwan University, Suwon, 16419, Republic of Korea
3
School of Civil, Architectural Engineering, and Landscape Architecture, Sungkyunkwan University, Suwon, 16419, Republic of Korea
Received April 13, 2022 Revised June 28, 2022 Accepted July 6, 2022
ABSTRACT
Fishing net is considered as one of the biggest problem in the world owing to the release of micro-plastics from abandoned fishing nets, which
contributes to marine pollution. Although disposal and recycling strategies are considered as effective methods for overcoming these problems,
the pyrolysis of abandoned waste has emerged as a strategy to recover massive quantities of waste materials. In this study, to develop an effective
method to valorize abandoned fishing net, the effect of the use of a CaCO3 catalyst after the loading method (i.e., in-situ and ex-situ) on pyrolytic
products of abandoned fishing net was investigated using micro-gas chromatography and gas chromatography/mass spectrometry. Compared
to non-catalytic pyrolysis, catalytic pyrolysis increased the yield of non-condensable and condensable gas. Particularly, the ex-situ method significantly
increased the yield of non-condensable gas to up to 37.2 wt.% at 900. Compared to the ex-situ method, in-situ loading method increased the
yield of condensable products to up to 82 wt.%. The understanding of the difference between different catalyst loading configurations will provide
useful insight on thermocatalytic waste conversion processes.
Keywords: Catalytic pyrolysis, Fishing net, Retrieving raw material, Waste recycling
Graphical Abstract
†
This is an Open Access article distributed under the terms Corresponding author
of the Creative Commons Attribution Non-Commercial License E-mail: jechanlee@skku.edu
(http://creativecommons.org/licenses/by-nc/3.0/) which per-
Tel: +82-31-219-2402
mits unrestricted non-commercial use, distribution, and reproduction in any
medium, provided the original work is properly cited. Fax: +82-31-219-1613
ORCID: 0000-0002-9759-361X
Copyright © 2023 Korean Society of Environmental Engineers
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Soosan Kim et al.
1. Introduction study demonstrated the use of calcinated scallop shells as catalyst
during pyrolysis, and they found that the catalyst reduced the
peak temperature [35]. In addition, the use of CaCO3 as a catalyst
Fish is one of the most consumed organic food in the world [1].
for increasing the quantity of oil production has been demonstrated
According to the Food and Agriculture Organization of the United
[36]. Gulab et al. reported that the use of CaCO3 as a catalyst
Nations (FAO), the global per capita consumption of fish was approx-
in the co-pyrolysis of biomass and polyethylene increased the
imately 20.5 kg in 2019 [2]. With the growth of the marine industry,
yield of oil compared to the yield under non-catalyst condition.
the amount of plastic wastes on the sea has increased as people
Moreover, CaCO3 was observed to favor the formation of aromatic
abandon numerous used plastic materials (fishing nets, buoys) in
hydrocarbons [37].
the sea [3]. Hence, untreated plastic wastes have remained in the
Although the degradation of nylon-6 has been widely investigated
ocean [4]. Particularly, fishing net is considered as the most serious
for a long time, it has rarely been used to recover polymer monomers
problem in marine biology, and it makes up 10% of the total marine
from waste material [38, 39]. In this study, we performed the valor-
waste [5]. For example, abandoned fishing net interrupts the swim-
ization of wasted fishing nets through catalytic pyrolysis over two
ming pattern of fishes as the net binds them [6]. In addition, plastic
different catalyst configurations (i.e., in-situ and ex-situ) using clam-
nets are sometimes regarded as food, and are consumed by fishes
shell waste. Two types of pyrolytic products, including gaseous
(or they emit feed smell, which lures fishes into the net, where
and liquid products, were identified and analyzed.
they cannot escape from) [7]. Consequently, these have resulted
in the death of numerous marine creatures and the destruction
of the marine ecology [8]. Moreover, the destruction of wasted
fishing nets by waves results in the production of micro-plastic,
2. Materials and Methods
which are very harmful to marine organism [9]. However, these
plastic nets cannot be degraded naturally [10]; thus, it is essential 2.1. Materials and Chemicals
to develop an appropriate treatment approach for micro-plastics. Abandoned fishing net and clamshell waste (CSW) were obtained
Generally, wasted plastic fishing nets are treated using recycling from a harbor located in the city of Buan, Republic of Korea. The
and landfill strategies. The recycling of plastic nets is a good method obtained plastic net was washed to remove soil, debris, and salt,
for treating wasted plastic fishing nets owing to its ability to remove after which it was soaked in water for 24 h and then dried in
waste without polluting the environment [11]. However, this method a drying oven at 60 ºC for 48 h. Dichloromethane (DCM; 99.9%
requires a high labor intensity [12] and costs [13]. Landfill is one purity) supplied by Samchun chemical (Seoul, Republic of Korea)
of the easiest and common method for disposing plastic waste. was used as the solvent. 5-methlyfurfural (5MF; 99% purity) was
Although this method is convenient [14] and simple [15], it can purchased from Sigma–Aldrich (St. Louis, MO, USA), and N2 gas
pollute underground water [16], occupy large area [17], and emit was purchased from DK gas (Hwaseong, Republic of Korea).
harmful materials [18].
To overcome the disadvantages of the consisting methods, ther- 2.2. Preparation of Activated Carbon Material
mochemical processes such as pyrolysis [19], gasification [20] and CSW catalyst was prepared in this study using the following
liquefaction [21] were emerged. Recently, these methods have been procedure. First, the purchased CSW was cleaned using water to
developed to increase efficiency by adding catalysts to obtain high remove surface impurities, after which it was dried at 60 ºC for
yield of production as well as to suppress coke formation [22]. 24 h. Subsequently, the dried shells were broken using a mortar
Thermochemical processes have upgraded the quality of products and pestle, and then ground into a fine powder using a pulverizer
using two different substances (e.g., biomass and plastic) simulta- (New Korea Metal Company, Republic of Korea). Thereafter, the
neously [23-25]. powders were separated based on their particle size using a sieve
In this study, we performed pyrolysis of plastic to treat plastic shaker (SS-D-S, Woo Ju Scientific, Republic of Korea) to ensure
efficiently as an effective chemical recycling strategy [26]. Pyrolysis that the small particles (>600 mm) of CSW powders were obtained.
has been used as a promising method to valorize various plastic Subsequently, the powders were placed in a tube furnace for carbon-
materials, such as polyethylene terephthalate (PET) [27, 28], ization at 400 ºC for 2 h under flowing N2 gas at 100 mL min-1.
low-density polyethylene (LDPE) [29], and polypropylene (PP) [30]. Thereafter, the powders were mixed with KOH solution (6 M)
The pyrolysis of plastic materials produces pyrolytic oil and py- at a ratio of 1:3, and then dried at 60 ºC for 48 h. The dried
rolytic gas in the absence of oxygen. Pyrolytic oil can be used powders were heated again using a tube furnace from 400 to 700
as an alternative fuel because it is composed of various kinds of ºC with a holding time of 30 min for 1 h at a heating rate of
condensable compounds [31]. In addition, pyrolytic gas produces 3 ºC min-1 under N2 gas. Lastly, the obtained activated materials
H2 (Hydrogen) CO (Carbon monoxide), CH4 (methane), and CO2 were mixed with HCl solution (2 M) in a water bath at 90 ºC
(Carbon dioxide), as well as hydrocarbons from C1 to C3, which to purify and remove the metal-oxide produced during the carbon-
can be used as energy sources [32-34]. ization process. The solution containing the powder was washed
Although pyrolysis is a relatively simple method and offers val- with deionized water several times until the pH of the solution
ue-added chemicals, it exhibits a high energy consumption owing was neutral, after which they were dried at 60 ºC.
to the requirement of an external energy supply to sustain the
required temperature during the process. To solve this problem, 2.3. Feedstock Characterization
catalysts are employed during pyrolysis. For example, a recent Proximate analysis of the wasted fishing net was performed using
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Environmental Engineering Research 28(3) 220162
a batch furnace. First, the moisture content was measured by placing 2.5. Pyrolytic Product Analysis
the fishing net on an uncovered crucible in the furnace at 105 The pyrolytic oil produced during the pyrolysis process was ana-
ºC for 24 h. Subsequently, the volatile matter content of the feedstock
lyzed using gas chromatography/mass spectrometry (GC/MS;
was determined by heating the covered crucible at 450 ºC for 1 Agilent 5975C, USA). The components of the pyrolytic oil were
h. Thereafter, the ash content was estimated when the open crucible qualified and quantified using an Agilent HP-5ms column (30 m
was heated at 750 ºC for 1 h. Lastly, the fixed matter content
× 0.25μm × 0.25 mm). The detailed conditions, including the
was calculated by subtracting the moisture, volatile matter, and temperature, heating rate, and flow rate, are listed in Table S1.
ash contents from the original mass. The quantitative analysis was conducted via internal standard meth-
The ultimate analysis of the elemental compositions of the fishing
od using Methylfurfural (5 μg mL-1).
net was performed using a Thermo Scientific FlashSmart 2000 The pyrolytic gas was analyzed using micro GC (Inficon,
elemental analyzer. The C, H, N, and S contents were calculated Switzerland). In addition, H2 and carbon monoxide (CO) gases
using a copper wire and tungstic anhydride catalysts at 1000 ºC.
were quantified using Rt-Molsieve 5A (0.25 mm × 10m); carbon
The content of O was estimated by calculating the difference be- dioxide (CO2), methane (CH4,), and hydrocarbons (from C1 to C4)
tween the initial mass and the sum of ash, C, N, H, and S contents. were identified using the Rt-Q-Bond (0.25 mm × 8 m). The specific
Table 1 shows the result of proximate and ultimate analysis.
conditions are listed in Table S2.
Table 1. Proximate and Ultimate Analysis of Fishing Net
Analysis Contents Composition (wt.%) 3. Result and Discussion
Moisture 2.01
Volatile compound 97.48 3.1. Characterization of Fishing Net
Proximate
Fixed carbon 0.01 Fig. 1 shows the change in the weight of the fishing net samples
analysis
Ash 0.5 with a change in temperature under N2 flow. Fig. 1 shows the
Total 100 TGA (thermogravimetric analysis) and DTG (Derivative
C 63.06 Thermogravimetry) curves of the fishing net. The first weight loss
N 12.27 of the fishing net was observed at 400 ºC, after which the weight
H 10.28 rapidly decreased until 500 ºC. With an increase in the temperature
Ultimate
to 900 ºC, more than 97 wt.% of the fishing net was thermally
analysis O(by difference) 15.35
degraded, which could be attributed to the thermal decomposition
S -
of volatile matter (i.e., devolatilization occurred). However, approx-
Total 100 imately 3.0% of the fishing net was not thermally decomposed
owing to the presence of fixed carbon. This result is very consistent
2.4. Pyrolysis Experiment with the proximate analysis result presented in Table 1: the fishing
net sample consisted of fixed carbon (0.01 wt.%), volatile matter
Three types of pyrolysis of fishing net (i.e., without catalyst, ex-situ,
(97 wt.%), and moisture (2 wt.%) without ash. This indicates the
and in-situ) were conducted using a tube furnace (Tube furnace-60,
high consistency of the TGA and proximate analysis results.
Hantech, Republic of Korea). Figure S1 shows the scheme of the
Ultimate analysis also revealed that fishing net were composed
pyrolysis process. The feedstock was placed in a quartz tube located
of 63.06 wt.% carbon, 12.27 wt.% nitrogen, 10.28 wt.% hydrogen,
at the center of the heating zone with a gas mask. For the ex-situ
and 15.35 wt.% oxygen
experiment, the catalyst was loaded next to the feedstock between
quartz wools. In contrast, for the in-situ process, the catalyst was
mixed with the fishing net, after which the mixture was placed
between quartz wools. Mass flow controller (KOFLOC, Japan) was
connected to a gas mask, through which N2 flows into the quartz
tube at 100 mL min-1 to achieve an oxygen-free atmosphere. The
pyrolysis temperature was controlled using the temperature con-
troller attached to the tube furnace.
The pyrolytic oil produced during the pyrolysis process was
collected using four inpingers. Because the oil was composed of
volatile compounds, the inpingers were located in the cold region.
The first inpinger contained 40 mL of DCM and it was placed
in an ice bath where the temperature was maintained at -1 ºC.
Next to the first inpinger, three inpingers were consecutive soaked
in cold traps where the temperature was sustained at -55 ºC using
a mixture of acetone and dry ice. To collect all the pyrolytic oil,
the inpingers, quartz tube, and line were washed with DCM. The
collected oil was dried at 60 ºC for 24 h to remove the DCM. Fig. 1. TGA result of the fishing net.
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Soosan Kim et al.
3.2. Analysis of Non-condensable Gas in temperature under all conditions; however, that of C2H4 de-
Fig. 2a shows the yield of non-condensable gas obtained from the creased between 500 and 600 ºC, and then increased until 900
ºC. The H2 produced from catalytic pyrolysis was higher than
pyrolysis of fishing net with and without catalyst with a change
that produced during the non-catalytic pyrolysis at all temper-
in temperature. The total yield of non-condensable gas increased
atures, and the difference between the results was not negligible
with an increase in the pyrolysis temperature. For example, there
(Fig. 3a). However, at temperatures above 700 ºC, the difference
was no significant difference in the total yield of gas at 500 and
in the H2 yield increased significantly. This could be attributed
700 ºC; however, with a further increase in temperature to 800
to the fact that an increase in the pyrolysis temperature promoted
°C, the total yield from the ex-situ process dramatically increased
the decomposition of vaporized species released from the feedstock
from 7.7 to 29.3%, and increased to 37.2% with a further increase
during the pyrolysis process [41]. In addition, compared to the
in temperature to 900 ºC. This could be attributed to the enhance-
non-catalytic pyrolysis, the ex-situ pyrolysis method generated
ment of the pyrolysis of volatile substances through gas and gas–sol-
more H2, but this was lower than that generated from the in-situ
ids reactions at high temperatures [40]. Further, the gas with the
pyrolysis method. This indicates that the use of CSW catalyst
highest concentration obtained during the pyrolysis processes was
for the pyrolysis of fishing net can increase the production of
CO2 (Fig. 2b). Although there was no significant difference in the
H2 gas, and the in-situ method generated a higher quantity than
evolution of the gas species in the absence of a catalyst, the difference
the ex-situ method. The quantity of generated CO from the pyrolysis
was enhanced when the catalyst was loaded. Particularly, the ex-situ
of fishing net is shown in Fig. 3b. Further, the use of CSW enhanced
loading method produced the highest quantity of CO2 compared
the generation of CO. It was expected that CO formation via reverse
to the non-catalytic and in-situ process. This may be attributed
to the generation of CO2 by the decomposition of the CSW catalyst. water-gas-shift reaction (rWGS, H2 + CO2 -> CO + H2O) could
The catalysts were prepared using CSW, which consists of calcium be realized using the CO2 produced from the CSW catalysts. Thus,
the CO2 produced by the calcination reaction of CSW catalyst
carbonate (CaCO3). With an increase in temperature, CaCO3 was
(CaCO3 -> CaO + CO2 +183kJ/mol) was used as a source of
decomposed into CO2, which was enhanced in the presence of
a catalyst. Accordingly, as more CSW was used during the ex-situ the WGS reaction [42]. Compared to the aforementioned gases
(Fig. 3c and 3d), there was no significant in the amount of CO2
process compared to the in-situ reaction, more CO2 was produced
generated from non-catalytic and ex-situ catalytic pyrolysis with
during the ex-situ reaction, which was evident at temperatures
an increase in the pyrolysis temperature. In contrast, the quantity
of 700 ºC or higher.
of gas generated by the in-situ method was higher than those
As shown in Fig. 3, the major gaseous products from the pyrolysis
produced by other methods. These results offer two messages.
of fishing net were H2, CO, CH4, and C2H4. In addition, C2H6, C3H6,
and C3H8 were observed in the product, but their concentration First, the effect of catalysts is evidence at temperatures above
700 ºC. Second, the in-situ method is more effective than the
was not comparable to those of the four major gas (Fig. 2). Further,
the concentration of H2, CO, and CH4 increased with an increase ex-situ method for producing combustible gas except CO.
a a
Fig. 2. (a) Yield of non-condensable gas at different pyrolysis temperatures; and (b) product distribution of non-condensable gas at 900 ºC for
the non-catalytic, in-situ catalytic, and ex-situ catalytic pyrolysis of fishing net.
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Environmental Engineering Research 28(3) 220162
a b
c d
Fig. 3. Volumetric portion of (a) H2, (b) CO, (c) CH4, and (d) C2H4 gas produced from the in-situ, ex-situ, and non-catalytic pyrolysis of fishing
net under N2 flow.
3.3. Analysis of Condensable Products and 1,8-diazacyclotetradecane-2,9-dione.
Fig. 4 shows the total yield of condensable products (Fig. 4a)
The weight of condensable products produced by the fishing net
and the distribution (Fig. 4b) of the condensable gas obtained from
was 48.5 to 88.8 wt.%, and the yield of liquid was highest at 500
the fishing net with and without catalysts at various pyrolysis
and 600 ºC and was lowest at 900 ºC at all conditions. The con- temperatures. The in-situ and non-catalytic pyrolysis exhibited sim-
densable gas produced from the pyrolysis of fishing net was com- ilar trend, in which the concentration of condensable products
posed of 3-pyrrolidinopropionitrile, four kinds of amine compounds decreased with increasing the pyrolysis temperature. However,
(azepan-2-one, 7-butyl-3,4,5,6(2H)-tetrahydroazepine, 2,3,4,5,6,7- there was a slight difference in the trend of the ex-situ pyrolysis
hexahydro-2-octylimino-1H-azepine, and oleylamine), 4-hex- compared to the other methods. With an increase in temperature
yl-2,5-dihydro-2,5-dioxo-3-furanacetic acid, 13-heptadecyn-1-ol, from 500 to 600 ºC, the concentration of condensable products
5
Soosan Kim et al.
a b
Fig. 4. (a) Yield of condensable products at different pyrolysis temperatures for the non-catalytic, in-situ catalytic, and ex-situ catalytic pyrolysis of
fishing net; (b) Distribution of the condensable gas obtained from the non-catalytic, in-situ catalytic, and ex-situ catalytic pyrolysis at 500 ºC.
increased, and then decreased until 900 ºC. For example, the amount conditions) under N2 condition to retrieve value-added chemical
of condensable products generated during the non-catalytic py- material. The study was conducted within the temperature range
rolysis and in-situ pyrolysis decreased from 45.1 to 33.7 wt.% and from 500 to 900 ºC. The total yield of non-condensable gas increased
from 63.6% to 53.3 wt.%, respectively. In contrast, the concentration with an increase in temperature. Particularly, at temperatures above
of condensable products produced during the ex-situ pyrolysis in- 700 ºC, the difference between the yield of non-condensable gas
creased from 46.2 to 50.2 wt.%, and then decreased to 39.3 wt.%. generated during the non-catalytic pyrolysis and ex-situ catalytic
Particularly, the quantity of condensable products generated by pyrolysis increased significantly owing to the occurrence of calcina-
the in-situ pyrolysis was higher than those generated by other meth- tion reaction. However, a higher amount of the major gases, except
ods at all temperatures. This result implies that the mixture of CO, was produced during the in-situ method compared to the
solid particles and feed would exhibit an effect on heat and mass ex-situ method. The HHV of pyrolytic gas was 5.4 MJ/kg, indicating
transfer [43], as well as increase the intimate contact of the feed that it can be used as an alternative energy source for the pyrolysis
with the catalyst and the change in the vapor residence time in reaction. The generated condensable products were mainly com-
the reactor [44]. This is consistent with the result of a recent study posed of amine compounds at all condition. Particularly, in-situ
on the comparison of the in-situ and ex-situ co-catalytic pyrolysis catalytic pyrolysis produced the highest yield of condensable prod-
of high-density polyethylene and torrefied yellow poplar, which ucts at 500 ºC. This work revealed that not only value-added
revealed that in-situ catalytic co-pyrolysis exhibited higher perform- chemical can be retrieved via pyrolysis of marine wastes, such
ance than ex-situ catalytic co-pyrolysis [45]. The distribution of as fishing net, but alternative energy sources could be generated.
the products obtained from the Non, in-situ and ex-situ catalytic
pyrolysis of fishing net at 500 ºC is shown at Figure 4b. Condensable
products were composed of amide, amine, acid, alcohol, and ketone Declaration of competing interest
compounds. Particularly, amine compounds exhibited the highest
The authors declare that they have no conflict of interest.
proportion (amine compounds consisted of 95.5 wt.%% of the total
products) at all conditions. However, the remained products were
not produced as high as amine compound. Particularly, in in situ
Acknowledgements
loading method, the proportion of amide, acid, alcohol, and ketone
compounds in the condensable gas product was 0.6, 1.1, 0.2, and This work was supported by the National Research Foundation of
3.7 wt.%, respectively. This could be attributed to the composition Korea (NRF) grant funded by the Korea government (MSIT) (No.
of fishing net: fishing nets are composed of polyamide, so the 2021R1A4A1031357). This work was also supported by C1 Gas
high-temperature depolymerization reaction enabled the extraction Refinery Program through the National Research Foundation of Korea
of the major compounds from the complete product. (NRF) funded by the Ministry of Science, ICT and Future Planning
(2015M3D3A1A01064899).
4. Conclusions
Author contributions
This study performed the catalytic pyrolysis of fishing net consist-
ing of nylon-6 using CSW catalyst (under in-situ and ex-situ loading S.K. (Researcher) conducted all the experiments and wrote the
6Environmental Engineering Research 28(3) 220162
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student) supported to conduct experiments and prepared the 2018.11.110.
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