toxics
Article
Potential Application Performance of Hydrochar from Kitchen
Waste: Effects of Salt, Oil, Moisture, and pH
Xuesong Su 1 , Jizu He 1 , Muhammad Amjad Khan 1 , Kenlin Chang 2 , Yin Liu 1 , Genmao Guo 1 , Xiaohui Li 3, *,
Fangming Jin 1 , Meijuan Kuang 4 , Shaban Gouda 5 and Qing Huang 1, *
Citation: Su, X.; He, J.; Khan, M.A.;
Chang, K.; Liu, Y.; Guo, G.; Li, X.; Jin,
F.; Kuang, M.; Gouda, S.; et al.
Potential Application Performance of
Hydrochar from Kitchen Waste:
Effects of Salt, Oil, Moisture, and pH.
Toxics 2023, 11, 679. https://doi.org/
10.3390/toxics11080679
Academic Editor: Tiecheng Wang
Received: 30 June 2023
Revised: 30 July 2023
Accepted: 31 July 2023
Published: 8 August 2023
Copyright: © 2023 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Toxics 2023, 11, 679. https://doi.org/10.3390/toxics11080679
1 School of Ecology & Environment, Hainan University, Haikou 570228, China
2 Institute of Environmental Engineering, Department of Public Health, National Sun Yat-Sen University,
Kaohsiung 804, China; klchang@mail.nsysu.edu.tw
3 Hainan Inspection and Detection Center for Modern Agriculture, Haikou 570100, China
4 Hainan Pujin Environmental Engineeering, Haikou 570100, China
5 Agricultural and Biosystems Engineering Department, Faculty of Agriculture, Benha University,
Toukh 13736, Egypt
* Correspondence: xdnycdhj@163.com (X.L.); huangqing@hainanu.edu.cn (Q.H.); Tel.: +86-155-9578-5619 (Q.H.)
Abstract: The surge in kitchen waste production is causing food-borne disease epidemics and is a
public health threat worldwide. Additionally, the effectiveness of conventional treatment approaches
may be hampered by KW’s high moisture, salt, and oil content. Hydrothermal carbonization (HTC)
is a promising new technology to convert waste biomass into environmentally beneficial derivatives.
This study used simulated KW to determine the efficacy of hydrothermal derivatives (hydrochar)
with different salt and oil content, pH value, and solid-liquid ratio for the removal of cadmium
(Cd) from water and identify their high heating value (HHV). The findings revealed that the kitchen
waste hydrochar (KWHC) yield decreased with increasing oil content. When the water content
in the hydrothermal system increased by 90%, the yield of KWHC decreased by 65.85%. The
adsorption capacity of KWHC remained stable at different salinities. The KWHC produced in
the acidic environment increases the removal efficiency of KWHC for Cd. The raw material was
effectively transformed into a maximum HHV (30.01 MJ/kg). HTC is an effective and secure method
for the resource utilization of KW based on the adsorption capacity and combustion characteristic
indices of KWHC.
Keywords: hydrochar; adsorption; combustion; resource utilization; food waste
1. Introduction
Human population growth and improved living standards have resulted in a sharp
rise in kitchen waste (KW) production. Foodborne illnesses caused by KW are still very
prevalent and public, which has a huge impact on global public health (for example, African
swine fever and recycling of gutter oil). Although strict regulations and advanced food
safety systems regulate the disposal of kitchen waste, millions of people still get sick, and
thousands of people die of related foodborne illnesses every year [1]. In addition, the
public panic caused by COVID-19 may have resulted in an increase in online food shopping
and disruption of the food supply chain, both of which further expanded the production
of KW and put additional pressure on waste management systems [2]. Many countries
are looking for new waste disposal methods and systems to cope with the environmental
pressures and potential risks posed by KW during the pandemic [3]. KW is typically
characterized by a high oil, salt, and moisture content due to human dietary habits and
practices [4]. These characteristics severely reduce the effectiveness of conventional waste
treatment techniques, including landfilling, incineration, and biological treatments, which
can also cause secondary sources of environmental pollution [5]. It has been reported
that the salt in KW is one of the reasons for the presence of dioxins in waste incineration
https://www.mdpi.com/journal/toxics
Toxics 2023, 11, 679 2 of 19

gas; similarly, the oil in KW forms leachates [6]. The chemical complexity and biological
toxicity of landfill leachate eventually migrate into soil and water, endangering public
health and environmental security [7]. Furthermore, the high moisture content in KW
reduces the efficiency of biological approaches (e.g., anaerobic digestion, composting) and
increases operating costs [8]. Appropriate disposal of KW is the key issue to maintaining
environmental sustainability and is crucial to its safe and effective disposal and utilization.
It has been a challenge for researchers to find a more rational resource treatment method to
assign the value of KW during the epidemic.
Hydrothermal carbonization (HTC), a new method of waste resource utilization, has
gained increasing attention from researchers in recent years due to the lack of restrictions on
the water content of the raw material and the fact that it does not require pre-drying, making
it more suitable for biomass waste. At a certain temperature and self-generated pressure,
HTC can quickly convert organic matter into carbon-rich products using water as a solvent
and reaction medium [9]. Prior research has discovered that COVID-19 was inactivated
by heating at 56 ◦ C for 30 min [10]. In addition, early articles demonstrated that the
HTC reaction temperature is relatively high (150–350 ◦ C) and can be used for sterilization
to reduce pathogens and prevent infection [11]. Therefore, HTC is a more suitable KW
disposal method to reduce potential risks for public health and safety. Meanwhile, as heavy
metal adsorbents and fuel replacements, hydrothermal derivatives also offer extraordinarily
high value for environmental applications [9].
Cadmium (Cd) is one of the most toxic heavy metals that can contaminate the soil and
build up in plants, which poses a risk to humans [12,13]. The scarcity of fossil fuels and
the inability of energy utilization structural monophyly to maintain globally growing fuel
demand and environmental sustainability, as well as the search for energy alternatives, are
imminent [14]. While KW hydrothermal derivative (hydrochar) can not only be used to
recover Cd-contaminated wastewater due to its porous and carbon-rich properties, it can
also be made as an alternative to traditional fuels, alleviating pollution of the environment
and global energy problems [15].
HTC offers an alternative for rapid, safe, and resource-based treatment of KW. How-
ever, when applying HTC to KW treatment, the material specificity of its high salt and high
oil content, which affects the mechanism of the physicochemical properties and application
performance of HTC process and its derivatives, is still not clear; pH and solid-liquid
ratio were taken as significant parameters to influence the hydrothermal reaction, and
the mechanism of their effects on the application of KW to HTC still deserves further
exploration [16].
In this study, HTC is employed to further improve the environment while easing the
burden of solid biomass waste disposal. The objectives of the present study are: (1) to
produce kitchen waste hydrochar (KWHC) from KW with various contents of salt and oil,
pH, and solid-liquid ratios; (2) to identify the effects of KWHC prepared with different
oil, salt, pH, and solid-liquid ratios on the Cd adsorption capacity and the combustion
characteristics of KWHC; and (3) to explore the correlation between oil, salt, and the
application performance of hydrothermal derivatives of KW.

2. Materials and Methods

2.1. Materials
In this study, rice, eggs, and lettuce were used as typical components representing
carbohydrates, protein, and cellulose as a simulated KW, and the proportion of components
used was mentioned in [17]. The solid-liquid ratio of 1:5 provided the highest yield of
hydrochar during the pre-experiment; hence, it was chosen as the blank control (CK).
On the other hand, four treatments were prepared using different salt concentrations (S),
solid-liquid ratios (R), pH (P), and oil concentrations (O). Moreover, various contents of
edible salt (0.5%, 1%, 5%, and 10%) were added to the simulated KW afterwards, referred
to as S1, S2, S3, and S4, respectively. Similarly, the simulated KW and water with different
solid-liquid ratios of 1:1, 1:5, 1:10, and 1:20 were prepared afterwards and named R1, R2,
Toxics 2023, 11, 679 3 of 19

R3, and R4, respectively. For pH, solutions of 3, 5, 8, and 10 pH values were adjusted with
NH3 •H2 O and HNO3 to make hydrochar, and different oil contents of 10%, 20%, 30%, and
40% were adjusted using cooking oil labeled P1, P2, P3, and P4, and O1, O2, O3, and O4,
respectively. All treatments are listed in Table 1.

Table 1. Treatments of the hydrothermal carbonization experiment.

Samples Rice (g) Egg (g) Vegetables (g) Salt (g) Oil (g) Water (g) pH
S1 9.99 ± 0.02 2.67 ± 0.02 0.67 ± 0.00 0.067 ± 0.00 0.00 66.67 ± 0.01 7
S2 9.99 ± 0.03 2.67 ± 0.00 0.67 ± 0.00 0.13 ± 0.00 0.00 66.67 ± 0.16 7
S3 9.99 ± 0.01 2.67 ± 0.00 0.67 ± 0.00 0.67 ± 0.00 0.00 66.67 ± 0.03 7
S4 9.99 ± 0.01 2.67 ± 0.00 0.67 ± 0.01 1.33 ± 0.00 0.00 66.67 ± 0.03 7
O1 9.99 ± 0.00 2.67 ± 0.02 0.67 ± 0.03 0.00 1.33 ± 0.02 66.67 ± 0.02 7
O2 9.99 ± 0.01 2.67 ± 0.00 0.67 ± 0.00 0.00 2.67 ± 0.02 66.67 ± 0.03 7
O3 9.99 ± 0.00 2.67 ± 0.00 0.67 ± 0.00 0.00 3.99 ± 0.01 66.67 ± 0.01 7
O4 9.99 ± 0.01 2.67 ± 0.00 0.67 ± 0.00 0.00 5.33 ± 0.01 66.67 ± 0.01 7
P1 9.99 ± 0.02 2.67 ± 0.02 0.67 ± 0.01 0.00 0.00 66.67 ± 0.05 3
P2 9.99 ± 0.00 2.67 ± 0.00 0.67 ± 0.01 0.00 0.00 66.67 ± 0.03 5
P3 9.99 ± 0.00 2.67 ± 0.00 0.67 ± 0.01 0.00 0.00 66.67 ± 0.05 8
P4 9.99 ± 0.00 2.67 ± 0.00 0.67 ± 0.01 0.00 0.00 66.67 ± 0.01 10
R1 30.00 ± 0.02 8.00 ± 0.02 2.00 ± 0.02 0.00 0.00 40.00 ± 0.01 7
R2(CK) 9.99 ± 0.02 2.67 ± 0.02 0.67 ± 0.01 0.00 0.00 66.67 ± 0.01 7
R3 5.45 ± 0.01 1.15 ± 0.02 0.36 ± 0.02 0.00 0.00 72.72 ± 0.02 7
R4 2.86 ± 0.01 0.76 ± 0.02 0.19 ± 0.02 0.00 0.00 76.19 ± 0.03 7

2.2. Hydrothermalcarbonization of Synthetic KW

All the prepared treatments were placed in a high-pressure hydrothermal reactor
(KH, Reactor, Wuhan, China) at 200 ◦ C for 10 h. After cooling to room temperature, the
solid-liquid parts were separated by 0.45 µm filter paper. Finally, hydrochar was dried at
80 ◦ C overnight to a constant weight.

2.3. Adsorption Capacity of KWHC

2.3.1. Sorption Kinetics
Kinetic models provide an explanation of adsorbent behavior. To evaluate the adsorp-
tion capacity, 0.2 g of each KWHC sample was added to a centrifuge tube containing 40 mL
of a 50 mg/L Cd solution. For 10, 20, 30, 90, 120, 150, 180, 240, and 300 min, the centrifuge
tubes oscillated at a temperature of 30 ◦ C at 180 rpm/min [18]. Pseudo-first-order (PFO)
and pseudo-second-order (PSO) models were used to describe the adsorption behavior.
The PFO and PSO kinetic models are represented in Equations (1) and (2), respectively,
as follows:
qt = qe(1 − exp(−k1 t)), (1)

k2 qe2 t
qt = , (2)
1 + k2 qet
where qe and qt are the adsorption capacities at equilibrium (mg/g) and time t (h), respec-
tively, and k1 and k2 are the kinetic adsorption rate constants for the PFO and PSO models
(h−1 ), respectively.

2.3.2. Sorption Isotherms

In the KWHC adsorption experiments, the Cd (II) solution concentrations were set
at 10, 20, 50, 100, 200, and 500 mg/L. KWHC (0.2 g) and 40 mL of Cd (II) solutions were
added into 50 mL centrifuge tubes [19]. The samples were shaken at 160 r/min at 25 °C for
24 h to achieve adsorption equilibrium [20]. The Langmuir and Freundlich models were
used to describe adsorption behavior.
The Langmuir and Freundlich models are represented in Equations (3) and (4), respec-
tively, as follows:
Ce 1 Ce
= + , (3)
qe qmKl qm
Toxics 2023, 11, 679 4 of 19

1
lgqe = lgKF + lgCe, (4)
n
where qm is the theoretical maximum adsorption capacity (mg/L), Ce is the equilibrium
concentration (mg/L), Kl is the Langmuir adsorption coefficient (L/mg), KF is the Fre-
undlich adsorption coefficient (L/g), and n is the adsorption strength (-).
The Cd (II) concentration was measured after the supernatant was filtered through
a 0.45 µm filter membrane. An atomic absorption spectrometer (TAS-990 SUPER AFG,
Beijing, China) was used to analyze Cd (II) concentrations.
The adsorption quantity of KWHC was calculated according to Equation (5):

(C0 − C1 ) × V
q= , (5)
m
where q is the adsorption quantity of KWHC (insert unit), C0 and C1 are the initial and
equilibrium concentrations of Cd (II) (mg/L), respectively, m is the adsorbent mass (g), and
V is the adsorption solution volume (L).

2.4. Thermogravimetric Analysis of KWHC

The combustion characteristics were tested by a thermal gravimetric analyzer (TG,
209 F3, China). An alumina sample cup containing 10 mg of sample was loaded into
the analyzer. The sample was heated to 40–105 ◦ C for 5 ◦ C per min, held at isothermal
conditions for 10 min to remove residual water, and then heated to 800 ◦ C at a rate of 20 ◦ C
per min in an N2 atmosphere to obtain decomposition data [21].
To provide further information on the combustion activity of the samples, Ti and
Tb were used to calculate the combustibility index (S) through Equation (6) to reflect the
overall combustion rate:
(dw/dt)max × (dw/dt)mean
S= , (6)
Ti 2 ×Tb

where (dw/dt)max and (dw/dt)mean correspond to the maximum and average rate of
weight loss (% wt./min), respectively, and Ti and Tb are the ignition temperature and
burnout temperature (◦ C), respectively.
In addition to peak deconvolution, Ti , peak temperature (Tp), and Tb were determined
from difference thermogravimetry (DTG) profiles using the TG-DTG tangent method [22].

2.5. Chemical Analysis of KWHC

Using an elemental analyzer (Elementar Vario EL cube, Germany), the contents of
carbon (C), oxygen (O), hydrogen (H), and nitrogen (N) in hydrochar were measured. The
higher heating value (HHV) of the samples was calculated according to Equation (7) [23].

HHV = 0.3383 × C + 1.422 × (H − O/8), (7)

where HHV is the higher heating value (MJ/kg), C, H, and O are the mass contents of
carbon, hydrogen, and oxygen (wt.%), respectively.

2.6. Analytical Methods

The functional groups were analyzed by Fourier Transform Infrared Spectrometry
(FTIR) (FTIR-650, Andong, China). The potassium bromide (KBr) and hydrochar samples
were mixed at a ratio of 1:100 and pressed into tablets. The spectral range measured was
4000–400 cm−1 . The mineral compositions were measured by X-ray diffraction (XRD,
DX-2700BH, China).
Toxics 2023, 11, 679 5 of 19

2.7. Statistical Analysis

Statistical analyses were performed by the analysis software SPSS v.18.0 for Windows
(IBM-SPSS, Statistics 22, Armonk, NY, USA). Means were compared by single-factor analy-
sis of variance (significant difference, p < 0.05). The structural equation model showed the
direct and indirect effects of salt, oil, pH, and solid-liquid ratio on the yield, adsorption,
and calorific value of KWHC. “*”, “**”, and “***” indicate significant differences at p < 0.05,
p < 0.01, and p < 0.001, respectively. The black solid arrows and the gray dashed arrows
represent a positive and negative relationship, respectively.

3. Results
3.1. Effects of Salt, Oil, pH, and Solid-Liquid Ratio on KWHC Productivity
The productivity of KWHC was stable with increasing salt content, except in the
treatment with 10% salt content, where the KWHC productivity slightly decreased by 4.11%
compared to CK (Figure 1a). According to the results of the present study, the oil content
had a negative relationship with the KWHC yield. The KWHC yield decreased from 64.80%
to 48.52% as the oil content of KW increased from 10% to 40% (Figure 1b). The productivity
of KWHC in the acid solutions (pH 3 and pH 5) was not significantly different compared
with the blank control, and there was also no observable yield difference under alkaline
conditions (Figure 1c). With the increase in solution pH from 3 to 8, the productivity of
KWHC decreased slightly by 5.21%. With the increase in water content in the hydrothermal
reaction system, the yield of hydrochar showed a declining trend (Figure 1d). When the
hydrothermal system’s water content increased from 50% to 95%, the production of KWHC
decreased by 65.85%.

ff
Figure 1. The productivity of KWHC as affected ff
by different treatments: (a) salt contents, (b) oil
ff
contents, (c) pH, and (d) solid-liquid ratios. For an experimental variable, different tt
letters indicate
ff
significant differences in concentration changes between the same treatments (p < 0.05).

3.2. Elemental Analysis of the KWHC

In KWHC, the C and N contents decreased by 6.81% and 13.26% after HTC, when the
salt content increased from 0.5% to 10%. The salt had no striking effect on the H content.
ff
The oil content strongly affected the elemental composition of KWHC. As the oil content
ff
increased, the C and N contents decreased by 31.20% and 37.69%, respectively. The carbon
content of KWHC decreased with decreasing pH in the range of 5 to 7. The C/N ratio in
Toxics 2023, 11, 679 6 of 19

KWHC increased with increasing pH (3–10). The solid-liquid ratio of 1:5 KWHC resulted
in the highest C/N ratio (Table 2).

Table 2. Composition analysis of hydrochar.

Ultimate Analysis (% d.b) Atomic Ratio

Samples C N H O H/C O/C C/N
S1 64.01 4.69 5.72 16.19 1.072 0.190 15.596
S2 62.13 4.65 5.84 18.78 1.128 0.227 15.913
S3 63.18 4.32 5.56 19.21 1.056 0.228 17.050
S4 59.65 4.07 5.59 18.84 1.125 0.237 17.097
O1 68.80 4.24 7.07 18.56 1.234 0.202 18.940
O2 66.90 3.82 7.18 18.18 1.287 0.204 20.430
O3 67.28 3.82 6.80 18.82 1.212 0.210 20.547
O4 47.33 2.64 4.58 16.97 1.160 0.269 20.913
P1 64.06 5.08 6.30 21.69 1.181 0.254 14.707
P2 62.01 4.52 6.30 19.11 1.220 0.231 16.016
P3 69.73 4.97 5.56 18.32 0.957 0.197 16.374
P4 66.17 4.55 5.78 18.66 1.048 0.212 16.986
R1 65.26 3.03 5.64 21.14 1.036 0.243 25.145
R2 (CK) 63.67 4.27 5.99 20.60 1.129 0.243 17.401
R3 64.47 4.52 6.17 18.22 1.149 0.212 16.626
R4 66.61 5.19 5.90 20.14 1.063 0.227 14.975

3.3. Adsorption of Cd (II) on KWHC with Different Treatments

Increasing salinity increased the Cd (II) removal efficiency of KWHC by 10.76%, which
showed that high salt content in KW promoted the adsorption performance of KWHC
(Figure 2a). With increasing oil content, the adsorption quantity and removal efficiency of
hydrochar in the solution with a high Cd (II) concentration decreased by 12.16%, which
means that the oil content had little adverse effect on the adsorption capacity of the
hydrochar (Figure 2b). The adsorption capacity of KWHC increased with the increase in pH
of the aqueous Cd (II) solutions. The removal capacity of hydrochar for Cd (II) increased
by 12.71% with the increase in the solution pH from 3 to 10 (Figure 2c). Increased water
content in the hydrothermal process reduced the Cd (II) adsorption capacity of KWHC. The
treatments prepared with a solid-water ratio of 1:5 had the highest adsorption capacity out
of all the treatment groups. The increase was 28.22% compared to the lowest adsorption
group (1:20 solid-water ratio) (Figure 2d).

3.4. Combustion Characteristics Analysis

3.4.1. HHV Analysis of KWHC
The HHV of CK KWHC was 26.376 MJ/kg. It has a high HHV compared to similar
waste hydrochar. For example, the HHV of sludge hydrochar was 9.04 MJ/kg, and with the
addition of 10% NaCl, its HHV decreased to 6.92 MJ/kg. The hydrochar HHV obtained in
the co-hydrothermal experiment of rape straw and microalgae was 22.30 MJ/kg. The HHV
of cattle manure hydrochar was 17.21 MJ/kg. With increased salt content, the calorific
value of hydrochar decreased slightly. The HHV of KWHC was only reduced by 7.8% even
when the salt content reached 10%. The HHV of KWHC decreased significantly by 35.07%
when the oil content increased. However, even when the oil fraction was as high as 40%,
hydrochar still exhibited a high calorific value (19.49 MJ/kg). Regarding pH, the HHV
of KWHC was slightly enhanced (4.12%) under alkaline conditions compared to acidic
conditions. As the amount of water in the hydrothermal process increased, the KWHC’s
HHV marginally increased (3.8%) (Table 3).
 Ⅱ
Ⅱ

Toxics 2023, 11, 679 7 of 19

Figure 2. Langmuir and Freundlich adsorption models of KWHC. Notes: (a) salt contents; (b) oil
contents; (c) pH; and (d) solid-liquid ratios.

Table 3. Combustion parameters of the KWHC.

Sample Ti (◦ C) Tp (◦ C) Tb (◦ C) S (%2 /◦ C−3 ·min2 ) HHV(MJ/Kg)

S1 246.74 349.98 481.95 6.86 × 10−7 26.886
S2 246.52 353.73 505.43 5.01 × 10−7 25.969
S3 253.84 352.02 503.87 5.26 × 10−7 25.846
S4 256.70 407.13 541.00 4.87 × 10−7 24.768
O1 tt 286.38 379.78 468.32 7.74 × 10−7 30.014
O2 281.38 379.78 472.32 7.58 × 10−7 29.583
O3 280.10 386.93 474.60 5.12 × 10−7 29.060
O4 243.92 382.33 543.91 4.93 × 10−7 19.488
P1 248.91 357.84 475.68 7.36 × 10−7 26.762
P2 247.82 364.92 506.87 5.48 × 10−7 26.525
P3 228.98 377.19 504.17 5.85 × 10−7 28.217
P4 227.89 377.19 549.33 4.66 × 10−7 27.266
R1 278.79 412.44 548.03 4.70 × 10−7 26.316
R2(CK) 252.80 349.84 536.76 4.59 × 10−7 26.376
R3 273.81 353.44 478.28 6.45 × 10−7 27.331
R4 235.26 351.14 500.81 7.10 × 10−7 27.330

The results of the present study revealed that salt had no significant impact on the
HHV of KW hydrothermal derivatives. However, KW with a high oil content still exhibits
excellent combustion performance after hydrothermal treatment. The phenomenon of the
high heating value increasing with the increase in pH corresponds to increased C content
and decreased O and H contents in the KWHC. It has been reported that the ratio of C
increases with the increase in alkalinity, indicating that carbonization is intensified [24]. The
contents of O and H decreased due to the formation of CO2 and H2 O by dehydration and
decarboxylation reactions during HTC (Table 3) [25]. This occurred because increasing the
water concentration accelerates the hydrolysis reaction during the hydrothermal process.
The rapid breakdown reaction brought on by increased water content is another factor
contributing to the increase in the HHV of hydrochar (Table 3) .
All treatments were found to have extremely high HHV (19.49–30.01 MJ/kg) (Table 3).
As Zhang et al. (2020) illustrated, the increase in HHV may be caused by the cleavage of
low-energy chemical bonds and the formation of high-energy chemical bonds in hydrochar
during HTC [26]. The outcome showed that even when the KW has a high level of salt
Toxics 2023, 11, 679 8 of 19

and oil, the hydrothermal process can still turn biomass waste into solid fuel with good
calorific value. The pH and water contents in the hydrothermal process do not need to
be tightly controlled to maintain the HHV of hydrochar (Table 3). Considering that KW
cannot be adequately treated with conventional procedures due to its high oil, salt, and
moisture content, the harmful effects of these components can be effectively avoided using
the hydrothermal approach. Compared to other treatment options, this treatment has a
distinct benefit regarding renewable energy.

3.4.2. Thermogravimetric Analysis of KWHC

Using the weight loss peaks in the combustion DTG curve as a guide, the combustion
of KWHC may be separated into three steps. The first stage is the drying stage, where water
evaporates completely before 120 ◦ C [27]. The second stage is the loss of volatile matter,
and the combustion stage occurs at about 240 ◦ C. There is a noticeable weight loss peak due
to a large number of volatile compounds burning and the heat produced by combustion
intensifying the combustion response [28]. The DTG curve exhibits a second conspicuous
weight loss peak in the third stage, which corresponds to the combustion stage at roughly
380 ◦ C. The primary cause is the transformation of the chemicals for the second-stage mass
loss into those for the third-stage combustion Figure 3a,c,e,g. Additionally, fixed carbon
combustion occurring during the hydrothermal reaction is the real source of the mass loss
in the third stage [29].

3.4.3. FTIR Analysis of KWHC

The adsorption capacity of hydrochar is related to surface complexation and ion
exchange by surface functional groups [30]. The spectra of KWHC before the adsorption
tests are depicted in Figure 4a–d). The -OH stretching vibration is close to 3400 cm−1 [30].
The -COOH vibration absorption peak around 1705 cm−1 is mainly due to absorption
by lipids and carboxylic acids [30]. Clearly, the peaks of hydroxyl and carboxyl groups
changed significantly after the adsorption of Cd, and the peaks of -OH and -COOH were
shifted from 3405 cm−1 to 3456 cm−1 , and 1705 cm−1 to 1751 cm−1 , respectively, as shown in
Figure 4e–h. Consequently, these two functional groups play a critical role in the adsorption
reaction due to their ability to interact strongly with Cd (II) through ion exchange and
surface complexation [31]. The C-O vibration bands appear at 1430 cm−1 and in the region
from 1000 to 1300 cm−1 . Interestingly, the C-O peak shifted from 1300 cm−1 to 1351 cm−1
in Figure 4e,h), suggesting that the C-O band also has a noticeable effect on adsorption by
hydrochar prepared at different solid-water ratios. The bands between 1000 and 1300 cm−1
for hydrochars prepared at 1:1 and 1:5 solid-liquid ratios become more intense. Vibrational
changes in these functional groups may be related to the high adsorptivity of hydrochar
with a low water content.
HTC’s solid products have excellent chemical and thermal stability, and thermogravi-
metric analysis and FTIR results confirm that there will be little secondary pollution during
the recycling of KW [32].
Toxics 2023, 11, 679 9 of 19

Figure 3. TG and DTG curves of KWHC combustion: (a,b) salt contents, (c,d) oil contents, (e,f) pH,
and (g,h) solid-liquid ratios. b
Toxics 2023, 11, 679 10 of 19

ff
Figure 4. FTIR spectra for KWHC prepared under different conditions before and after Cd (II) Ⅱ
ff
adsorption; (a,c,e,g) represent different treatment groups of KWHC before adsorption; and (b,d,f,h)
ff
represent different treatment groups of KWHC after adsorption.

3.4.4. XRD Analysis of KWHC

The graphitization degree of KWHC can be characterized by XRD and could have
an impact on the combustion reaction. According to XRD data, the graphite structure
of hydrochar was not significantly altered by the oil or salt concentrations of KW. At 2θ θ
values of about 20◦ –30◦ , the typically sharp and narrow peak of graphite vanished and
was replaced by a broad peak (Figure 5). This means that the development of this peak
demonstrated the extent of carbonization and the presence of the graphite structure in the
hydrochar [33]. Liang et al. (2022) reported that hydrochar can be utilized as a replacement
for conventional fuels since it has a structure that is comparable to that of bituminous
coal [15]. The XRD results indicated that variations in oil, salt, water, and pH will not
Toxics 2023, 11, 679 11 of 19

ff the flammability of the hydrothermal derivatives of KW. This further

significantly affect
demonstrates the high thermal stability of the KW hydrothermal derivatives.

ff
Figure 5. X-ray diffraction of hydrochar: (a) salt contents, (b) oil contents, (c) pH, and (d) solid-liquid
ratios. ♦represents sodium chloride (NaCl).

4. Discussion
4.1. Effects of Salt, Oil, pH, and Solid-Liquid Ratio on the Productivity of KWHC
ff
4.1.1. Effect of Salt Content on the Productivity of KWHC
ff
Salt slightly inhibits the production of KWHC. According to Ma et al. (2021), NaCl
can catalyze the release of more organic compounds into the aqueous phase during the
hydrothermal process, and Cl− can disrupt the ether bonds between monosaccharides,
catalyzing the hydrolysis of cellulose and causing a decrease in solid content [34]. It
was assumed that the causes of this phenomenon were the same in our case. The salt
concentration did not significantly affect the yield of KWHC (p > 0.05).
ff
4.1.2. Effect of Oil Content on Productivity of KWHC
Theff production of carbon decreases with an increase in oil content. The possible
explanation for this reduction in yield may lie in the fact that lipids undergo complex
processes to produce monoglycerides and fatty acids by hydrolysis and oxidation reactions
tt
at high temperatures [35]. Some volatile lipids evaporate or turn into gas, lowering the
amount of fat in the solid phase and the solid mass [36]. Lipids also speed up the amidation
reaction and create numerous liquid phases, lowering the yield of hydrochar [12].

4.1.3. Effect of the pH of the Solution on the Productivity of KWHC

The production of KWHC is higher under acidic conditions. It was reported that
acid canffdrive the self-assembly of F127 micelles and pentose in cellulose to form a stable
structure and contribute to the formation of hydrochar [37]. Meanwhile, the fatty acids pro-
duced during protein hydrolysis can aid in the breakdown of holocellulose into hydrochar
and produce chemicals that prevent further degradation of biomass waste [38]. Similarly,
tt
Toxics 2023, 11, 679 12 of 19

alkaline catalysts prevent the development of hydrochar, and an alkaline environment

tends to reduce hydrochar generation [39].

4.1.4. Effect of the Solid-Liquid Ratio on the Productivity of KWHC

High moisture content reduces the yield of KWHC. This can be accounted for by the
faster conversion of wet biomass at a lower solid concentration, which leads to the almost
total dissolution of the organic matter with minimal residue [13]. Additionally, when the
water content drops, subcritical water results in significant carbonization, leading to the
development of additional hydrochar [40]. According to reports, the solid load should
be as large as feasible to enhance the production of hydrochar [41]. In comparison to salt,
oil, and pH, the results demonstrated that the solid-to-water ratio has the most significant
impact on the yield of hydrochar.

4.2. Effects of the Salt, Oil, pH, and Solid-Liquid Ratio on Elemental Analysis of KWHC
4.2.1. Effects of Salt on the Elemental Analysis of KWHC
The C, N, and H contents decrease with increasing salt content. Similar results were
obtained by Ma et al. (2021), who reported that the elemental contents of hydrochar with
a high salt content were relatively lower than those of hydrochar without salt or with a
low salt content [24]. This suggests that NaCl can catalyze hydrolysis and decarboxylation
during hydrothermal carbonization, bringing more organic matter into the liquid phase
and lowering the amount of solid phase produced [42].

4.2.2. Effects of Oil on the Elemental Analysis of KWHC

Increasing the oil content reduces the nitrogen content. This may be because proteins
participate in amination and Maillard reactions; adding lipids weakens the intensity of the
Maillard reaction, which results in a weaker N-heterocyclic structure. At the same time,
enhancement of the amination reaction will promote decarboxylation and deamination
reactions, further reducing the N content in hydrochar [43]. The O/C ratio showed a distinct
increasing trend with the increase in oil content, which implied that the decarboxylation
reaction might be promoted by oil in the hydrothermal reaction [12].

4.2.3. Effects of pH on the Elemental Analysis of KWHC

Under the high temperature and alkaline conditions, the C/N ratio in KWHC increased
with increasing pH (3–10) due to the loss of N [44,45].

4.2.4. Effects of the Solid-Liquid Ratio on the Elemental Analysis of KWHC

The solid-liquid ratio of 1:5 KWHC resulted in the highest C/N ratio. This finding
agreed with the results of Kavindi et al. (2022). The content of N increased by 70% with the
increase in water content (Table 2). Xu et al. (2021) explained that the increase in N content
might be caused by the aggravation of the decarbonization and dehydration reactions by
water [45].

4.3. Adsorption of Cd (II) on KWHC with Different Treatments

4.3.1. Effects of Salt on Adsorption of Cd (II) on KWHC
Two explanations may be given for the enhancement of the adsorption capacity of
KWHC by raising the salt content. Firstly, the Na+ ions will increase with increased salt
addition. However, Na+ does not compete with Cd (II) for negatively charged adsorption
sites, and the electrostatic repulsion between the two positive ions does not hinder the
loading of Cd (II) at the surface sites. The mechanism by which Cd (II) is removed is
primarily inner sphere complexation [4,46]. Secondly, in desalination techniques, for most
capacitive deionization (CDI) studies, an increase in NaCl concentration will lead to an
increase in salt adsorption capacity (SAC), which could affect the specific surface area of
carbon materials [47]. Moreover, salinity has little effect on the hydrothermal treatment of
KW, which demonstrates that the hydrothermal approach can effectively limit the adverse
Toxics 2023, 11, 679 13 of 19

impact of high salt content in KW and provide steady Cd (II) adsorption performance in
hydrothermal products.

4.3.2. Effects of Oil on Adsorption of Cd (II) on KWHC

According to the findings of this study, it can be assumed that the hydrothermal
approach can effectively reduce the drawbacks brought on by high oil content and maintain
the Cd (II) adsorption efficiency of hydrochar at a generally steady level. Jin et al. (2016)
showed a successful hydrolysis of organics in KW to small molecules and inorganic species
after thermal treatment, and a considerable portion of the oil fraction was dissolved from
the KW into the liquid phase [26]. Hydrothermal procedures have better degreasing efficacy
than conventional pre-treatments, which many researchers have employed to effectively
de-oil KW [7].

4.3.3. Effects of pH on Adsorption of Cd (II) on KWHC

This phenomenon of Cd (II) adsorption increasing with the decrease in solution pH
can also be explained by the competition between metal ions and protons for binding sites
decreasing with increasing pH, so that metal ion binding sites become easier to obtain [47].
Cui et al. (2016) speculated that the protonation/deprotonation of surface functional groups
on the hydrochar is influenced by the water’s pH, which in turn impacts the adsorption
reaction [38]. The presence of H3 O+ or H+ ions, which compete with Cd (II) for adsorption
sites, may cause a reduction in adsorption capacity at low pH [48]. Another explanation
could be that the acidic functional groups are protonated at lower pH levels, which results
in widespread metal ion repulsion and less Cd (II) adsorption [49]. Increasing pH increases
the adsorption capacity due to the cationic -π interaction between Cd (II) and hydrochar.
This is attributed to the deprotonation of carboxyl and hydroxyl groups, where the weak π
electron donor of the -COOH functional group is deprotonated to form -COO-, a strong π
electron donor [37,39,48,49].

4.3.4. Effects of Solid-Liquid Ratio on Adsorption of Cd (II) on KWHC

The results show that the water content is important for the mechanism of HTC
because the carbonization process is accelerated by water [50]. On the one hand, water acts
as a favorable medium for the ionic interaction of nonpolar organic molecules during the
HTC process. Particularly during the hydrolysis process, high temperatures cause the break
of hydrogen bonds, increasing the amount of H+ and OH− ions [41,51]. Due to competition
for adsorption sites and a decrease in adsorption capacity, a high water content will result
in a high H+ ion content [51]. On the other hand, water molecules may participate in
carbonization reaction steps as reactants or products, facilitating hydrolysis, hydrogen
exchange, condensation, and cleavage. However, the amount of water that is needed
for these functions is minimal. With lower solid-water ratios, there have been reports
that the hydrochar surface can form more oxygen-containing functional groups because
the hydrochar surface is susceptible to hydrolysis. This may result in an increase in the
adsorption capacity of the hydrochar [52]. It can be inferred from the experimental results
that the use of an appropriate solid-liquid ratio can effectively increase the adsorption
efficiency of hydrochar. However, the influence of water content on the Cd (II) adsorption
performance of hydrochar needs further study.
According to the analysis of the adsorption efficiency of KWHC, the removal efficiency
of KWHC is higher when the Cd (II) content in solution is low, while it is lower when the
Cd (II) concentration is high. The KWHC is more suitable for adsorbing and removing low
Cd (II) concentrations from aqueous solutions.

4.4. Adsorption Mechanism of KWHC

4.4.1. Sorption Isotherms
According to the analysis of the fitting degree of the equilibrium concentration of
Cd (II) adsorption and the adsorption capacity of KWHC using the Langmuir adsorption
Toxics 2023, 11, 679 14 of 19

model and the Freundlich models, the fitting coefficient of Langmuir is higher than that
of Freundlich, as illustrated in Figure 2 and Table 4. Therefore, the isothermal adsorption
model of KWHC is more suitable for the Langmuir model, which proves that the adsorption
mechanism of KWHC for Cd (II) is a single-layer homogeneous adsorption process [53,54].
This further confirms that KWHC has a greater affinity for Cd (II), and stable inner spherical
complexes can be generated inside KWHC to enhance the coordination of Cd (II) with
surface functional groups (-OH, -COOH) [47,54].

Table 4. Langmuir and Freundlich model parameters.

Langmuir Freundlich
Treatment Qmax (mg/g)
b R2 n R2
S1 4.31 4.06 0.89 0.50 0.80
S2 5.31 7.22 0.92 0.54 0.85
S3 6.02 8.41 0.90 0.52 0.81
S4 8.13 11.14 0.86 0.48 0.76
O1 12.80 11.27 0.98 0.17 0.95
O2 10.93 8.61 0.92 0.15 0.98
O3 10.22 14.98 0.97 0.20 0.94
O4 6.87 7.51 0.93 0.36 0.96
P1 15.16 8.60 0.94 0.15 0.98
P2 7.23 8.19 0.99 0.35 0.88
P3 7.62 9.69 0.88 0.37 0.70
P4 4.10 4.30 0.97 0.31 0.90
R1 16.90 21.22 0.98 0.47 0.90
R2 (CK) 18.33 22.24 1.00 0.43 0.94
R3 15.99 19.86 0.98 0.43 0.90
R4 11.08 12.35 1.00 0.37 0.92

4.4.2. Sorption Kinetics

The fitting results of the adsorption equilibrium time for Cd (II) and the adsorption
capacity of KWHC show that both the PFO and PSO models can well fit the adsorption
performance of KWHC for Cd (II). The adsorption capacity of KWHC for Cd (II) increases
rapidly with time, tends to stabilize after 50 min, and then reaches the adsorption equilib-
rium (Figure 6). From the analysis of the fitting coefficients of the PFO and PSO models,
the PSO fitting coefficient of KWHC is higher than the PFO kinetic fitting coefficient, which
indicates that the adsorption process of KWHC for Cd (II) is mainly chemical adsorption
(Table 5) [55]. Chemical adsorption results from the chemical bond force between the solid
surface of the adsorbent and the adsorbed substance, which greatly exceeds the Van der
Waals force of physical adsorption, and the chemical adsorption process is irreversible [56].
Therefore, chemical adsorption is more stable for the fixation of adsorbates than physical
adsorption [57]. The adsorption mechanism of KWHC on Cd (II) is chemical adsorption,
and its adsorption performance is more stable.

4.5. Correlation between Different Parameters and Application Performance

The correlation between the application performance of KWHC and the oil, salt, pH,
and solid-liquid ratio was determined by Pearson correlational analysis. The salt did not
significantly affect the sorption of KWHC, but it decreased the HHV values. However,
the S value of KWHC with high salt content is still more than 2 × 10−7 , which still has
good combustion applicability. Oil negatively impacts the HHV and adsorptive properties
of KWHC, but according to actual experimental data, it has a limited inhibitory effect on
application performance. The adsorptive capacity and S value are almost at the same level.
The HTC can control the negative impact of oil content. The correlation analysis indicated
that the pH of the water in the HTC process was positively correlated with adsorption
and HHV. Increased water content has no direct effect on the adsorptivity of KWHC and
increases the HHV (p > 0.05) (Figure 7).
Toxics 2023, 11, 679 15 of 19

Figure 6. PFO and PSO adsorption models of KWHC: (a,e) represent salt KWHC in PFO and PSO
models, (b,f) represent oil KWHC in PFO and PSO models, (c,g) represent pH KWHC in PFO and
PSO models, and (d,h) represent solid-liquid-ratio KWHC in PFO and PSO models.

This explored the negative effects of oil salts in KW that HTC can reliably treat, while
the application performance of the hydrothermal derivative of KW also does not show
obvious limitations on the hydrothermal parameters (pH and moisture). The inclusiveness
− −
of the HTC process for raw materials and) production process parameters is described.
Toxics 2023, 11, 679 16 of 19

Table 5. PFO and PSO model parameters.

Pseudo-First-Order Pseudo-Second-Order
Treatment Qmax (mg/g)
K1 (h−1 ) R2 K2 (h−1 ) R2
S1 4.92 0.02 0.84 2.28 0.91
S2 5.55 0.02 0.95 0.00 0.87
S3 6.59 0.02 0.85 3.35 0.90
S4 8.78 0.02 0.98 2.90 0.78
O1 12.41 0.06 0.84 0.00 1.00
O2 9.93 0.04 0.93 0.00 0.99
O3 9.80 0.06 0.90 7.96 1.00
O4 6.83 0.02 0.98 0.00 0.95
P1 11.24 0.05 0.77 0.00 0.99
P2 10.88 0.04 0.07 0.00 0.99
P3 8.92 0.03 0.95 0.00 0.98
P4 6.86 0.04 0.93 0.00 0.99
R1 16.90 0.11 0.59 7.85 1.00
R2 (CK) 18.35 0.11 0.68 3.83 1.00
R3 15.99 0.09 0.67 7.65 1.00
R4 11.22 0.06 0.84 8.66 1.00

Figure 7. Correlation between treatment parameters and application performance: (a) the correlation
between salt oil content and KWHC production, Cd (II) adsorption, and HHV value; and (b) the
correlation between pH and solid liquid ratio and KWHC production, Cd (II) adsorption, and
HHV value.
ff
Toxics 2023, 11, 679 17 of 19

5. Conclusions
This study explored whether the high salt content does not inhibit the Cd (II) adsorp-
tion performance of KWHC. The oil content slightly inhibits the Cd (II) adsorption and
calorific value of KWHC. The water content has a reduced hydrochar yield compared to
the oil, salt, and pH. In addition, the combustion characteristics of KWHC have more stable
combustible properties under alkaline conditions. All KWHC treatments were more suit-
able for combustion after HTC treatment (S values over 2 × 10−7 ). Based on experimental
results, it could be speculated that the KWHC can maintain the stability of application
performance when the self-reaction mechanism changes the pH. Furthermore, HTC is
highly inclusive of raw materials and process parameters because it removed the step
of screening sources and special treatment, which expands the feasibility of large-scale
industrial production of hydrochar from KW in the future. Based on the findings from this
study, it is concluded that the HTC is more suitable and efficient for treating and utilizing
KW, thereby achieving a safer and more environmentally friendly disposal method during
a national crisis.

Author Contributions: Investigation, methodology, writing—original draft, X.S.; investigation, J.H.;

visualization, writing—review and editing, M.A.K.; writing—review and editing, K.C.; data curation
and editing, Y.L.; data curation, editing, and polishing, G.G.; editing and polishing, X.L.; editing and
polishing, F.J.; editing and polishing, M.K.; editing and polishing, S.G.; conceptualization, funding
acquisition, supervision, and project administration, Q.H. All authors have read and agreed to the
published version of the manuscript.
Funding: This study was supported by the Hainan Provincial Natural Science Foundation of China
(423RC430; YSPTZX202205; 421RC669; and 422RC601), the Hainan Province Science and Technology
Special Fund (ZDYF2022SHthe2), the Education Department of Hainan Province (Hnjgzc2022-3), the
National Nature Science Foundation of China (41571288), the Research Initiation Fund of Hainan
University (KYQD(ZR)20032), and supported by the specific research fund of Academician He Hong’s
team Innovation Platform for Academicians of Hainan Province.
Data Availability Statement: Data will be made available on request.
Conflicts of Interest: The authors declare no conflict of interest.

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