Journal of Environmental Management 362 (2024) 121340

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Journal of Environmental Management

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

Research article

Synergistic effects of Co-pyrolysis on the immobilization and

transformation of lead (Pb), chromium (Cr), nickel (Ni), and fluorine (F) in
phosphogypsum-biomass mixtures
Minjie He a, b, Rui Xu a, b, Guangfei Qu a, b, *, Xianyu Fu a, b, Xinxin Liu a, b, Hanghang Wang a, b,
Yaxin Tian a, b, Chenyang Yin a, b
a
Faculty of Environmental Science and Engineering, Kunming University of Science and Technology, Yunnan, Kunming, 650500, China
b
National-Regional Engineering Research Center for Recovery of Waste Gases from Metallurgical and Chemical Industries, Kunming, 650500, Yunnan, China

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

Keywords: Co-pyrolysis of biomass with phosphogypsum (PG) presents an effective strategy for facilitating the recycling of
Phosphogypsum PG resources. However, it is crucial to note the environmental threats arising from the presence of Pb, Cr, Ni, and
Biomass F in PG. This study investigated the effect of immobilization and transformation of four elements during co-
Co-pyrolysis
pyrolysis with biomass and its components. The co-pyrolysis experiments were carried out in a tube furnace
Hazardous elements
Immobilization and conversion
with a mixture of PG and corn stover (CS), cellulose (C), lignin (L), glucose (G). Co-pyrolysis occurred at varying
temperatures (600 ◦ C, 700 ◦ C, 800 ◦ C, and 900 ◦ C) and different addition ratios (10%, 15%, and 20%). The
results indicated that an increase in co-pyrolysis temperature was more conducive to the immobilization and
transformation of harmful elements in PG, demonstrating significant efficacy in controlling F. Additionally, the
addition of biomass components exerts a significant impact on inhibiting product toxicity, with small molecules
such as glucose playing a prominent role in this process. The mechanism underlying the control of harmful el­
ements during co-pyrolysis of PG and biomass was characterized by three main aspects. Firstly, biomass com­
ponents have the potential to melt-encapsulate the harmful elements in PG, leading to precipitation. Secondly,
the pyrolysis gas produced during the co-pyrolysis process contributes to the formation of a rich pore structure in
the product. Finally, this process aids in transforming hazardous substances into less harmful forms and stabi­
lizing these elements. The findings of this study are instrumental in optimizing the biomass and PG blend to
mitigate the environmental impact of their co-pyrolysis products.

1. Introduction Canada, and Italy, policy support the recycling of PG by enabling pro­
ducers or certified treatment firms. They can process and recycle PG
Phosphogypsum (PG) is a significant by-product of the wet phos­ according to local standards. In China, governmental laws and regula­
phoric acid production process, with every ton of phosphoric acid tions have been established to tackle the issue of long-standing PG
yielding approximately 4.5 tons of PG (QIAN et al., 2024). Currently, the stockpiles. These regulations explicitly stipulate that companies must
global accumulation of PG has soared to 6 billion tons, increasing refrain from constructing new PG stockpiles, avoid excessive accumu­
annually at a rate of 100–280 million tons. However, worldwide, less lation, and risk closure if stockpile limits are exceeded (BOUNAGA et al.,
than 25% of PG was utilized (WANG and DONG, 2024). This low utili­ 2022).
zation rate is predominantly due to the elemental composition of PG and The feasibility of reusing PG largely hinges on its chemical compo­
various regulatory policies. For instance, in countries like the United sition. In countries endorsing PG reuse, radioactive elements in PG are
States and Belgium, local governments outrightly prohibit PG use due to minimal, posing negligible environmental and human health risks.
its high radioactive element content (STIDHAM et al., 2014). However, However, in the wet process of phosphoric acid production, phosphate
in nations such as Morocco and Netherlands, PG was often discharged ore reacts with sulfuric acid, yielding phosphoric acid and PG. The heavy
into the sea (CHOUAYBI et al., 2023). Conversely, in nations like China, metals present in the raw materials do not integrate with the phosphoric

* Corresponding author.
E-mail address: qgflab@sina.com (G. Qu).

https://doi.org/10.1016/j.jenvman.2024.121340
Received 23 February 2024; Received in revised form 21 April 2024; Accepted 30 May 2024
Available online 1 June 2024
0301-4797/© 2024 Elsevier Ltd. All rights are reserved, including those for text and data mining, AI training, and similar technologies.
M. He et al. Journal of Environmental Management 362 (2024) 121340

acid but instead accumulate in the by-product. Consequently, PG serves 2. Materials and methods
as a repository and distribution center for these heavy metals (KOUZ­
BOUR et al., 2019). Heavy elements (Pb, Cr, Ni and F) constitute a 2.1. Raw materials
significant barrier to its reuse (CHEN and GRAEDEL, 2015). To address
these challenges, researchers have focused on the solidification and The PG utilized in this study was collected from a PG yard in Yunnan,
transformation of hazardous elements. This involves solidifying toxic China, and had been in storage for a duration of three years. Table 1
substances through the formation of insoluble compounds, adsorption, delineates selected properties of the PG leach solution, while Fig. 1 il­
and encapsulation. These techniques frequently employed in con­ lustrates the morphology of four key elements - Pb, Cr, Ni, and F - within
structing materials and road bases (AHMAD et al., 2024). For instance, the PG. CS, used in the experiments, was sourced from the mechanized
gelling materials or alkaline activators can effectively inhibit the cultivation experimental base at the College of Agricultural Engineering,
leaching of toxic substances from PG. Ren et al. (REN et al., 2023) Kunming University of Science and Technology. Analytical grade cel­
developed a PG slag-based gelling material that enabled Cd in PG to lulose (CAS: 9004-34-6), lignin (CAS: 9005-53-2), and glucose (CAS:
interact with sulfoaluminate and silicate, leading to its replacement by 14,431-43-7) were procured from Tianjin Zhiyuan Chemical Reagent
Ca or Cd(OH) in C–S–H, thus entirely suppressing Cd’s leaching toxicity. Co. Ultrapure water with a resistivity exceeding 18.2 MΩ/cm was used
Shi (SHI et al., 2023) and colleagues employed CaCO3 as a pretreatment for all experimental procedures. Information on the reagents used for
agent for PG, producing mine backfill material. This approach generated fugitive morphology extraction is presented in Table s1 of the Sup­
Ca2+ ions, which reacted with F in a liquid phase, achieving a 99% porting Materials.
fixation of F. Furthermore, numerous researchers have been exploring
methods to alter the form of heavy metals and F in PG, aiming for 2.2. Samples preparation
environmentally sustainable treatment. Bouargane (BOUARGANE et al.,
2023) and colleagues treated PG with various carbonate media, trans­ 2.2.1. Experimental materials and setup construction
forming the harmful elements into more stable, carbonate-bound state. PG and CS were independently crushed and processed using a
These two approaches are currently among the most effective for the crusher. Subsequently, the crushed materials were sieved through a 200-
innocuous treatment of PG. However, given the significant challenge of mesh stainless steel mesh for subsequent use. Fig. 2 illustrates the
vast global PG stockpiles, meeting the demand for large-scale con­ schematic representation of the experimental setup. The co-pyrolysis
sumption of PG through conventional methods, like building material reaction was conducted in a tube furnace (BTF-1200C, Anhui Beckett
production or roadbed raw material preparation, proves challenging. Equipment Technology Co., Ltd.), to which a nitrogen cylinder was
Consequently, a novel method involving the co-pyrolysis of PG with attached. Nitrogen (N2) was uniformly introduced into the furnace at a
biomass for soil conditioner production has been proposed. During the flow rate of 200 ml/min. The prepared experimental samples were
co-pyrolysis process, biomass reacts with the harmful substances in PG placed inside a quartz box, situated at the center of the quartz tube. This
to form precipitates, thereby effectively mitigating the toxicity of these tube was connected to a lye absorption tank, positioned at its end, for the
substances (JIANG et al., 2022). This co-prolysis approach yields a purification of exhaust gases.
high-quality carbon-based soil amendment, enhancing agricultural
production while mitigating PG’s environmental risks. Vineet Vimal 2.2.2. Co-pyrolysis product preparation
(VIMAL et al., 2022) and colleagues utilized banana peduncle for The additives –CS, C, L, and G – were combined with PG in a 1:4 wt
co-pyrolysis with PG, producing a material that not only fully inhibited ratio. This mixture was homogenized to prepare four distinct sample 1
leaching toxicity but was also enriched in P and K, thereby offering an (HUANG et al., 2024). Experimental Sample 1 underwent co-pyrolysis at
innovative approach to PG utilization. The incorporation of biomass in various temperatures (600 ◦ C, 700 ◦ C, 800 ◦ C, and 900 ◦ C), each for a
the co-pyrolysis process significantly contributes to the environmentally duration of 1 h, to examine the impact of differing temperature gradients
responsible treatment of PG. Biomass primarily comprises cellulose, on the characteristics of the co-pyrolysis products (ZENG et al., 2024).
hemicellulose, and lignin (ZONG et al., 2020). Additionally, the The four additives were amalgamated with PG in proportions of 10%,
co-pyrolysis process involves the cleavage of large molecules into 15%, and 20% (wt%) respectively. Subsequently, these mixtures were
smaller ones (CAI et al., 2023). However, the precise roles and mecha­ subjected to co-pyrolysis at 900 ◦ C for 1 h to evaluate the influence of
nisms of these substances in the co-pyrolysis process warrant further varying additive ratios on the properties of the resultant products.
in-depth investigation.
To explore the impact of biomass components and the substances 2.3. Test methods and characterization
produced during pyrolysis on the immobilization and transformation of
Pb, Cr, Ni, and F in PG, this study will employ four distinct sub­ 2.3.1. Test methods
stances—corn stover (CS), cellulose (C), lignin (L), and glucose (G)—as Following the guidelines of the "Solid Waste Leaching Toxicity
additives. Initially, the leaching toxicity of the co-pyrolysis products at Leaching Method Horizontal Shock Method" (HJ 557–2010) of China,
varying temperatures (600 ◦ C, 700 ◦ C, 800 ◦ C, and 900 ◦ C) and the the solids products from the reaction processes in all experiments were
morphology of these elements will be examined (ZHU et al., 2024a). subjected to leaching using deionized water, maintaining a liquid-to-
This will be followed by an investigation into the leaching toxicity and solid ratio of 10:1. The mixture was agitated for 8 h at 25 ◦ C(water-
elemental composition of the products at different biomass addition bath thermostatic shaker, model SH2-82A, purchased from Changzhou
levels (10%, 15%, and 20%) (CHAI et al., 2022). Additionally, the Longyue Instrument Manufacturing Co). Subsequently, letting stand
microscale physicochemical properties of the products will be analyzed fora 16-h period, the mixture was filtered using a 0.45 μm filter mem­
using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), brane. The filtrate was then analyzed using an atomic absorption spec­
and Fourier-Transform Infrared Spectroscopy (FTIR). A series of assays trophotometer (Model AA-7020, purchased from Beijing East-West
are planned to elucidate the mechanisms by which various biomass Analytical Instruments Co.) to determine the leaching concentration of
components affect the transformation of Pb, Cr, Ni, and F during the
pyrolysis. The findings are expected to inform the optimization of Table 1
biomass and PG co-pyrolysis processes, aiming for the environmentally Physical and chemical properties of PG leachate.
benign treatment of PG.
Norm pH Conductivity Pb Cr Ni F

Value 3.89 2.39 ms/cm 1.7 mg/ 1.45 mg/ 0.36 mg/ 1.207 mg/
L L L L

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M. He et al. Journal of Environmental Management 362 (2024) 121340

rate of 2◦ /min over a 2-theta range of 5◦ –90◦ , with a step-length of

0.02◦ . The microstructural characterization of the solid samples was
conducted using scanning electron microscopy (SEM), specifically the
ZEISS Gemini 300 and OXFORD Xplore systems, with a gold-spraying
target composed of a gold–palladium alloy. The characteristic vibra­
tion bands of the solid samples were identified using Fourier transform
infrared spectrometry (FTIR, Japan). The FTIR spectra were recorded on
a Nicolet 5700 spectrometer, utilizing the KBr pellet technique at a
resolution of 4 cm-1. Subsequently, the samples underwent 20 scans in
the spectral range of 400–4000 cm− 1.

2.4. Statistical analysis

Data compilation and analysis were conducted utilizing Origin

software. The leaching toxicity inhibition efficiency metric (S) was
employed to quantify the extent of inhibition exerted by various co-
pyrolysis conditions on the leaching toxicity of the four elements. The
S index was computed in accordance with Equation (1). Here, ’Ud’ de­
notes the final concentration, while ’Ic’ represents the initial concen­
tration. A higher value of S indicates a more pronounced inhibition
Fig. 1. Occurrence morphological distribution of Pb, Cr, Ni and F in PG. effect on the harmful elements under the given conditions.
( )
Ud
heavy metals (WU et al., 2022a). The pH value of the leaching solution S(%) = 1 − × 100% (1)
Ic
was ascertained using an ion meter (model PXSJ-216F, Shanghai Lei Ci
Co., Ltd.). Prior to measurement, the pH meter was calibrated with a
3. Results and discussion
standard pH calibration solution. Following calibration, the pH elec­
trode was immersed in the filtrate and the reading was taken
3.1. Leaching toxicity of products
post-stabilization. The concentration of F ions was determined via anion
chromatography (Ion Chromatography, Model IC1800, Sunny Hengping
3.1.1. Leaching toxicity at different co-pyrolysis temperatures
Co., Ltd.). The procedure for using the F ion electrode mirrored that of
To evaluate the environmental safety performance and physical
the pH electrode. The conductivity of the leaching solution was
properties of the co-pyrolysis products at varying temperatures, the
measured using a conductivity meter (DDS-307A, Shanghai Shengke
leachates were subjected to testing. As depicted in Fig. 3a–a consistent
Instrument Co., Ltd.). The SMT extraction method was employed for
rise in the pH of CS is observed with increasing temperature. Conversely,
detecting elemental fugitive morphology (WU et al., 2022b). The spe­
C and L exhibit an initial increase followed by a decrease in pH, whereas
cific extraction process is demonstrated in the supplementary material.
G maintains a relatively stable pH. The impact of adding individual
components significantly differs from that of adding complete CS. It can
2.3.2. Characterization of production
be inferred that the alkalization phenomenon observed is influenced not
The solid samples underwent drying at 45 ± 5 ◦ C, following which
only by the co-pyrolysis temperature but also by other related factors
alterations in their crystal structures were assessed using X-ray diffrac­
(Zhu et al., 2024). Additionally, this phenomenon might result from the
tometry (XRD, Physics Ultima IV), employing a Cu Kα radiation scan at a
interaction between biomass components and PG during co-pyrolysis

Fig. 2. Scheme for building the experimental setup.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

Fig. 3. Physical properties of product leachate at different co-pyrolysis temperatures (a) pH (b) Conductivity.

(YANG et al., 2024). Fig. 3b illustrates the variations in conductivity at the co-pyrolysis products.
different temperatures. At 700 ◦ C, C and G exhibit a marked peak in Fig. 4 clearly demonstrates that all four additives significantly
conductivity, suggesting that pyrolysis at this temperature results in the mitigated the risk of hazardous substance leaching in PG. As depicted in
maximum ion production for these substances (BARTOLI et al., 2022). Fig. 4a, both CS and G played a substantial role in diminishing the Pb
Conversely, CS and L display a steady decrease in conductivity, indi­ concentration as the temperature increased. Under C, there was a
cating that the ions within the reactants gradually stabilize as the tem­ gradual increase in Pb concentration, whereas L exhibited an initial
perature increases, aided by these additives, with higher temperatures increase followed by a decrease, peaking notably at 800 ◦ C. This phe­
facilitating this stabilization (LI et al., 2022). Furthermore, it can be nomenon could be attributed to environmental alterations, such as pH
speculated that L plays a pivotal role in stabilizing the ionic state within changes, induced by pyrolysis at this temperature, which facilitate the

Fig. 4. Leaching concentration of products at different co-pyrolysis temperatures (a) Pb (b) Cr (c) Ni (d) F.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

release of Pb (WANG et al., 2024). Additionally, the formation of spe­ As evidenced in Fig. 5a, the addition of CS and L demonstrates a
cific compounds at this temperature may augment the solubilization of positive correlation with pH levels, whereas the addition of G exhibits a
Pb or modify its partitioning pattern, thereby simplifying its leaching negative correlation, marked by a trend of initial decrease followed by
process (AL-HARAHSHEH et al., 2022). According to Fig. 8a, the S-index an increase. This implies that an increased presence of biomass com­
of G for Pb, Cr, and F exceeds 90% and approaches 100%, indicating a ponents is likely to confer alkaline properties to the co-pyrolysis prod­
high efficiency. This suggests that small organic molecules, such as ucts. Although small molecular entities, either inherent in the biomass
glucose, generated during co-pyrolysis are advantageous for the or produced during co-pyrolysis, tend to react with PG to yield acids, but
immobilization of harmful elements (WANG et al., 2023a). Fig. 4b the influence of these reactions is relatively mild (GHESTI et al., 2022).
shows that the Cr concentration in the leachate of co-pyrolysis products, According to the results shown in Fig. 5b, the conductivity of the
with the addition of L and G, remained stable across varying tempera­ co-pyrolysis products comprising C and G did not exhibit significant
tures, with G exhibiting complete inhibition of Cr leaching toxicity. variations across different additive levels. The conductivity of
Conversely, the addition of C led to an escalation in the leaching con­ co-pyrolysis products augmented with CS displayed a slight uptick
centration of Cr with rising temperatures. Fig. 4c illustrates that the correlating with increased additive quantities. Conversely, the addition
inhibition of Ni leaching toxicity by all four components intensified as of L resulted in a marked decrease in conductivity as the quantity of the
the temperature rose, with CS and G exhibiting parallel trends. This may additive increased, suggesting that L plays a significant role in stabiliz­
be due to the fact that the small molecule-like substances generated by ing the ions present in PG (MESKINI et al., 2021). This observation
biomass cracking at higher temperatures promote the morphological aligns with the findings presented in Fig. 3b.
transformation of Ni, which leads to its easier precipitation (BOUSSAFIR The data presented in Fig. 6 indicate that escalating the addition of
et al., 1995). The results depicted in Fig. 4d indicate a gradual decrease CS effectively inhibits the leaching concentration of Pb and Cr, while its
in the concentration of F in the products with the addition of C, L, and G, impact on Ni and F is less pronounced. This can be attributed to the
correlating with an increase in temperature. However, the leaching physical encapsulation phenomenon observed during the co-pyrolysis
concentration of F in the products with added CS exhibited an initial process (KONAROVA et al., 2024). Ni and F are encapsulated during
increase followed by a decrease as the temperature rise. This phenom­ the addition of small amounts of biomass, but diminished effectiveness
enon could be attributed to the decomposition of fluoride precipitates at with larger additions. This theory similarly applies to the varying effects
approximately 700 ◦ C, which facilitates the leaching of F. As tempera­ of L and G additions on Ni. As observed in Fig. 6b, the leaching con­
tures continued to rise, the fluoride in the samples vaporized and tran­ centration of Ni is increased with the increase of C addition, while
sitioned into the gas phase (MOUHOVSKI, 2007). This effect became modifications in the addition of other biomass components do not. An
more pronounced at higher temperatures. increase in G addition contributes significantly to the inhibition of Pb
Additionally, corroborating with data from Fig. 7a, it is evident that leaching concentration, yet exhibits a lesser effect on Cr, Ni, and F. This
the leaching inhibition efficiencies of the four components on F in the indicates that 10% of G can realize the toxicity control of Cr, Ni and F in
product exceeded 90%. This observation suggests that F in PG is more the products. Fig. 6d demonstrates that the increased additions of C and
prone to reacting with organic matter at elevated temperatures, leading L contributed to the control of F leaching toxicity. This could be
to the formation of precipitates (DANOUCHE et al., 2023). In summary, attributed to these macromolecules’ propensity to enrich F escaping
the inhibition efficacy for Pb and Cr during the co-pyrolysis process from PG during high-temperature processes and subsequently form
across various temperature gradients can be ranked as follows: G > CS > stable precipitates on their surfaces (SHEN et al., 2020). However, the
C > L. The inhibition effectiveness for Ni and F follows the order of CS > variations in the S-index depicted in Fig. 7b indicate that increasing CS
C > L > G and G > C > L > CS, respectively. The results indicate that addition significantly enhances the inhibition efficiency of Pb and Cr
biomass is particularly effective in mitigating the leaching toxicity of Pb, leaching toxicity, with a similar improvement noted for lead toxicity
Cr, Ni, and F. Especially the small molecular entities are more likely to upon increasing G addition. The escalation in the addition of other
engage in reactions with deleterious components of PG, leading to the components exhibited a less pronounced effect on their leaching toxicity
formation of precipitates or inducing morphological transformations. inhibition efficiency. In summary, alterations in the addition levels of
the four biomass components had a more significant impact on Pb,
3.1.2. Leaching toxicity at different addition levels whereas Cr, Ni, and F were either minimally affected or exhi bited
Investigating the impact of varying additive dosages on the leaching fluctuations within a narrow range.
toxicity of co-pyrolysis products not only enhance our comprehension of
the distinct components’ effects on the co-pyrolysis process but also aid
in devising a more logical and cost-effective processing strategy.

Fig. 5. Physical properties of the product leachate at different biomass fraction additions, (a) pH (b) Conductivity.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

Fig. 6. Leaching toxicity of products at different biomass fraction additions (a) Pb (b) Cr (c) Ni (d) F.

Fig. 7. S Index (a) different temperatures (b) different additions.

3.2. Distribution of combined forms (1) Residual State (RT): Typically denotes the most stable binding
form, resistant to release via conventional biological and chem­
Heavy metals in natural environments exist in five distinct forms, ical processes.
differentiated by their interactions and chemical combinations with (2) Organic Matter-bound State (OT): This state involves metals
other elements in the vicinity (DEBNATH et al., 2024). forming complexes with organic matter, ranking second in sta­
bility following the residual state.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

(3) Ferromanganese Oxide Bound State (FMOT): Here, heavy metals (3) Ferromanganese Oxide Bound Fluorine (FMTF): Fluorine in this
are bound to iron and manganese oxides. This state is typically form is bound to ferromanganese oxides and generally remains
stable under oxidizing conditions but may release metals under stable in oxidizing environments, yet may be released under
reducing environments. reducing or acidifying conditions.
(4) Carbonate Bound State (CT): In this state, metal ions combine (4) Exchangeable Fluorine (ETF): This form is adsorbed onto soil
with carbonate minerals, resulting in a stable mineral particle surfaces and is readily exchangeable via ion exchange. It
configuration. represents a more reactive form, capable of being absorbed by
(5) Exchangeable State (ET): This represents the most unstable form, plants or migrating with water flow.
where heavy metal ions are adsorbed onto soil particle surfaces, (5) Water Soluble Fluorine (WTF): Present as dissolved ions in water,
readily exchanged and released, thus posing significant envi­ this form is the most readily transportable and absorbable by
ronmental and biological risks. organisms, exerting significant influence on aquatic ecosystems.

The categorization of fluorine forms in the environment is primarily

based on the nature of its combination with other substances and sta­ 3.2.1. Distribution of Pb, Cr, Ni and F in different co-pyrolysis temperatures
bility, delineating into these five types (FU et al., 2022). This study aimed to elucidate the alterations in elemental forms of
various biomass fractions across different temperatures by investigating
(1) Residual State Fluorine (RTF): This form is tightly integrated into the distribution of combined forms in pyrolysis products. Results from
mineral structures, representing the most stable form of envi­ Fig. 8a reveals that both the high-temperature pyrolysis environment
ronmental fluorine, resistant to removal by environmental pro­ and the addition of the four biomass fractions significantly influenced
cesses, such as acid washing. the transformation of combined forms of elemental Pb. The ET content
(2) Organic Matter-bound Fluorine (OTF): This type binds to organic exhibited a marked decrease from 32% in the raw PG material, indi­
matter, including fluorine within soil organic content. It is rela­ cating a substantial conversion of ET into FMOT and CT. The addition of
tively stable but may be released during the decomposition of C was found to be particularly conducive to the formation of RT, and the
organic matter. residual Pb will not be destroyed by temperature rise. Conversely, the
addition of L solely facilitated the conversion of other combined forms of

Fig. 8. Distribution of combined forms at different co-pyrolysis temperatures (a) Pb (b) Cr (c) Ni (d) F.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

Pb to RT at lower temperatures. This could be attributed to the residual Additionally, the inclusion of biomass components also led to an
state of Pb induced by L lacking thermal stability, rendering it prone to elevation in the content of exchangeable state Ni, potentially due to the
decomposition at elevated temperatures (TIAN et al., 2023). The find­ absence of adequate confined space in the surface layer of the PG within
ings from Fig. 8b indicate that Cr in the product predominantly exists in the reaction system, thus facilitating the formation of exchangeable state
the ET. This phenomenon was consistent across all four biomass frac­ Ni (YAO et al., 2023). Therefore, strategizing the control of the reaction
tions added, with ET content surpassing 50% and reaching as high as system involving PG and biomass components to enhance the binding of
70%, signifying an enhancement of 30%–50% relative to the original ET feedstock is imperative for more effective management of harmful ele­
content in PG. The occurrence of this phenomenon is likely linked to the ments during the co-pyrolysis process. The results depicted in Fig. 8d
production of organic acids during biomass pyrolysis. As biomass de­ suggest that the transformation of the combined forms of F is predom­
composes, it generates low molecular weight organic acids, including inantly temperature-dependent. As the co-pyrolysis temperature
acetic and formic acids (QIU et al., 2023). These acids can react with increased, the RTF content in the products, following the addition of the
heavy metal ions to form soluble metal-organic complexes, thereby four biomass fractions, exhibited a significant upward trend, reaching as
facilitating the presence of chromium in an exchangeable state. This high as 95%. Consequently, it can be inferred that high-temperature
observation suggests that co-pyrolyzing PG with biomass fractions conditions significantly contribute to the stabilization of F in PG. In
promotes the transformation of the Cr form into the ET. The promotion summary, a high-temperature environment plays a crucial role in the
effect of G on this transformation was the most pronounced, exhibiting a transformation of the combined forms of F, with the contributions of the
progressive increase with escalating temperatures. Fig. 8c demonstrates four biomass components to the transformation of the fugitive form of
that the addition of various biomass fractions is conducive to the for­ Pb being in the order of CS > G > L > C, and for Ni, the order is G > L >
mation of RT Ni, with a notable increase in RT Ni observed under the C > CS. However, the addition of biomass components does not signif­
addition of all four biomass fractions, surpassing the original 17% icantly control the transformation of the combined forms of Cr, which
content in PG. The addition of G was particularly impactful in this may result in the precipitation of Cr during the use of the product.
conversion, with the RT Ni content reaching up to 62%. This phenom­
enon could be attributed to the propensity of small molecules to react 3.2.2. Distribution of Pb, Cr, Ni and F in different biomass fraction
with Ni under high temperature conditions, facilitating the conversion additions
of Ni back to its original mineral form (WANG et al., 2023b). Investigating the impact of varying biomass component additions on

Fig. 9. Distribution of combined forms with different biomass fraction additions (a) Pb (b) Cr (c) Ni (d) F.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

the transformation of hazardous elements in PG into combined forms 3.3. Characterization

will facilitate enhanced control over the process conditions. Analysis of
Fig. 9a indicates that with the augmented addition of biomass fractions, 3.3.1. SEM analysis
there was a noticeable elevation in the FMOT of Pb in the products of all High-temperature pyrolysis involving biomass components and PG
four experimental groups, while the OT was reduced. This implies that significantly alters the surface morphology of PG. Fig. 10 depicts the
increasing the additive dosage fosters the transition of Pb from a rela­ microscopic morphology of the co-pyrolysis products of four composi­
tively stable state to a more unstable state (KEGL et al., 2021). This tions - CS, C, L, and G - with PG, each at a 20% addition and a co-
phenomenon could be attributed to the influence of pyrolysis oil/gas, pyrolysis temperature of 900 ◦ C. As observed in Fig. 10a, the surface
generated by biomass components during pyrolysis, on the reaction of PG is characterized by numerous granular materials with smooth
system (CHATURVEDI et al., 2024). The data in Fig. 9b show that the textures. This implies that the complex biomass components and heavy
addition of CS, C and G does not have a large effect on the Cr combined metal elements on the PG surface are prone to melt-encapsulation at
forms. However, the increase of L addition will facilitate the conversion high temperatures, resulting in granular precipitates that adhere to the
of the ET Cr to RT and OT, which indicates that L can play a more PG surface (ZHU et al., 2024b). The lower left corner of the image il­
important role in the stabilization of Cr in PG. The addition of the four lustrates that the more irregular the shape of PG, the higher the likeli­
biomass types exerted a minimal effect on the transformation of the hood of granular precipitate formation on its surface. Consequently, the
combined forms of Ni, as corroborated by the results in Fig. 9c. Fig. 9d extent of PG fragmentation is directly correlated with the efficacy of
reveals a distinct correlation between the change in the combined forms co-pyrolysis in toxicity inhibition. Fig. 10b reveals that the addition of C
of F and the quantity of added biomass components. An increase in the also results in a melt-wrap phenomenon on the surface of PG. Notably,
addition of biomass components will favor the conversion process of F due to the addition of pure cellulose, the precipitated particles on the PG
from ET to the RT. In summary, the quantity of added biomass compo­ surface are smaller and more densely packed. Fig. 10c displays the
nents significantly influences the transformation of the combined forms co-pyrolysis product with L addition, which significantly differs from the
of Pb and F, while exerting a lesser impact on Cr and Ni. Moreover, the effects observed with CS and C. The incorporation of pure L facilitates
extent of biomass addition is negatively correlated with the sta bilization the formation of internal pores in PG, likely attributable to the sub­
degree of Pb and positively correlated with that of F. stantial volume of pyrolysis gases generated from the reaction of PG
with L under high-temperature conditions, resulting in a rich pore
structure (MA et al., 2022). As evidenced by the microscopic
morphology in Fig. 10d, the addition of G resulted in an abundance of

Fig. 10. SEM characterization diagram (a) CS (b) C (c) L (d) G.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

needle-like structures on the PG surface. This indicates that crystal impurities in PG, leading to the formation of stable precipitates, and also
growth may have transpired due to the co-pyrolysis of G with surface promotes internal reactions of these impurities to produce precipitates
impurities on PG, with a fraction of these impurities being encapsulated (GU et al., 2023). Pb was detected in the products with C addition, and
in the process, thereby mitigating the leaching toxicity of the product its presence became more pronounced with increasing temperature,
(KHAN et al., 2024). corroborating the findings of Fig. 4a. Contrary to the CS group, F readily
reacts with Zn in PG in the presence of C to form ZnF2. The data in
3.3.2. XRD analysis Fig. 11b reveal that with L addition, the number of crystals containing
To substantiate the principle of inhibiting harmful components in PG Pb, Cr, and Ni escalates as temperature rises, although this trend is not
through co-pyrolysis, XRD analysis of the products was conducted at reflected in the leaching toxicity assay. It can be inferred that under L
varying temperatures and with different biomass additions. Fig. 11 re­ addition, harmful elements in the high-temperature pyrolysis products
veals that calcium sulfate (CaSO4) and silicon dioxide (SiO2) are present are capable of forming a stable precipitated state at lower pyrolysis
on the surface of almost all products, indicating that these two com­ temperatures, a conclusion corroborated by Fig. 9. The crystal compo­
pounds form the basic structure of the products. However, Fig. 11d sition becomes increasingly homogeneous with the addition of G as the
shows that in the L-20% curve, the presence of CaSO4 and SiO2 is not temperature rises. Figs. 11c and d demonstrate that an increase in the
detected, suggesting an anomaly in this particular composition. Coupled addition of raw components reduces the detection of CaSO4 and SiO2,
with the SEM characterization results from Fig. 10, the extensive melt- the inherent components of PG. This suggests that augmented addition
encapsulation post-precipitation produced by substantial L addition favors the generation of more precipitates on the PG surface, thereby
during co-pyrolysis with PG may result in uniform encapsulation of the encapsulating its original components internally.
PG particles, thereby rendering them more stable (CHEN et al., 2024).
According to the results presented in Fig. 11b, this phenomenon is 3.3.3. FTIR analysis
significantly influenced by the reaction temperature. Fig. 11a shows that FTIR analysis is instrumental in identifying the nature and intensity
the diversity of crystal compositions increases with rising temperature of reactions between PG and biomass within this system (SAMANTA and
following the addition of CS. The Ni and Cr crystals primarily exhibit a SRIVASTAVA, 2020). Fig. 12 illustrates that the infrared peaks for the
spinel phase morphology. This suggests that the high-temperature four biomass fractions are consistent across various temperatures and
environment facilitates reactions between biomass components and ratios. The peak at 3431 cm− 1 is indicative of the stretching vibration of

Fig. 11. XRD Characterization (a)CS and C at different temperature (b)L and G at different temperature (c)CS and C at different additive proportion (d)L and G at
different additive proportion.

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M. He et al. Journal of Environmental Management 362 (2024) 121340

Fig. 12. FTIR Characterization, (a)CS and C at different temperature (b)L and G at different temperature, (c)CS and C at different additive proportion (d)L and G at
different additive proportion.

the O–H bond, associated with moisture changes in the raw material summary, the temperature of co-pyrolysis is a decisive factor in the
during high-temperature pyrolysis (KRASNOSHCHEKOV et al., 2020). occurrence of various intrinsic reactions within the co-pyrolysis process.
The vibrational peak at 1151 cm− 1 potentially corresponds to the Conversely, the proportion of added biomass components exerts a
stretching vibration of the C–O–C bond, suggesting the generation of relatively minor influence on these reactions.
numerous polysaccharides during the pyrolysis of the biomass fraction
(W et al., 2023). The vibrational peak at 1119 cm− 1 aligns with the C–O
stretching vibration, indicating the formation of ether bonds or hydroxyl 3.4. Mechanism of inhibition of Pb,Cr,Ni and F release by biomass
groups in the course of co-pyrolysis (RAO et al., 2021). The vibrational fractions
peaks at 676 cm− 1, 613 cm− 1, and 594 cm− 1 are likely associated with
metal-ligand vibrations in metal complexes, suggesting specific re­ The co-pyrolysis of biomass fractions with PG has been shown to
actions of metal elements in PG with biomass components or other PG effectively mitigate the leaching toxicity of Pb, Cr, Ni, and F in PG, while
constituents at high temperatures (HALCROW, 2007). Analysis of the also facilitating the transformation of their combined forms. Fig. 13 il­
data from Figs. 12a and b reveals that none of the four additives exhibit lustrates the underlying mechanism of the immobilization and trans­
the vibrational peak at 1119 cm− 1 at 600 ◦ C. In conjunction with the formation processes of Pb, Cr, Ni, and F during the co-pyrolysis of PG
complexes identified in the XRD analysis, it can be concluded that higher with biomass. During pyrolysis, C (along with hemicellulose, which
temperatures are conducive to the formation of complexes, and biomass shares similar properties) and L within the biomass decompose into
components can generate stable complexes with PG constituents small molecules. These small molecules can effectively interact and
post-decomposition. The L-900 ◦ C curve in Fig. 12b shows multiple undergo chemical reactions with well-mixed PG at elevated tempera­
shocks in the lower wave number range, indicative of an increased tures, thereby promoting the immobilization and transformation of the
occurrence of heavy metal chelation/complexation reactions at higher four detrimental elements (LI et al., 2024).
temperatures in PG with added L (HATIMI et al., 2023). The findings The fixation and transformation process is facilitated via three pri­
from Fig. 12c indicates that the quantities of CS and C added exert a mary pathways. The first pathway involves the generation of pre­
minimal impact on the co-pyrolysis reaction. Conversely, Fig. 12d re­ cipitates. Organic groups such as -C-O-C- and -C-O- are formed through
veals that an increased addition ratio of L and G significantly diminishes high-temperature cleavage of biomass, enabling fusion-encapsulation
the intensity of chemical reactions within the co-pyrolysis system. In with harmful elements in PG. Complexation and chelation reactions
occur during this process, yielding stable precipitates. XRD analysis

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M. He et al. Journal of Environmental Management 362 (2024) 121340

Fig. 13. Inhibition mechanism of leaching toxicity of Pb, Cr,Ni and F under co-pyrolytic action.

results from Fig. 11 suggest that CS, with its complex composition, not temperatures (600 ◦ C, 700 ◦ C, 800 ◦ C, and 900 ◦ C) and different biomass
only enhances the diversity of species in these precipitates but also addition ratios (10%, 15%, and 20%) were systematically explored. It
substantially increases their total quantity. The second pathway involves was discovered that an increase in co-pyrolysis temperature enhances
the creation of an internal porous structure within the product. The PG the immobilization and conversion of harmful elements in PG, with
mixed with biomass components, upon undergoing pyrolysis, produces a notable efficacy in controlling F. Concurrently, the addition of biomass
substantial volume of pyrolysis gas. This, coupled with the melting- components significantly influences the reduction of product toxicity,
encapsulation phenomenon during co-pyrolysis, culminates in a solid with small molecules like glucose playing a prominent role in this pro­
porous structure of the product. This porous structure is expected to cess. The mechanism by which harmful elements are controlled during
enhance the enrichment of microorganisms during the agricultural the co-pyrolysis of PG and biomass is primarily manifested through three
application of the product (CUI et al., 2024). Additionally, SEM char­ distinct aspects. Firstly, biomass components have the capability to
acterization images in Fig. 10 reveal that L plays a significant role in this melt-encapsulate with harmful elements in PG, leading to their precip­
pathway. The third pathway entails the transformation of the storage itation. Secondly, the pyrolysis gas generated during the co-pyrolysis
form of harmful elements. The incorporation of biomass components process contributes to the formation of a rich porous structure within
facilitates the transformation of most elements into more stable forms the product. Finally, the co-pyrolysis process facilitates the trans­
(BI et al., 2022). This transformation process may occur in a single step, formation of the fugitive forms of hazardous substances into more stable
such as a direct transition from the exchangeable state to the residual compounds. The findings of this research enhance the understanding of
state. Alternatively, the transformation might be gradual, transitioning how mixed biomass-PG pyrolysis impacts the immobilization and
from the active state to a relatively stable carbonate-bound state. The transformation of hazardous elements in PG and aid in optimizing the
results presented in Fig. 8 confirm this mechanism. The contributions of process for effective leaching toxicity suppression.
the four biomass fractions to the transformation of the fugitive form of
Pb were in the order of CS > G > L > C, and for Ni, the order was G > L > Funding information
C > CS. However, the addition of biomass fractions was not effective in
controlling the transformation of the fugitive form of Cr. However, the Financial support for this project was provided by Application of
addition of biomass components did not play a good role in controlling Clean Value-added Processing Technology for Large Livestock and
the transformation of Cr. Moreover, the quantity of added biomass Poultry Farm Waste(202302AE090014)
components significantly influences the conversion of Pb, though it has a
lesser impact on Ni and Cr. Within the co-pyrolysis system, temperature CRediT authorship contribution statement
serves as a critical control factor. Elevated temperatures are more
favorable for the immobilization and transformation of harmful ele­ Minjie He: Data curation, Conceptualization. Rui Xu: Supervision,
ments in PG. The conclusion that leaching toxicity diminishes with Writing – review & editing. Guangfei Qu: Formal analysis, Conceptu­
increased temperature was effectively corroborated in the experiments alization. Xianyu Fu: Investigation, Formal analysis. Xinxin Liu: Proj­
involving various components. From the standpoint of controlling the ect administration, Investigation. Hanghang Wang: Visualization,
four elements, temperature was most efficacious in mitigating the Software. Yaxin Tian: Writing – original draft. Chenyang Yin: Writing
leaching toxicity of the F element. – review & editing.

4. Conclusion
Declaration of competing interest
This study investigates the inhibitory effects of various biomass
components on the leaching toxicity of Pb, Cr, Ni, and F during the co- The authors declare the following financial interests/personal re­
pyrolysis with PG. The properties of the co-pyrolysis products at varying lationships which may be considered as potential competing interests:
Guangfei Qu reports financial support was provided by Science and

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M. He et al. Journal of Environmental Management 362 (2024) 121340

Technology Department of Yunnan Province, China. Kunming Univer­ Ghesti, G.F., Silveira, E.A., GuimarãES, M.G., et al., 2022. Towards a sustainable waste-
to-energy pathway to pequi biomass residues: biochar, syngas, and biodiesel
sity of Science and Technology is the undertaking unit of the project.
analysis. Waste Manag. 143, 144–156.
Guangfei Qu reports a relationship with Kunming University of Science Gu, L., Guo, M., He, J., et al., 2023. Experimental study on hydrogen production
and Technology that includes: employment. Guangfei Qu has patent characteristics of kaolin supported Ni catalyzed by steam gasification of citrus peel.
pending to Guangfei Qu. None If there are other authors, they declare Fuel 340, 127431.
Halcrow, M.A., 2007. The spin-states and spin-transitions of mononuclear iron(II)
that they have no known competing financial interests or personal re­ complexes of nitrogen-donor ligands. Polyhedron 26 (14), 3523–3576.
lationships that could have appeared to influence the work reported in Hatimi, B., Loudiki, A., Mouldar, J., et al., 2023. Physicochemical and statistical
this paper. modeling of reactive Yellow 145 enhanced adsorption onto pyrrhotite Ash-Based
novel (Catechin-PG-Fe)-Complex. Materials Science for Energy Technologies 6,
65–76.
Data availability Huang, J., Su, B., Fei, X., et al., 2024. Enhanced microalgal biomass and lipid production
with simultaneous effective removal of Cd using algae-bacteria-activated carbon
consortium added with organic carbon source. Chemosphere 350, 141088.
Data will be made available on request. Jiang, S.-J., Sun, J., Tong, G., et al., 2022. Emerging disposal technologies of harmful
phytoextraction biomass (HPB) containing heavy metals: a review. Chemosphere
Acknowledgements 290, 133266.
Kegl, T., Kovač Kralj, A., Kegl, B., et al., 2021. Nanomaterials as fuel additives in diesel
engines: a review of current state, opportunities, and challenges. Prog. Energy
Financial support for this project was provided by Application of Combust. Sci. 83, 100897.
Clean Value-added Processing Technology for Large Livestock and Khan, M.S.J., Mohd, SIDEK L, Kamal, T., et al., 2024. Catalytic innovations: improving
wastewater treatment and hydrogen generation technologies. J. Environ. Manag.
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