Review

Recent Progress in Turning Waste into Catalysts for

Green Syntheses
Konstantin Wink * and Ingo Hartmann

Deutsches Biomasseforschungszentrum Gemeinnützige GmbH, Torgauer Straße 116, 04347 Leipzig, Germany;
[email protected]
* Correspondence: [email protected]

Abstract: The recycling of catalysts has emerged as a key solution to address environmental pollution
and the scarcity of natural resources. This dynamic is further reinforced by the growing industrial
demand for catalysts and the urgent need to transition to more sustainable production methods. In
the context of chemical transformations, the direct reuse of recycled catalysts for chemical applications
in particular represents an elegant route towards greener syntheses. In this article, we review recent
advancements in the recycling of homogeneous and heterogeneous catalysts since 2020, emphasizing
the utilization of waste-derived catalysts for chemical reactions. In particular, we consider three
primary sources of waste: electronic waste, spent lithium-ion batteries, and industrial wastewater.
For each of these waste streams, different extraction methods are explored for their effectiveness
in obtaining catalysts suitable for a broad spectrum of chemical reactions. These presented studies
emphasize the potential of recycled catalysts to contribute to a sustainable and waste-efficient future.

Keywords: waste valorization; catalysis; green chemistry; recycling

1. Introduction
The technological expansion in the modern era has resulted in a substantial accumula-
tion of metal-rich wastes [1–3]. The valorization of such wastes requires a comprehensive
strategy that integrates smart and effective waste management technologies and efficient
Citation: Wink, K.; Hartmann, I. recycling methods. Given the limited reserves of some critical metals and other valuable ele-
Recent Progress in Turning Waste into ments and the challenges linked with their mining and purification, their recycling becomes
Catalysts for Green Syntheses. Sustain. a critical environmental goal [4]. This is particularly evident in the context of recycling
Chem. 2024, 5, 27–39. https://
catalysts due to their indispensable function in the chemical, energy, and environmental
doi.org/10.3390/suschem5010003
sectors. Given these circumstances, innovative methodologies for the extraction of precious
Academic Editor: Konstantinos or critical metals from metal-enriched waste have been presented recently [5–7]. Within the
S. Triantafyllidis field of sustainable chemistry, the transformation of waste into high-performance catalysts
for applications under mild conditions is of particular interest [8,9]. Such strategies embody
Received: 12 February 2024
the principles of green chemistry and a circular economy, emphasizing resource efficiency
Revised: 13 March 2024
as well as waste and energy minimization [10–12]. In recent years, many literature reviews
Accepted: 14 March 2024
Published: 16 March 2024
covering various facets of recycling metal-loaded wastes have been published [6,13–18]. The
direct application of waste-derived catalysts is comprehensively covered in some reviews,
including utilizing waste-derived nanomaterials [19], organic syntheses using recycled Pd
and Au [9], catalytic hydrogen production [20], pollutant decontamination [21,22], water
Copyright: © 2024 by the authors. splitting [20,23], and glycerol transformation [24].
Licensee MDPI, Basel, Switzerland.
This article is an open access article 2. Catalyst Recycling and Reuse
distributed under the terms and This review addresses current innovative approaches in the generation of waste-
conditions of the Creative Commons derived catalysts for chemical transformations. Table 1 gives an overview of the presented
Attribution (CC BY) license (https://
articles. We divided the articles according to the waste type, recycled catalyst, recycling
creativecommons.org/licenses/by/
method, and applied catalytic reaction. The waste type is organized as e-waste, spent
4.0/).

Sustain. Chem. 2024, 5, 27–39. https://doi.org/10.3390/suschem5010003 https://www.mdpi.com/journal/suschem

Sustain. Chem. 2024, 5 28

lithium-ion batteries, and wastewater from different sources. The recycled catalyst systems
range from noble metals such as Au, Pd, and Ru to transition metals (oxides) such as Cu, Ni,
CuNi, and LiNix Mny Coz oxides from used lithium-ion batteries. The methods for recycling
and extracting the catalyst span a wide spectrum, from chemical, physical and mechanical
processing to thermal treatment, and complexation-based methods, and methods based
on functionalized nanoparticles. The applied reactions catalyzed by the recycled catalysts
cover different organic syntheses such as cross-coupling, oxidation, or reduction.

2.1. Catalysts from e-Waste

E-waste covers a wide range of discarded electronic and electrical equipment and its
components. It ranges from consumer electronics such as televisions and smartphones to
more complex and larger equipment such as laptops, desktop computers, and servers. The
metals found in these devices vary considerably in both composition and quantity. Base
metals, including Al, Fe, Cu, Sn, Zn, Ni, and Pb, are ubiquitous in all forms of electronic
waste. They are commonly found in wiring, structural elements, power supplies, and
printed circuit boards (PCBs). In contrast, precious metals such as Au, Ag, and Pd are more
selectively localized, mainly in specialized components such as electrical contacts, PCBs,
and capacitors. The following studies have explored innovative methods to recover such
metals and utilize them for catalysis.
Ryabchuk et al. developed a feasible route for the valorization of base metals from
low-quality PCBs that have low amounts of precious metals [25]. The approach involved
incorporating the abundant Cu present in PCBs into an alumina support and using this
system as a catalyst. After leaching different metals such as Cu, Ni, Zn, Fe, Pb, Ag, and
Sn from PCBs with 5 M HNO3 , non-noble metals were selectively deposited onto an
alumina substrate by dropping the metal solution into an alkaline γ-Al2 O3 suspension
(Figure 1a,b). Subsequent pyrolysis at 800 ◦ C produced a Cu-based γ-Al2 O3 catalyst
with a Cu content of 5.7 wt%. The catalyst showed high catalytic activity for several
reactions, including the hydrogenation of N-heterocycles and acetophenones, as well as
deoxygenation and methanol synthesis via formamide hydrogenation, with moderate-to-
high yields depending on the reaction investigated. Other synthesized supported catalysts,
such as Cu on TiO2 , SiO2 , or MgO, showed no or negligible activity. In comparison to
a CuO/γ-Al2 O3 catalyst, the developed catalyst showed similar activity while requiring
higher temperatures and higher catalyst loading. A shortcoming of this catalyst was that its
catalytic activity dropped rapidly to 0% after its third use due to Cu leaching. Interestingly,
the residual undeposited solid e-waste still contained precious metals, which could be
utilized in further recycling processes.
Sustain. Chem. 2024, 5, 3 3 of 13
Sustain. Chem. 2024, 5 29

Figure 1.
Figure Catalysts from
1. Catalysts from e-waste.
e-waste. (a)
(a) Cu/Al
Cu/Al22OO3 3catalyst
catalystfrom
fromPCBs.
PCBs.(b) (b)Scanning
Scanningelectron
electronmicroscopy
microscopy
(SEM) image (scale bar: 500 nm). Reprinted (adapted) with permission from Ryabchuk etetal.
(SEM) image (scale bar: 500 nm). Reprinted (adapted) with permission from Ryabchuk al.[25].
[25].
Copyright
Copyright 2021 American Chemical Society.
American Chemical Society. (c) Preparation
Preparation and synthesis of a homogeneous Au(III)
a homogeneous Au(III)
catalyst. Adapted from
catalyst. from McCarthy
McCarthyetetal. al.[26].
[26].Used
Usedunder
underCC CCBY
BY4.0. (d)(d)
4.0. Principle
Principleof of
Pd(II) recovery
Pd(II) recoveryfor
for micellar
micellar catalysis.
catalysis. Reproduced
Reproduced withwith permission
permission fromfrom Lacanau
Lacanau et al.et[27].
al. [27]. Copyright
Copyright 2020,2020, Wiley-
Wiley-VCH.
VCH. (e) Preparation
(e) Preparation of thiourea-functionalized
of thiourea-functionalized magnetic magnetic core rods
core stirring stirring rods (MCSR-ATU,
(MCSR-ATU, allyl
allyl thiourea
thiourea functionalized magnetic core stirring rods). (f) SEM image of Au(0)
functionalized magnetic core stirring rods). (f) SEM image of Au(0) catalyst (scale bar: 1 µm). catalyst (scale bar: 1
µm). (g) Hydrogenation of 4-nitrophenol by Au(0) catalyst. Reproduced from Li et al. [28] with
(g) Hydrogenation of 4-nitrophenol by Au(0) catalyst. Reproduced from Li et al. [28] with permission
permission from the Royal Society of Chemistry.
from the Royal Society of Chemistry.

McCarthy
McCarthy et et al.
al. have
have recently
recently demonstrated
demonstrated that that catalyst
catalyst recovery
recovery mustmust notnot focus
focus
primarily on recovering the metal of interest, but that complexed
primarily on recovering the metal of interest, but that complexed metal ions recoveredmetal ions recovered
from
from e-waste
e-waste can can also
also bebe used as effective
used as effective homogeneous
homogeneous catalysts
catalysts for various chemical
for various chemical
reactions [26]. The authors showcased this by extracting Au(III) with different
reactions [26]. The authors showcased this by extracting Au(III) with different complexing complexing
agents
agents from
from old
old subscriber
subscriber identity
identity module
module (SIM)
(SIM) cards
cards using
using aa mild
mild and
and efficient
efficient leaching
leaching
method (Figure 1c). The extraction process consisted of stripping
method (Figure 1c). The extraction process consisted of stripping the organic parts the organic parts
fromfrom
SIM
SIM
cardscards
using using tetrahydrofuran
tetrahydrofuran (THF), followed
(THF), followed by the sequential
by the sequential removal of removal of co-
co-incorporated
incorporated
Cu and Ni metals.Cu andWhile NiCumetals. While Cu
was oxidized withwas
H2oxidized with H2O2 in
O2 in an ammoniacal an ammoniacal
sulfate solution, Ni
sulfate solution,
was oxidized with NiHCl.
was Various
oxidizedsynthesized
with HCl. dithiooxamide-derived
Various synthesized dithiooxamide-derived
leaching agents were
leaching
evaluatedagents were
to extract evaluated
Au(III) to extract
as a complex Au(III)
under mildas a complex
conditions. underrefining
Further mild conditions.
to recover
Further refining to recover elemental Au from the Au(III) complexes
elemental Au from the Au(III) complexes would not be economically feasible, according would not be to
economically feasible, according to the authors. Instead, the Au(III) complex
the authors. Instead, the Au(III) complex was utilized directly as a catalyst. The catalyst’s was utilized
directly as a evaluated
efficacy was catalyst. The for catalyst’s efficacy was
various reactions, suchevaluated for various
as the cyclization reactions, such
of propargylic amides,as
the
the cyclization
condensation of propargylic amides,
of acetylacetone andtheo-iodoanilin,
condensationaddition
of acetylacetone
reactionsand o-iodoanilin,
of electron-rich
addition
arenes and reactions of electron-rich
α,β-unsaturated arenes
carbonyl and α,β-unsaturated
compounds, and oxidative carbonyl compounds,
C–C couplings of and
aryl
oxidative
silanes and C–C couplings
arenes. of aryl silanes
For example, and arenes.
the cyclization For example,
reactions showed thecomparable
cyclization reactions
yields to
a benchmark
showed catalyst
comparable aftertothe
yields use of an additive
a benchmark during
catalyst after thethe
usesynthesis.
of an additive Theduring
estimated the
cost of theThe
synthesis. recovered
estimatedAu(III)
costcatalyst was estimated
of the recovered to catalyst
Au(III) be less thanwas half of a comparable
estimated to be less
commercially
than half of a available
comparable catalyst (AuCl3 ). available
commercially This cost catalyst
advantage would
(AuCl be amplified
3). This when
cost advantage
considering the additional profit generated from co-produced Cu(II) and Ni(II) salts.
Sustain. Chem. 2024, 5 30

A similar approach was conducted by Lacanau et al. by extracting Pd from e-waste

and utilizing Pd(II) as a catalyst, thus circumventing conventional isolation and purifi-
cation steps [27]. The authors integrated hydrometallurgy for the extraction of Pd and
the use of surfactant-based aqueous systems for its direct application in a cross-coupling
reaction (Figure 1d). The waste of choice was multi-layer ceramic capacitors from computer
motherboards and camera boards, where Pd is alloyed with Ag. After leaching with 3 M
HNO3 , Pd was selectively extracted from the leaching solution with an organic extractant,
either bis(2-ethylhexyl)sulfoxide or N,N′ -dimethyl-N,N′ -dibutyltetradecylmalonamide.
Subsequently, one of the two tris-(hydroxymethyl)acrylamide-based surfactants developed
was used to back-extract Pd(II) into an aqueous micellar solution. The aqueous micellar
solution containing Pd(II) was employed in a Suzuki–Miyaura cross-coupling reaction
of an aryl halide and aryl boronic acid in water. The catalyst exhibited similar catalytic
activity to conventional media prepared from commercial Pd(II) salt. The aqueous micellar
Pd(II) solutions were found to be stable for months after back-extraction, as no Pd(II)
hydrolysis was observed. This suggests that the micellar solutions can be stored and used
for further experiments without significant degradation or loss of the catalyst. Additionally,
the authors demonstrate that this process simplifies the recovery of Pd by avoiding several
waste-generating steps, such as precipitation, burning, and electrowinning of Pd.
In the context of upcycling precious metals, Li et al. developed a sophisticated and
highly selective adsorbent for recycling gold from e-waste [28]. The leaching process
involved immersing PCBs in a 10 M NaOH solution to remove the epoxy coating, followed
by soaking in aqua regia. The approach employed capturing and reducing Au(III) ions
in situ from the solution as Au(0) particles via a magnetic adsorbent functionalized with
thiourea. The redox-active adsorbent was synthesized by functionalizing non-porous silica-
coated magnetic Fe3 O4 core stirring rods with thiourea through distillation-precipitation
polymerization (Figure 1e,f). The rapid adsorption kinetics and remarkable selectivity of the
adsorbent rendered it an excellent candidate for practical Au recovery from complex waste
solutions. Hence, the catalytic activity of the gold-loaded adsorbent was demonstrated
for the hydrogenation of 4-nitrophenol to 4-aminophenol in the presence of NaBH4 as
a reducing agent (Figure 1g). In comparison to several other supported Au catalysts,
the catalyst exhibited exceptional reaction rates. Its high reusability without significant
efficiency losses and ease of recovery by magnetic separation render it a promising method
for sustainable catalysis. In a similar approach by their working group, Wu et al. also
demonstrated the recovery of Pd(II) via functionalized magnetic particles for a Suzuki–
Miyaura cross-coupling reaction between bromobenzene and 4-formylphenylboronic acid
with conversion efficiencies of up to 99% [29].

Table 1. Overview of the presented literature.

Applied Catalytic
Waste Type Recycled Catalyst Recycling Method References
Reaction
Precipitation of acid leachate Hydrogenation,
Ryabchuk et al.,
Cu-based on Al2 O3 and subsequent deoxygenation, and
2021 [25]
pyrolysis hydrogenolysis reactions
Mild extraction with Set of different organic McCarty et al.,
Au(III)
complexing agents reactions 2022 [26]
Electronic waste
Selective extraction with Lacanau et al.,
Pd(II) Cross-coupling
extractants and surfactants 2020 [27]
In situ capture and reduction
Hydrogenation of
Au of Au ions by functionalized Li et al., 2022 [28]
4-nitrophenol
particles
Sustain. Chem. 2024, 5 31

Table 1. Cont.

Applied Catalytic
Waste Type Recycled Catalyst Recycling Method References
Reaction
Amarasekara et al.,
Oxidation of furans
2022 [30]
Oxidation of D-glucose to Amarasekara et al.,
LiNix Mny Coz O2 Pyrolysis of spent Li-ion glycolic acid 2022b [31]
Spent lithium-ion battery black material
batteries Decarboxylative
Amarasekara et al.,
dimerization of
2023 [32]
levulinic acid
Reduced black Ball milling, calcination, and
Hydrogenation of furfurals Paone et al., 2022 [33]
mass of battery reduction with H2
Extraction with porous
Photothermal catalytic
Ni core-shell particles and Wang et al., 2022 [34]
CO2 -to-CO hydrogenation
calcination/reduction
Selective adsorption by MOF
Electrochemical CO2
Au and calcination/reduction Zhu et al., 2022 [35]
reduction
with H2
Selective adsorption by
hybrid absorbent and
Au, Pd Oxidation of 4-nitrophenol Li et al. [36]
calcination/reduction
with H2
Selective Pd(II) extraction by
Wastewater
Pd porous polymer and NaBH4 Cross-coupling Song et al., 2022 [37]
reduction
Electrochemical reduction of Cross-coupling and
Oladeji et al.,
Pd Pd(II) on carbon electrocatalytic H2
2022 [38]
black particles generation
Slavik and Smith
Extraction and in situ
2020 [39]
Pd reduction of Pd(II) by a Cross-coupling
Piras et al., 2020 [40]
hybrid hydrogel
Albino et al., 2023 [41]
Impregnation method
Ru on Nb–carbon
followed by NaBH4 Hydrogenation of furfurals Yao et al., 2022 [42]
support
reduction

2.2. Catalyst from Spent Lithium-Ion Batteries

Lithium-ion batteries (LIBs), integral to modern energy storage, contain several ele-
ments and compounds in varying amounts, depending on the type of battery. They contain
metals, often as their respective oxides, such as Li, Co, Ni, Mn, Fe, Al, and Cu, as well as
non-metallic elements such as graphite and organic solvents, binders, and separators. As
the global demand for LIBs increases rapidly, the resulting waste creates a need to recycle
spent batteries into valuable materials. Currently, recycled catalysts from LIBs are mainly
being investigated for their catalytic pollutant decontamination or water electrolysis capa-
bilities. From the viewpoint of a circular economy approach together with an advancement
of green chemistry, our focus is on articles that use the recycled catalytic materials from
LIBs for the synthesis of organic molecules.
In this context, Amarasekara et al. reported innovative approaches to enhance the
value of biomass-derived compounds through conversion by recycled catalysts from spent
LIBs [30–32]. The recycling of LIBs for reuse as catalysts involved a discharging and
mechanical dismantling process (Figure 2a). Interfering organic residues, e.g., binders, were
removed by pyrolyzing the cathode and anode black material at 600 ◦ C. After grinding and
sieving, the resulting powder of LiNix Mny Coz O2 /C was used as a catalyst (Figure 2b). The
 [33]. Similar to Amarasekara et al., after the mechanical separation, the black mass, con-
sisting of metal oxides and graphite, was sieved, ball-milled, and calcinated at 600 °C for
6 h. However, additionally, the material was reduced at 500 °C for 6 h under hydrogen
flow in the last step. The final catalyst particles consisted mainly of Co and Ni metals and
Sustain. Chem. 2024, 5
oxides of Mn and Al. The catalyst was demonstrated for selective reduction reactions of
32
biomass-derived furfural and other aldehydes and ketones. The catalyst was showcased
for direct hydrogenation with H2 as well as for milder and safer transfer hydrogenation
using 2-propanol as both the solvent and hydrogen donor. Furfural was successfully con-
authors demonstrated the practicability of this catalyst for the transformation of different
verted to furfuryl alcohol in 90 min at 120 °C using H2 in 2-propanol. The conversion of
biomass-derived substrates, namely the oxidation of cellulose-derived furans to their
furfural under transfer hydrogenation conditions using 2-propanol as the solvent and pro-
corresponding carboxylic acids [30], the oxidation of D-glucose to glycolic acid [31], and the
ton donor resulted in a 70% yield. At temperatures above 150 °C, the yield increased to
decarboxylative dimerization of levulinic acid [32]. For example, the oxidation of furans,
98%, achieving
including similar results5-hydroxymethyl
furan-2-aldehyde, as the H2 route. The catalyst
furfural, andwas
5,5able to convert other sub-
′ -[oxybis(methylene)]bis

[2-furaldehyde], achieved moderate-to-high yields ranging from 82% to 97%and

strates, namely 5-hydroxymethylfurfural, benzaldehyde, acetophenone, cyclohexa-
depending on
none, with varying yields, indicating a broader possible scope of substrates. These
the substrate used. The catalyst showed robust reusability over four cycles under optimized find-
ings highlight
conditions the oxidation
for the importance of of the reduction of with
furan-2-aldehyde, the black mass
a slight to metallic
decrease Co and
in yield fromNi as
97%
a necessary step for the hydrogenation
to 86% while maintaining full conversion. reaction.

Figure
Figure 2. Catalystsfrom
2. Catalysts fromspent
spentlithium-ion
lithium-ionbatteries.
batteries.
(a)(a) Preparation
Preparation of catalytic
of catalytic LIBLIB black
black mass.
mass. (b)
(b) SEM image of catalyst (scale bar: 5µm). Reprinted (adapted) with permission from
SEM image of catalyst (scale bar: 5µm). Reprinted (adapted) with permission from Amarasekara et Amarasekara
et
al.al. [30].
[30]. Copyright
Copyright 2022American
2022 AmericanChemical
ChemicalSociety.
Society.(c)(c)Preparation
Preparationstepssteps for
for catalytic
catalytic LIB black
mass. Reprinted
Reprinted(adapted)
(adapted) with permission
with from
permission Paone
from et al.et[33].
Paone Copyright
al. [33]. 2022 American
Copyright Chem-
2022 American
ical Society.
Chemical Society.

Amarasekara et al. finalized their recycled catalyst by oxidizing it at 600 ◦ C, resulting

in an oxide catalyst. In contrast, Paone et al. included a reduction step in the recycling of
LIBs, leading to the partial production of catalytically active metal particles (Figure 2c) [33].
Similar to Amarasekara et al., after the mechanical separation, the black mass, consisting
of metal oxides and graphite, was sieved, ball-milled, and calcinated at 600 ◦ C for 6 h.
However, additionally, the material was reduced at 500 ◦ C for 6 h under hydrogen flow
in the last step. The final catalyst particles consisted mainly of Co and Ni metals and
oxides of Mn and Al. The catalyst was demonstrated for selective reduction reactions of
biomass-derived furfural and other aldehydes and ketones. The catalyst was showcased for
direct hydrogenation with H2 as well as for milder and safer transfer hydrogenation using
2-propanol as both the solvent and hydrogen donor. Furfural was successfully converted
to furfuryl alcohol in 90 min at 120 ◦ C using H2 in 2-propanol. The conversion of furfural
under transfer hydrogenation conditions using 2-propanol as the solvent and proton donor
resulted in a 70% yield. At temperatures above 150 ◦ C, the yield increased to 98%, achieving
similar results as the H2 route. The catalyst was able to convert other substrates, namely
5-hydroxymethylfurfural, benzaldehyde, acetophenone, and cyclohexanone, with varying
yields, indicating a broader possible scope of substrates. These findings highlight the
Sustain. Chem. 2024, 5 33

importance of the reduction of the black mass to metallic Co and Ni as a necessary step for
the hydrogenation reaction.

2.3. Catalysts from Wastewater

Metal-contaminated wastewaters, whether from industrial effluents or urban runoff,
are known for their potential toxicity, posing acute and chronic risks to both human health
and ecosystems. The mandatory removal of hazardous metals from wastewater often
requires a high energy input and can result in the release of secondary pollutants. Such
processes, while effective, come with their own environmental costs, amplifying the chal-
lenge of sustainable wastewater treatment. However, the simultaneous sequestration and
transformation into useful catalysts enable these environmental liabilities to be converted
into promising tools for green chemistry. Due to the concurrent presence of metal ions
in wastewater, the key obstacle to the recovery of metals from wastewater is the creation
of highly selective adsorbents for specific metal ions. This is mainly achieved by porous
3D networks with a functionalized surface. By utilizing such sophisticated architectures,
the formation of metal particles is scaled down to particle sizes at the nanoscale, enabling
faster reaction rates. This section will present several innovative approaches that focus on
such strategies.
Wang et al. introduced a novel approach for extracting Ni from widely available elec-
troplating wastewater and built it into an advanced photothermal catalyst for converting
CO2 to CO, which is a significant reaction step in numerous chemical transformations [34].
The group employed a core-shell adsorbent comprising a magnetic Fe3 O4 core encapsu-
lated by two layers: a dense SiO2 layer that protected the core as an etching barrier in the
acidic wastewater and an outer layer of amine-functionalized mesoporous SiO2 that could
efficiently scavenge Ni(II) from the wastewater (Figure 3a,b). Upon reaching adsorption
equilibrium, the Ni(II) captured alongside the adsorbent was magnetically isolated. This
assembly was subsequently calcined and reduced under H2 , yielding a core-shell catalyst
with highly dispersed Ni in the mesoporous SiO2 layer. In its practical application, the
catalyst excelled in the reverse water–gas shift reaction, underlining the potential of waste-
derived materials for carbon capture and utilization strategies. The catalyst demonstrated
not only high CO production rates and selectivity but also remarkable stability and a re-
duced CO2 footprint compared to the conventional thermocatalytic pathway. The catalyst’s
performance can be ascribed to the Fe3 O4 core’s light-harvesting and high photo-to-thermal
conversion efficiency (Figure 3c). This resulted in temperatures of up to 400 ◦ C under
concentrated light, primarily driving a thermochemical reaction route. The SiO2 shell
confines the energy due to its thermal insulation properties while also functioning as a
support for Ni particles. Wang et al.’s innovative catalyst displayed a higher CO production
rate than commercial Cu-ZnO-Al2 O3 catalysts and other reported photothermal catalysts.
The consistent chemical composition of the catalyst across three different waste solutions
indicates a stable absorption performance of the particles despite the varying mixtures of
Ni(II) wastewater used.
In a separate study on CO2 reduction, Zhu et al. presented a novel Metal–Organic
Framework (MOF) for the selective adsorption of AuCl4 − from solution and its subsequent
transformation into an active electrochemical catalyst [35]. The synthesis of the MOF was
carried out via solvothermal synthesis using ZrCl4 , Ni(NO3 )2 , and isonicotinic acid in DMF
as precursors. The MOF exhibited a high surface area of 1570 m2 /g and a high Au(III)
capacity of 415 mg/g. The immersion of the MOF in an artificial e-waste solution containing
AuCl4 − , followed by calcination at 200 ◦ C under a H2 /Ar atmosphere, resulted in Au
nanoparticles uniformly dispersed within the MOF network with adjustable Au particle
sizes between 2.4 and 4.4 nm depending on the initial AuCl4 − concentration (Figure 3d).
The selectivity for Au(III) adsorption was notably robust. Despite the presence of competing
metal ions such as Fe, Ni, Cu, Co, Zn, and Mn at concentrations an order of magnitude
greater than AuCl4 − , the interference of the adsorption was minimal. The Au/MOF system
proved to be highly efficient for the electrochemical reduction of CO2 to CO with a Faradaic
Sustain. Chem. 2024, 5 34

efficiency of 95%, maintaining its performance for 15 h with a minor decrease in activity
(−13%) and efficiency (−7%). This breakthrough underscores the multifaceted potential of
MOFs to obtain low-cost and high-performance size-adjustable Au-based catalysts from
wastewater.
The ability of MOFs to scavenge precious metals from complex wastewater mixtures
was also demonstrated by Li et al. with a hybrid absorbent for the selective recovery
of Au and Pd for the catalytic degradation of 4-nitrophenol [36]. The hybrid adsorbent
consisted of a functional graphene foam linked with a Cu-based MOF. The graphene
foam was activated at 120 ◦ C for 12 h and functionalized with 4,4′ -thiodibenzenethiol at
40 ◦ C with a reaction time of 48 h, yielding a thiol-functionalized graphene foam (FGF).
To synthesize the MOF@FGF hybrid, the FGF was modified with a benzene-1,4-dithiol
linker and subsequently mixed with an ammoniacal cupric nitrate solution, washed, and
dried. The prepared hybrid absorbent was able to recover Au(III) and Pd(II) from artificial
wastewater with recovery rates of 90.4% over five cycles and high adsorption capacities of
3715 mg/g for Au(III) and 3345 mg/mg for Pd(II) at concentrations ranging from 20 mg/L
to 2000 mg/L. The addition of potentially interfering ions of Ag(I), Li(I), Pt(II), Co(II), Fe(II),
Cu(II), Al(III), Sb(III), Fe(III), and Sn(IV) at 200 mg/L did not result in a significant reduction
of Au(III) and Pd(II) adsorption. The synthesis of the carbon-supported metal nanoparticle
catalysts involved calcination at 800 ◦ C under N2 and H2 for 2 h, which generated particles
with sizes between 2 nm and 5 nm. To prove the catalytic efficiency, a catalytic oxidation of
4-nitrophenol via peroxymonosulfate activation was used as a model reaction.
A similar nanocage approach was presented by Song et al., who developed porous
polyisothiocyanurates, termed covalent isothiocyanurate framework (CITCF), for Pd ad-
sorption [37]. This approach enabled the recovery of Pd(II) from artificial wastewater,
followed by the reduction of Pd(II) to Pd particles within the polymer and their subse-
quent use as a catalyst for the Suzuki–Miyaura cross-coupling reaction. CITCFs were
synthesized by heating a mixture of 1,4-phenyl-diisothiocyanate and ZnCl2 (Figure 3e) in a
sealed ampoule at 300–500 ◦ C. The resulting material was thoroughly washed and purified
through various solvents and dried overnight at 90 ◦ C. The CITCFs exhibited high surface
areas of up to 1589 m2 /g. Due to the thiourea sites in the framework, the extraction from
artificial wastewater containing PdCl4 2− showed a high Pd(II) capacity of 909 mg/g. The
reduction of Pd(II) within the polymer matrix was achieved by treatment with NaBH4 and
subsequent washing and drying steps, resulting in Pd particle sizes of 1.49 nm. The high
thermal and chemical stability of the material, coupled with its exceptional selectivity for
Pd(II)—notably five times greater than for Pt(IV) and significantly higher than for other
transition metals like Ni, Fe, Zn, and Cd—emphasizes its potential for selective metal
recovery. The catalytic activity of Suzuki–Miyaura cross-coupling reactions was confirmed
using both Pd(II) and Pd(0) within the polymer, with the reduced Pd particles giving
superior results. Several reactions with bromobenzene derivatives and phenylboronic acid
derivatives were carried out under optimized conditions, displaying exclusive selectivity
and high yields between 81.6% and 99.9%. Over five catalytic cycles, the catalyst exhibited
no loss of activity and no reduction in surface area, demonstrating its robustness as an
environmentally friendly waste-derived catalyst.
Sustain. Chem. 2024, 5, 3 9 of 13
Sustain. Chem. 2024, 5 35

Figure 3. Catalysts from wastewater. (a) Preparation of Ni-based catalyst for water–gas shift reaction.
Figure
(b) TEM 3. image
Catalysts from wastewater.
of catalyst (a) Preparation
particle. Scale bar: 50 nm. of (c)
Ni-based catalyst for
CO production water–gas
rate and CO shift reac-
selectivity
tion. (b) TEM image of catalyst particle. Scale bar: 50 nm. (c) CO production rate and CO selectivity
for different compositions of the catalyst in a batch reactor. Adapted from Wang et al. [34]. Used
for different compositions of the catalyst in a batch reactor. Adapted from Wang et al. [34]. Used
under CC BY 4.0. (d) MOF. Reproduced (adapted) with permission from Zhu et al. [35]. Copyright
under CC BY 4.0. (d) MOF. Reproduced (adapted) with permission from Zhu et al. [35]. Copyright
2020, Wiley.
2020, Wiley. (e)
(e) Synthesis
Synthesis of
of porous
porous polyisothiocyanurate
polyisothiocyanurate network
network forfor Pd
Pd capture.
capture. Reprinted
Reprinted from
from
Song et al. [37]. Copyright 2022, with permission from Elsevier. (f) Pd nanoparticles
Song et al. [37]. Copyright 2022, with permission from Elsevier. (f) Pd nanoparticles on carbon black on carbon black
nanoparticlesafter
nanoparticles afternanoimpact
nanoimpactdeposition.
deposition.Scale
Scale bar
bar (left
(left image):
image): 0.20.2
µm;µm; scale
scale barbar (right
(right image):
image): 50
nm. Adapted
50 nm. Adapted fromfrom
Oladeji et al. et
Oladeji [38].
al. Used
[38]. under CC BYCC
Used under 4. (g)
BYPreparation of gelatinous
4. (g) Preparation Pd scaven-
of gelatinous Pd
ger network
scavenger and beads:
network (1) Suspending
and beads: DBS-CONHNH
(1) Suspending DBS-CONHNH 2 in alginate solution,
2 in alginate (2) heating
solution, for com-
(2) heating for
plete dissolution, (3a) adding dissolved CaCl 2, (4a) forming of a gel network. Alternatively, a solu-
complete dissolution, (3a) adding dissolved CaCl2 , (4a) forming of a gel network. Alternatively, a
tion of CaCl
solution 2 can be added dropwise or in a continuous stream to form (3b) beads or (4b) strings.
of CaCl 2 can be added dropwise or in a continuous stream to form (3b) beads or (4b) strings.
Adapted from Piras et al. [39] Used under CC BY 4.0. (h) Image of Pd-loaded gel beads. (i) TEM
Adapted from Piras et al. [39] Used under CC BY 4.0. (h) Image of Pd-loaded gel beads. (i) TEM
image of Pd nanoparticles encapsulated in the hydrogel. Adapted from Albino et al. [41]. Used un-
image of Pd nanoparticles encapsulated in the hydrogel. Adapted from Albino et al. [41]. Used under
der CC BY 4.0. (j) Preparation of Ru/Nb–carbon catalyst. Reprinted (adapted) with permission from
CC BY
Yao 4.0.
et al. (j) Preparation
[42]. of Ru/Nb–carbon
Copyright 2022 American Chemicalcatalyst. Reprinted (adapted) with permission from Yao
Society.
et al. [42]. Copyright 2022 American Chemical Society.
An innovative method for the upcycling of a noble metal was presented by Oladeji et
An innovative method for the upcycling of a noble metal was presented by Oladeji
al. via impact electrochemistry for the recovery of Pd from solution and its subsequent
et al. via impact electrochemistry for the recovery of Pd from solution and its subsequent
use as a catalyst [38]. The authors used the nanoimpact technique to generate carbon-sup-
use as a catalyst [38]. The authors used the nanoimpact technique to generate carbon-
ported Pd catalysts from artificial wastewater with low concentrations of PdCl2. The syn-
supported Pd catalysts from artificial wastewater with low concentrations of PdCl2 . The
thesis involved the collision of carbon black nanoparticles (CB NPs) with an electrode im-
synthesis involved the collision of carbon black nanoparticles (CB NPs) with an electrode
mersed in wastewater, leading to the reduction and irregular deposition of Pd onto the
immersed in wastewater, leading to the reduction and irregular deposition of Pd onto the
surface of the nanoparticles (Figure 3f). In the absence of CB NPs, the recovery rate of
surface of the nanoparticles (Figure 3f). In the absence of CB NPs, the recovery rate of Pd(II)
Sustain. Chem. 2024, 5 36

was about 65%. However, upon their addition, this rate increased to 85%. Notably, the
introduction of CB NPs during chronoamperometric experiments considerably reduced
the background deposition on the electrode. To demonstrate the catalytic properties of
the resulting material, both a Suzuki–Miyaura cross-coupling reaction of phenylboronic
acid with iodobenzene and an electrocatalytic hydrogen generation were carried out in a
proof of concept. Although insights into the selectivity of the nanoimpact method for Pd
were not reported, this approach highlights the capability of electrochemical techniques for
metal extraction and catalyst production from wastewater.
Another promising strategy to recover Pd from wastewater was demonstrated by
Smith et al. [39–41]. The key concept revolves around the use of a gelatinous material
for the selective capture of Pd from aqueous solutions and the subsequent use of Pd as a
catalyst. The hybrid hydrogels developed have a high affinity and specificity for Pd(II) ions
and can reduce Pd(II) to Pd(0). Such an approach is particularly relevant when considering
recycling Pd-rich wastewater. The catalytic active material was prepared by encapsu-
lation of Pd nanoparticles via an in situ reduction of Pd(II) in a hybrid hydrogel made
from an acylhydrazide-functionalized 1,3:2,4-dibenzylidenesorbitol (DBS-CONHNH2 ) low-
molecular-weight gelator combined with a polymer gelator such as alginate (Figure 3g,h).
The Pd(II) solution used was an acidic PdCl2 solution mimicking wastewater. The cat-
alytic material could be prepared either as a catalytic gel block [39] or as catalytic gel
beads/worms [40]. In particular, the catalytic beads prepared with agarose as the polymer
gelator were mechanically more stable, easier to reuse, and not prone to Pd leaching com-
pared to the gel block and the beads/worms prepared with alginate (Figure 3i) [41]. The
beads also demonstrated thermal stability up to 99 ◦ C and showed three-time reusability
after filtering and washing. These Pd-enclosing materials were extensively demonstrated to
be effective catalysts for cross-coupling reactions, including Sonogashira and Heck [39,40]
and Suzuki–Miyaura [41] reactions, under environmentally friendly and mild conditions
with high yields.
Yao et al. developed a novel method for fabricating Ru-based catalysts using Ru-
rich waste from lignite depolymerization processes [42]. The recycled catalyst showed
comparable efficiencies to conventional Ru catalysts in the hydrogenation of ethyl levulinate
to γ-valerolactone, maintaining its activity across multiple cycles. The catalyst synthesis
was achieved via an impregnation method in which a Nb–carbon support was mixed
with Ru-containing wastewater, stirred for 2 h, and then directly reduced with NaBH4
solution in an ice bath for 2 h. The Nb–carbon support itself was synthesized by mixing Nb
oxalate with activated carbon, followed by drying, grinding, and calcination in an inert
atmosphere (Figure 3j). The catalyst was applied to a broad substrate scope and proved to
be an effective catalyst for reducing saturated aldehydes and ketones to their corresponding
alcohols. However, it exhibited limitations in the hydrogenation of aromatic compounds,
particularly benzaldehyde and acetophenone, where the yields were significantly reduced
due to complete ring hydrogenation or deoxygenation side reactions.

3. Conclusions and Perspective

Both waste recycling and sustainable chemical processes are urgent global needs that
require innovative strategies. This review has presented insights from various studies since
2020 to highlight the transformative potential of using catalysts derived from different types
of waste. The ability of these waste-derived catalysts to catalyze reactions with reduced
environmental footprints—through diminished greenhouse gas emissions or reduced
solvent use—aligns directly with the 12 principles of green chemistry. As highlighted by
many studies, their catalytic efficiencies often parallel, if not surpass, those of conventionally
sourced catalysts in reactions ranging from biomass conversion to carbon dioxide reduction
or building block synthesis. Techniques such as selective extraction with green complexing
agents, functionalized particles, or smart chemical architectures not only minimize the
environmental impact of the catalyst production process but also often provide unique and
favorable properties to the catalysts.
Sustain. Chem. 2024, 5 37

However, challenges still exist. Fluctuations in waste composition can create irregular-
ities in catalyst properties, potentially lowering their activity, e.g., due to catalyst poisoning.
The transition from laboratory to industrial applications will require process optimization
and further exploration to fully understand their long-term stability and recyclability. The
exact mechanisms by which some waste-derived catalysts accelerate reactions might not be
fully understood. Further insight into the molecular-level interactions can benefit the opti-
mization of the catalytic process. While some studies suggest potential economic benefits,
comprehensive lifecycle evaluations are necessary to quantify both ecological and economic
impacts across the catalyst’s lifecycle. This includes considering the energy and resources
used in the catalyst production, operation, and disposal stages. Addressing these issues
requires an interdisciplinary approach from chemistry, material science, environmental sci-
ence, economics, and policy-making. Despite the complexities, the potential environmental,
resource, and economic benefits make this a highly desirable and significant objective.

Author Contributions: Conceptualization, K.W. and I.H.; writing—original draft preparation, K.W.;
writing—review and editing, K.W. and I.H.; visualization, K.W.; supervision, I.H. All authors have
read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: No new data were created or analyzed in this study. Data sharing is
not applicable to this article.
Conflicts of Interest: The authors declare no conflicts of interest.

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