Research Synopsis [BS-ENVIRONMENTAL SCIENCE]

Nanomaterial Coated 3D Structured Clay Filter for Photocatalytic Treatment of

Water/Wastewater from Batch to Scaleup Reactors

By:

Bilal Ahmed
(ENV-20F-001)

Fazal-ur-Rehman
(ENV-20S-009)
____________________________________________

Supervisor:

Abdul Majeed Pirzada

A SYNOPSIS SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENTS

FOR THE DEGREE OF BS OF ENVIRONMENT IN

ENVIRONMENTAL SCIENCES

SINDH MADRESSATUL ISLAM UNIVERSITY

(2024)

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 Research Synopsis [BS-ENVIRONMENTAL SCIENCE]

Introduction:

The growing population demands industrial growth for their survival, but such development has
placed the environment under serious threat[1]. In an era marked by rapid urbanization and
industrial expansion, wastewater management has emerged as a critical global concern.
Discharging untreated or inadequately treated wastewater into natural water bodies has
reached alarming levels, presenting an imminent threat to public health, environmental
sustainability, and socio-economic stability.

Addressing water pollution requires a multifaceted approach, including stricter regulations,

better waste management practices, promoting sustainable agriculture, and investing in
technologies for water treatment and purification. It's crucial to raise awareness and promote
responsible behavior to protect our precious water resources for future generations[2].

The pursuit of efficient wastewater treatment technologies has been at the forefront of
scientific and engineering endeavors. Over the years, innovative methodologies have emerged,
harnessing the power of diverse treatment processes, from physical and biological mechanisms
to cutting-edge advancements in chemical and resource recovery techniques[3].

The cornerstone of these technologies lies in their ability to remove contaminants and
pollutants from wastewater streams, mitigating the adverse impacts on water bodies and
ecosystems. Physical treatments, such as screening and filtration, serve as initial steps in
removing solid debris and suspended particles[4]. Meanwhile, biological treatments employ the
power of microorganisms to break down organic matter, while chemical treatments facilitate
the coagulation and disinfection necessary for purification.

Advancements in technology have led to the development of sophisticated systems like

membrane filtration and reverse osmosis, capable of achieving higher purification standards by
removing even minute pollutants[5]. Emerging technologies, such as electrocoagulation and

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nanotechnology, offer promising avenues for enhanced efficiency and pollutant removal in
wastewater treatment processes.

Yet, amidst these advancements, challenges persist. The increasing complexity of pollutants, the
demand for sustainable resource recovery, and the need for decentralized systems pose
ongoing hurdles in the realm of wastewater treatment.

This exploration aims to delve into the multifaceted landscape of wastewater treatment
technologies. By examining their strengths, limitations, and evolving paradigms in addressing
wastewater challenges, this endeavor seeks to underscore the importance of continual
innovation and collaboration in safeguarding our water resources for a cleaner, healthier future.

Material processing stands at the forefront of scientific and technological advancements,

particularly in the domain of drinking and wastewater treatment. Among the array of materials,
clay emerges as a noteworthy candidate owing to its cost-effectiveness and multifaceted
properties. Comprised of hydrated aluminum silicates and metal oxides such as Fe2O3 and K2O,
clay exhibits exceptional efficacy in the removal of both organic and inorganic pollutants from
water matrices.

Central to the effectiveness of clay in water treatment is its inherent Cation Exchange Capacity
(CEC)[6], attributed to the permanent negative charge residing on its surface. While natural clay
presents a moderate capacity for anion absorption, refinement through physical and chemical
modifications significantly enhances its Anion Exchange Capacity (AEC). Thermo-activation,
involving controlled calcination between 100°C to 700°C, elevates clay's porosity and surface
area, thereby augmenting its pollutant sorption capabilities[7].

Clay-based filtration systems manifest impressive characteristics including thermal stability,

mechanical robustness, and heightened permeability, thereby substantiating their suitability
and resilience in water treatment applications.

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The advent of 3D printing technology has recently garnered substantial interest, particularly
concerning its application in fabricating porous clay filters tailored for water treatment systems.
Leveraging 3D printing methodologies affords advantages in terms of energy efficiency, raw
material utilization, and customizable filter design, marking a paradigm shift in filter
manufacturing approaches.

Moreover, beyond its independent efficacy, clay serves as an immobilized support for
nanomaterials, underpinning diverse environmental applications, notably in water treatment.
This symbiotic association between clay and nanomaterials accentuates their collective efficacy
in targeted pollutant removal and remediation endeavors. Notably, the utilization of
nanomaterials supported by clay demonstrates immense promise in the photocatalytic
degradation of organic pollutants, signifying a pivotal stride towards purifying water sources
from contaminants.

In amalgamating clay with cutting-edge technologies, the horizon of water treatment is

undergoing a transformative phase. This amalgamation not only underscores the significance of
clay-based solutions in addressing water pollution but also heralds a concerted effort towards
fostering a cleaner and safer environment for all.

Various studies reported improved catalytic and photocatalytic reactions and effective
water/wastewater remediation using TiO2, ZnO, CuO, Fe2O3 immobilized clay
composite/immobilized materials. However, much research is needed to have standardization
and upscaling methods for using clay to support photocatalytic materials for large-scale
applications[8].

In this study, 3D structured clay filters will be designed, and 3D printed. The 3D molded clay is
calcined to produce solid 3D structured clay filters. One promising solar light active
nanomaterial x, y, z chosen as an immobilized photocatalyst. The photocatalytic experiments
will be performed using batch and recirculating semi-batch scaleup reactors under visible light
(LED irradiated light source) and natural sunlight.

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Literature Review:

The environmental strains arising from the escalating demands for industrial and agricultural
expansion by an ever-growing population have culminated in a concerning surge in untreated
wastewater discharge[9]. This untreated effluent, comprising agricultural runoff teeming with
synthetic fertilizers, pesticides, industrial effluents laden with diverse chemicals, and sewage
sludge, has substantially augmented the presence of nutrient-rich micropollutants and
pathogens within ground and surface water sources[10]. This ominous trend portends a severe
threat to these invaluable resources, imperiling the natural ecosystem and casting shadows on
human health.

Water pollution, a persistent global ecological concern, casts its shadow over both daily human
life and the sanctity of the natural environment[11]. The elevated concentrations of pollutants
within aquatic environments serve as breeding grounds for myriad diseases due to their toxic
nature, imposing dire consequences on human health and ecological stability[12]. Recent
studies have extensively documented the prevalence of an array of organic and inorganic
pollutants, particularly highlighting the burgeoning presence of nitrogen-based compounds,
notably nitrate, precipitating a rapid degradation in the quality of diverse water resources[13].

The pernicious implications of nitrate pollution loom large, presenting a formidable and
persistent threat to environmental equilibrium. Nitrate, as a stable and soluble form of nitrogen,
stems from multiple sources encompassing sewage, agricultural runoff, food processing,
manufacturing, and livestock waste[14]. The pressing need for nitrate removal arises from its
central role in fostering eutrophication and its consequential detrimental impacts on aquatic
biodiversity and human health[15].

Despite strides in addressing nitrate pollution, conventional techniques such as biological

denitrification, ion exchange, and reverse osmosis pose challenges[15]. While efficacious, these
methodologies prove energy-intensive and carry the risk of generating secondary pollutants.

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Their limitations include susceptibility to temperature fluctuations, dissolved oxygen effects,

nitrite ion accumulation, and concentration build-up in separated streams[16].

In recent years, the advent of photocatalytic approaches utilizing semiconductor photocatalysts

like TiO2 has emerged as a promising avenue for oxidative degradation[17]. Harnessing low-
energy UV-A light, photocatalysis presents an alternative for treating organically contaminated
water sans additional oxidants[18]. Yet, the substantial band gap of TiO2 restricts practical
efficiency under solar irradiation, prompting investigations into modifying TiO2 for enhanced
visible light absorption, such as through Fe doping[19].

Addressing challenges associated with powder-form photocatalysts, supporting media like clay
have garnered attention for their high porosity and robust sorption properties. Clay's ion
exchange capabilities and widespread availability position it as a resilient adsorbent for water
and wastewater treatment[20].

The recent surge of interest in 3D printing technology has directed focus toward synthesizing
structured and porous filters to support photocatalysts in water treatment applications. Coating
nanoparticles onto 3D clay filters fortifies the photocatalyst, amplifying its strength and
interaction, thereby supporting ion exchange reactions. Techniques such as sol–gel have been
instrumental in coating TiO2 onto 3D clay filters, enabling meticulous control over
nanostructure and porosity[21].

This comprehensive review illuminates the unfolding dynamics within the realm of water
treatment, addressing the exigencies imposed by nitrate pollution, the constraints of
conventional techniques, and the transformative potential of photocatalytic methodologies[22].
It underscores the pivotal roles of TiO2, clay-supported photocatalysts, and innovative 3D
printing approaches in ushering in novel solutions for water remediation, signifying promising
strides toward a sustainable and cleaner aquatic environment[23].

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This literature review offers a more intricate and detailed exploration of the challenges posed by
water pollution, specifically nitrate contamination, and underscores the evolving role of
photocatalytic approaches, highlighting the potential of TiO2, clay-supported photocatalysts,
and innovative 3D printing techniques in shaping water treatment strategies.

Problem Statement:
“Despite advancements in wastewater treatment methodologies, current approaches face
significant limitations in addressing the escalating global water pollution crisis. Conventional
techniques exhibit inefficiencies in removing contaminants and struggle with high energy
consumption and the generation of harmful byproducts. Additionally, membrane-based
methods encounter challenges with fouling and the inability to eliminate dissolved inorganic
substances. The need for more sustainable, efficient, and adaptable solutions to ensure
comprehensive water treatment and mitigate the detrimental effects of pollutants on the
environment and human health remains a pressing concern.”

Novelty Statement:
“The integration of nanomaterials with 3D structured clay filters represents a groundbreaking
advancement in wastewater treatment. By combining the robustness of clay filters with
precisely designed nanomaterial coatings, this fusion unlocks a transformative synergy. It
redefines traditional treatment methods, offering scalable, selective, and eco-friendly systems
capable of efficiently degrading pollutants. This innovation marks a new frontier in
environmental remediation, poised to revolutionize sustainable wastewater treatment
practices.”

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Objectives:

1. Preparation of Immobilized Nanomaterial 3D structured clay filter

2. Photocatalytic treatment of wastewater from batch to scaleup reactors

Materials and methods

Materials:

A 3D mold for the media support will be designed using AutoCAD.

PLA filament will be used for the 3D printing.

Earthenware Clay will be obtained from a pottery shop.

Nanomaterial will be used for the immobilization.

Effluent will be taken from the industry.

Designing of the 3D mold and synthesis of the clay filters:

The 3D molds will be designed in AutoCAD and sliced using UltiMaker Cura software. The
prepared molds will be used to give a standard shape to the clay filter for batch-scale and semi-
batch photocatalytic studies. Clay paste will be prepared by adding an adequate amount of
water to the clay. For structuring the clay filter, once the mold was 3D printed, it was filled with
the obtained clay paste to get the shape of the 3D mold and allowed to sun dry until it smoothly
withdrew from the mold initially. The clay filter will then be sun-dried for two consecutive days.
Finally, annealing will be performed at around 600 ◦C inside the furnace in an open atmosphere
to harden the clay particles for more stability. Physically, after annealing, it will change color to
reddish-brown and become more hard/stable without any powdery appearance on the surface.
To clarify, the whole procedure is schemed out and shown below.

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CAD Based Design PLA Filament

3D Printer 3D PLA Mold

Earthenware Clay Molding the Clay

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Annealing at 6000 C
Dried Clay filter
 Research Synopsis [BS-ENVIRONMENTAL SCIENCE]

Annealed Clay filter

Nanomaterial Immobilization:

The precursor solution will be prepared by dissolving a nanomaterial in a 1M HNO 3 solution.

The solution will be stirred for about 1 hour to obtain a transparent solution. To grow
nanomaterial films on the substrate, the annealed clay filter will be soaked in the uniformly
mixed precursor solution and allowed for 20 minutes of adsorption. The filter will then be dried
and calcined in a muffle furnace at 150 ◦C, 300 ◦C, and 450 ◦C for 45 min, 30 min, and 90 min,
respectively[8]. The immobilized filter will be named on the name of nanomaterial, and the only
calcined clay filter was named a bare filter.

Characterization Method:

The crystalline structures and phase compositions of the nanomaterial immobilized filter and
bare filter will be investigated using (XRD) X-ray diffraction on an X’Pert Phillips diffractometer.
The morphology of both filters will be analyzed by field-emission scanning electron microscopy
(FESEM) on a ZEISS MERLIN 4248 FESEM instrument. Energy-dispersive X-ray spectroscopy (EDS)
will be performed for the elemental analysis of the immobilized nanomaterial filter. The UV–Vis
diffuse reflectance spectra (DRS) will be recorded on a Shimadzu 2600 UV–Vis
Spectrophotometer equipped with an integration sphere. The energy bandgap (Eg) of the
immobilized nanomaterial filter will be calculated using the Tauc plot method[8].

Photocatalytic Analysis on Batch Scale:

The dye degradation will be initially examined on a batch scale to investigate the photocatalytic
activity and efficiency of the immobilized nanomaterial and bare filters.

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Three white LED lamps will be obtained from the local market, with a maximum emission
spectrum ranging from 400 to 700 nm and an irradiance of 100 W/m2 of each, which will be set
at 50 cm from the 5 ppm IC solution for visible light irradiation. This LED light source selection
avoided any UV irradiation’s influence on photocatalytic performance[24], [25].

The batch-scale study will be performed on a multi-position stirrer, holding, and simultaneously
stirring three beakers (control, immobilized nanomaterial filter, and bare filter), each containing
200 mL solution. In the beginning, the solutions will be stirred in the dark for 60 min to obtain
adsorption-desorption equilibrium before exposure to irradiation. A 3 ml aliquot will be taken at
different irradiation time intervals to analyze the absorbance spectra of the dye solution using a
UV–vis spectrophotometer. The photocatalytic removal of the dye will be estimated by
recording the decrease of the main absorbance peak at 610 nm[26]. The photocatalytic analysis
will also made be at another dye solution concentration (10 ppm) to understand the change in
photocatalytic kinetics at varied dye loading. Moreover, photocatalytic evaluation will be
performed under natural sunlight to compare the results obtained with visible light LED lamps.
The intensity of the sunlight was measured as 94500 lux using a digital lux meter. The study will
be performed between 9:00 a.m. and 5:00 p.m. (the noted temperature varies from 37 ◦C to 42
◦C). Afterward, the same study will be continued on a batch scale for the heavy metals
photodegradation. The photocatalytic degradation of heavy metals will be investigated under
both the LED lamp and sunlight to evaluate the photocatalytic efficiency of the filter.

Photocatalytic Analysis on Semi-batch Scale:

Based on the results obtained from the batch scale study, it will then be decided to evaluate the
scaleup study under natural solar light. Such an upscaled clay filter will be used for immobilized
nanomaterial films by using the previously described similar method. A recirculating semi-batch
scaleup reactor will be designed at a maximum volume of 2 L. With a central upright position of
the filter and the pollutant solution passing in an upside-down direction i.e. for a maximum
free-oxygen and irradiation passage to the immobilized nanomaterial films. The pollutant

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solution will be passed in the up-flow direction from the center channel of the filter, further
generating an effect of the fountain to provide back-flow from every channel/groove set in the
filter design, where possibly the nanomaterial films have immobilized. Photocatalytic studies
will be performed using either dye or heavy metals. The study of the mixed solution will be
designed to replicate wastewater conditions, where the dye and heavy metals pollutants could
be treated simultaneously, and possible mechanisms and changes in kinetics could be explored.
The selection of the optimum 5 ppm concentration of the mixed solution will be based on a
better understanding of the mechanisms and interaction of the immobilized nanomaterial filter
with mixed pollutants and avoiding the bulk loading of both pollutants in a mixed solution. The
solution was recirculated at 100 mL/min using a mini water pump, which connects the inlet and
outlet of the reactor.

Time Frame:

MONTHS
S.N M1 M2 M3 M4 M5 M6 M7 M8 M9
TASK
O Oct Nov Dec Jan Feb Mar Apr May Jun

1st to
1. Literature review
31st
Resource availability 1st to
2.
evaluation 30st
Research topic 1st to
3.
selection 15th
Research synopses
3. 16th 10th
write-up
4. Experimental Research 1st 31st
Data Compilation 1st to
5.
15th

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15th
Data Assessment and
6. to
Analysis
30th
1st to
7. Final thesis write-up
31st
8. Final thesis submission 15th

Conclusion:
The proposed methodology combines 3D structured clay filters with nanomaterials to
revolutionize wastewater treatment. It addresses the limitations of current methods by offering
a systematic approach from designing molds to synthesizing filters, utilizing advanced
characterization techniques. Planned experiments in batch and semi-batch reactors under
different light sources and pollutant concentrations promise practical insights. This innovative
fusion of materials and technology represents a significant leap toward sustainable and effective
water treatment, paving the way for a cleaner future.

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