DEPARTMENT OF CHEMICAL ENGINEERING, ACTECH, ANNA UNIVERSITY

FINAL THESIS PRESENTATION FOR PROJECT PHASE 2 (CH5711)

SYNTHESIS OF BIOELECTRODE FOR THE

TREATMENT OF WASTEWATER

Guided by Team members:

Dr. T SANTHOSHINI PRIYA
Assistant Professor, 1. Myleshwari.S (2021303534) - B-Tech Final year
Chemical Engineering
Department of Chemical Engineering,
2. Akshaya .S (2021303005)- B- Tech Final year
Alagappa College of Technology,
Chemical Engineering
Anna University, Chennai 600 025.

APRIL 2025 1
1. INTRODUCTION :

DEPARTMENT OF CHEMICAL ENGINEERING ,ACTECH ,ANNA UNIVERSITY 2

1.1 FLOW CAPACITIVE DEIONIZATION (EMERGING DESALINATION
TECHNOLOGY)

FCDI Concept: Advantages:

Flow Capacitive deionization (FCDI) removes ions FCDI is more energy-efficient and cost-effective
from saline water using static electrical forces. than traditional methods.

It adsorbs ions onto charged electrodes for efficient It produces fewer secondary pollutants, making it
desalination. environmentally friendly.

Applications: Challenges:

FCDI is applicable in industrial water treatment, Challenges include electrode scalability and
agricultural irrigation, and household water efficiency at high salinity levels and Optimizing
purification. electrode materials for better performance is a key
research area.
Types of electrode used :

Synthetic Electrodes includes Activated carbon, carbon aerogels, graphene-based materials.

Bio-based Electrodes includes Biomass-derived carbon (e.g. coconut shell, rice husk).

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1.2 BIOMASS CHOSEN:
The biomass chosen for the synthesis of bio electrode was Sesame oil cake biomass (SCB ). It is a
sustainable, renewable resource derived from sesame oil extraction waste. Rich in carbon, nitrogen,
and fiber, it offers promising applications in bioenergy, bioelectrodes, and environmental
remediation. The properties includes ,
1.Sustainable resource: Derived from sesame oil extraction waste.
2.Rich in nutrients: High in carbon, nitrogen, and fiber.
3.Bioenergy potential: Suitable for bioelectricity and biofuel production.

4.Environmental applications: Useful for soil amendments and pollution remediation.

5.Renewable and biodegradable: Offers a green alternative to fossil fuels.mediation.

FIG 1 SESAME OIL CAKE

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2. LITERATURE REVIEW :

ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

FCDI facilitates continuous operation

1.Exploring flow-electrode capacitive Li, H. et.al., (2025) by enabling material regeneration
deionization: An overview and new external to the cell; improving
insights Chemical Engineering Journal electronic conductivity is key.

2. Capacitive deionization: An Chen et.al., (2025)

Outlines fundamentals and frontiers of
emerging electrosorption technology
CDI for removing U, Cs, Sr, Co, I
for efficient radioactive wastewater Journal of Environmental Chemical
from radioactive wastewater.
treatment Engineering

5
 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

Liu et.al., (2023)

3.Hydrogen production from seawater
Integrated on-line FCDI with alkaline
splitting enabled by on-line flow-
Renewable and Sustainable Energy electrolyzer achieved 100h at 500
electrode capacitive deionization to
Review mA/cm² with 296 mV overpotential.

4.Enhanced desalination performance

Xu et.al., (2023) Nitrogen-doped porous carbon
in flow electrode capacitive
electrode yielded 0.0459 mg/cm²/min
deionization with nitrogen doped
New Journal of Chemistry salt removal at 1.2 V.
porous carbon

6
 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

PratimaDevi Sivasubramanian et.al.,

5. Capacitive deionization and
(2023) This paper recognized and explained,
electrosorption techniques with
a comprehensive and prominent
different electrodes for wastewater
Science and technology of desalting progression in capacitive deionization
treatment applications
and water purification and electrosorption’

6. A Novel Integrated Flow-Electrode

Three-chambered unit achieved cation
Capacitive Deionization and Flow Wang et.al., (2023)
removal, nitrate reduction, and
Cathode System for Nitrate Removal
ammonia generation without added
and Ammonia Generation from Environmental Science & Technology
chemicals.
Simulated Groundwater

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

Yan, B., Zheng, J., Feng, L. et al.,

Basswood-derived free-standing thick
7. Wood-derived biochar as thick (2022)
carbon electrodes were developed for
electrodes for high rate performance
supercapacitors. The optimized
supercapacitors Science and technology of
electrode exhibited good rate
desalination and Purification
performance and stability.

Biochar based soil fertilizers have

Aleksandra Rombel et.al.,(2022).
positive effects on soil properties and
8. Sustainable biochar-based soil
crop yields, reduced the use of
fertilizers and amendments as a new Science and technology of
inorganic fertilizers leading to high
trend in biochar research desalination and purification
yield of safe food

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

Sanchita Bipin Patwardhan et.al.,

9.Recent advances in the application Biochar electrodes in MFCs enable
(2022)
of bio char in microbial wastewater treatment and power
electrochemical cells generation
Environmental Research

Kim et.al., (2021)

10. Enhanced salt removal
FCDI operated up to 2.5 V without
performance of flow electrode
Separation and Purification carbon oxidation or gas generation.
capacitive deionization with high
cell operational potential Technology

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

11. Highly flexible, Self-healable and Jiayi Ai et.al.,(2020). The electrode performed a salt
conductive Poly(vinyl adsorption capacity of about 51
alcohol)/Ti3C2Tx MXene film in Separation and mg/g at a current density of 10 mA g
CDI. Purification Technology -1 and a voltage window of 1 V .

The industrial scale of ED can

Sajjad Al-Amshawee et.al., (2020)
process 2500–3000 mg L of salinity.
12. Electrodialysis desalination for Thus, it has been applied widely to
Chemical Engineering
water and wastewater -A review recover 85% of fresh water from low
Journal
salinity feed, i.e. 3000 mg L of
TDS..

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

13. Water Desalination by Flow- Lim et.al., (2020) .Overlimiting current FCDI achieved
Electrode Capacitive Deionization in >100 mg/m²/s salt removal with
Overlimiting Current Regimes Environmental Science & Technology stable cycling.

SWRO-FCDI selectively removed

14. Feasibility study of reverse Kim et.al., (2020)
osmosis–flow capacitive deionization monovalent ions, producing
(RO-FCDI) for energy-efficient Desalination divalent-rich water for corrosion
desalination control.

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

15.Selective Ion Separation by Zhang et al., (2020) Reviews tailored electrode materials
Capacitive Deionization (CDI) Based and strategies for targeted ion
Technologies: A State-of-the-Art Water Research separation.
Review

16.A Review of Modification of

Carbon Electrode Material in Cheng et al., (2019) Summarizes carbon electrode
Capacitive Deionization enhancements via doping, oxide
RSC Advances modification, and coatings.

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

Flowable electrodes enable important

17.Measurements of the electric Elad B. Halfon et.al., (2019) functionalities not available to static
conductivity of an electrode as it electrodes, but suffer from
transitions between static and Science and technology of significantly lower electric
flowable mode. desalination and purification conductivity, typically of order 1 or
10 mS/cm

Htet Htet et.al.,(2019) The electrosorption efficiency was

18.Biobased polyporphyrin derived
enhanced from 17% to 33% for Pb2+,
porous carbon electrodes for highly
Electrochemistry Communication 12% to 35% for mixed Pb2+ and
efficient capacitive deionization.
Cd2+ ion

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 ARTICLE TITLE AUTHOR AND JOURNAL HIGHLIGHTS

The electrochemical analysis of

Abdul Hai et.al., (2019)
19.Date seeds biomass-derived DSAC-1:1.5 sample showed a higher
activated carbon for efficient specific capacitance of 400 F/g at 10
Science and technology of
removal of NaCl from saline solution mV/s with lower internal resistance
desalination and purification
and good stability.

20.Influence of operating conditions Lutfi Agartana et.al., (2019) Hydrothermally synthesized α-MnO2
and cathode parameters on was selected as the active material in
desalination performance of hybrid Process Safety and Environmental the cathode. Desalination results
CDI systems. Protection, Volume 129. indicate notable dependence of
HCDI performance on the
investigated parameters.

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3. RESEARCH GAP:
1. Non Degradability of the synthetic electrodes used in waste water treatment.
2. Lack of sustainability in the synthetic electrode used CDI technology
3. High time consumption for regenerating the static electrode(which adsorbs ions from water and gets
saturated)
4. Limited research on synthesis of bio-electrode for waste water treatment.

4. OBJECTIVE:
1. To synthesis Nitrogen doped chitosan functionalised KOH Activated carbon (N – CS KOH AC )
BioElectrode from SCB by hydrothermal treatment using potassium hydroxide, chitosan polymer
grafting ,nitrogen doping.
2. To characterize the obtained N- CS KOH- AC using TGA, SEM, XRD, cyclic voltammetry,
Electrochemical impedencce spectroscopy
3. To prepare the Bio-Flow electrode by dispersing N –CS KOH- AC in electrolyte solution.
4. To utilize the produced Bio-Flow electrode for the application of CDI.
5. To optimize the parameters such as feed concentration, electrolyte concentration, feed and electrode flow
rates, applied voltage, feed to electrolyte concentration ratio.

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5. MATERIALS AND METHODS:
5.1 CHEMICALS AND MATERIALS USED

1. Sesame oil cake biomass 6. Melamine(C3H6N6) 12. Ultra sonicator

2. Potassium Hydroxide 7. AceticAcid(CH3COOH) 13. Oven
(KOH) 8. Distilled water 14. Tubular furnace
3. Hydrochloric Acid (HCl) 9. Ethanol 15. Boat and tray
4. SodiumHydroxide(NaOH) 10. pH meter 16. crucible and beakers.
5. Chitosan(C6H11NO4)​n 11. Magnetic Stirrer 17. Thermometer
5.2 SESAME OIL CAKE PRE PREPARATION:
SCB sample of 1Kg was crushed in a jaw crusher to obtain
coarse particles of SCB and then again crushed in a mortor and
pestle to obtain fine particles of SCB.

The SCB fine particles were sieved to obtain particles ranging

in size from 0.5-2 mm.

The crushed SCB particles were washed using distilled water

until impurities (dust or any other visible contaminants) were FIG 2 SESAME OIL CAKE PARTICLES PREPARATION

removed.
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 5.3 SYNTHESIS OF N DOPED CHITOSAN FUNCTIONAL ISED KOH ACTIVATED
CARBON (N- CS KOH AC )

Impregnation of KOH in SCB particles by magnetic stiring

Hydrothermal treatment of impregnated solution using

Teflon autoclave in Oven at 180° C to get KOH BC
Fig 3 SCB KOH SOLUTION

Thermal Activation of KOH B using tubular furnace at 800°

Fig 3.1 KOH BC
C to get KOH AC

Chitosan polymer grafting of KOH AC by stirring and drying

to get CS KOH AC Fig 4 KOH AC

Fig 6 N CS KOH AC
Melamine derived Nitrogen doping by grinding and thermal
treatment to get N – CS KOH AC

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Fig 5 CS KOH AC
6. FLOW CAPACITIVE DEIONIZATION (FCDI) :
6.1 EXPERIMENTAL SETUP:
Cell Design Operation Mechanism
The FCDI cell consists of
A DC power supply applies
flow electrode channels
voltage to the system, enabling
made from epoxy-
ion adsorption on the flow
impregnated graphite
electrodes.CV
plates

Performance Evaluation:
Electrode Used:
Synthesized N-CS Desalination performance is
KOH AC is dispersed assessed by measuring
in the electrolyte changes in feed salt water
solution to form flow concentrations with a
electrode conductivity meter.

Fig 7 FCDI EXPERIMENTAL SET-UP

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FLOW BIO-ELECTRODE PREPARATION

• Preparation of Dispersant solution by dissolving 1-2 grams of poly vinyl alcohol in 100 mL DI water by
magnetic stirring by maintaining temperature at 60 -80 degree celcius and let it cool.

• Preparation of carbon suspension by adding 1000 ppm NaCl solution to the dispersant solution while stirring
then slowly adding the N-CS KOH-AC and carbon black in the ratio. Of 90:10 (by weight).

• Vigorous stirring of the mixture is done to avoid clumping .

• For homogenization, at first it is mixed using magnetic stirrer for 30 -60 mins followed by ultrasonication
for 15-30 mins .

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 6.2 ADSORPTION ISOTHERM STUDY OF FCDI:
Adsorption isotherms describe the equilibrium relationship between the amount of adsorbate retained on an
adsorbent surface and its concentration in the solution at a constant temperature.

Two widely used isotherm models in adsorption studies are

Langmuir isotherm : assumes monolayer adsorption Freundlich isotherm : assumes multilayer adsorption

•q = Amount of adsorbate adsorbed per unit mass of •q = Amount of adsorbate adsorbed per unit mass of
adsorbent (mg/g) adsorbent (mg/g)
•Q = Maximum monolayer adsorption capacity •k = Freundlich adsorption constant ((mg/g)(L/mg)
(mg/g) •n = Heterogeneity factor, indicating surface
•C = Equilibrium concentration of adsorbate in heterogeneity and adsorption intensity.
solution (mg/L) •C = Equilibrium concentration of adsorbate in
•K​= Langmuir adsorption constant (L/mg) solution (mg/L)

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7. RESULTS AND DISCUSSION :
7.1 THERMOGRAVIMETRIC ANALYSIS:
The primary substance (SCB) was heated at 10 K per minute. The
outcomes of this analysis are visually presented in belowgraph. Within
the graphical representation , discrete stages in the thermogravimetric
analysis (TGA) are evident:

PHASE TEMPERATURE INTREPRETATION

RANGE
I 100°C to 210°C. preliminary drying process that
eliminates stored moisture and
evaporates light components
II 100–240°C. degassing of biomass
III 240°C -700°C the decomposition of lignocellulosic
compounds

Fig 8 TGA for SCB

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7.2 PROXIMATE ANALYSIS : 7.3 UV SPECTROSCOPY:
Proximate analysis had been done for the sesame oil
cake biomass and the results are found to be as
mentioned below in table

COMPOUNDS PERCENTAGE PRESENT

Moisture content 8.7% Fig 9 UV VIS SPECTROSCOPY

Volatile matter 11.92% • The observed n → π* transition peaks in the 280-310

Ash content 7.84% nm range indicate the presence of functional groups
such as C=O, N-H, and hydroxyl (-OH) in chitosan.
Percent Carbon 71.54 %

• The slight red shift (~310 nm) and increased

TABLE 1 PROXIMATE ANALYSIS
absorbance intensity from CS < Ultrasonicated CS-
AC < Final CS-AC suggest enhanced π-π interactions
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and structural modifications due to grafting.
7.4 XRD ANALYSIS :

The XRD plot for synthesized activated carbon from KOH-AC, CS KOH AC and N CS KOH AC were
mentioned in the figure.

SAMPLE CRYSTALITE INTREPRETATION

SIZE ( nm)
KOH AC 10.1 Broadest peak; indicates
smallest crystallite size and
highest amorphous nature.
CS KOH AC 13.4 Moderate peak sharpness;
suggests improved ordering and
larger crystallites.
N CS KOH 20.1 Sharpest peak; reflects largest
AC crystallite size and enhanced
graphitic structure.

Fig 10 XRD for KOH-AC , CS KOH AC , N CS KOH AC TABLE 2 XRD ANALYSIS

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7.5 ELECTROCHEMICAL CHARACTERIZATION:

7.5.1 CYCLIC VOLTAMMETRY(CV): • The average specific capacitance value of KOH-AC for
different scan rates 5mV/s, 30mV/s, 50mV/s and 70mV/s
is 157.6F/g.

• The curves exhibit increasing current response with

increasing scan rates, indicating a capacitive or faradaic
behavior which inturn suggests a good charge storage
properties.
SCAN RATE SPECIFIC
mv/s CAPACITANCE
F/g
5 138

10 143

20 155

50 172

Fig 11 CYCLIC VOLTAMMOGRAM OF N CS KOH AC

100 180
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TABLE 3 CV DATA
7.5.2 ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY(EIS):

N CS KOH AC •N CS KOH AC shows a reduced real impedance range

implying a lower charge transfer resistance and improved
conductivity.

•The decreased impedance in N CS KOH AC, with a

resistivity of 15.16 Ω·cm, suggests better electrochemical
performance.

Fig 12 Nyquist plot ( EIS - CS KOH AC )

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7.6. FCDI EXPERIMENTAL RESULTS:
Feed(NaCl) flow rate : 20ml/min, Voltage : 1.2 V
Flow Electrode ( N- CS KOH AC ) Loading : 7 % , feed (NaCl)
concentration : 1000 ppm – 2500 ppm

Fig 13 Desalination efficiency of N- CS KOH AC

at different concentration
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Voltage applied : 0.8-1.2 V , Feed (NaCl) flow rate : 20ml/min
Feed (NaCl) Concentration :2000 mg/L , Flow Electrode (N-CS KOH AC) Loading : 7 %

Fig 14 Desalination efficiency of N- CS KOH AC at

different applied voltages of 0.8, 1.0 and 1.2 V in 2000
mg L-1 of NaCl solution

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Feed (NaCl)flow rate : 20ml/min, Feed (NaCl)Concentration :2000 mg/L
Voltage :1.2 V, Flow Electrode (N-CS KOH AC ) loading - 5- 10 %

Fig 15 Desalination efficiency of N- CS KOH AC at

different carbon loading of 5 ,7, and 10 weight % of
carbon as Flow Electrode in 2000 mg / L of NaCl
solution.

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Flow Electrode ( N- CS KOH AC ) loading : 7% , Feed (NaCl) Concentration :2000 mg/L
Voltage :1.2 V, Feed(NaCl)flow rate : 18-28ml/min

Fig 16 Desalination efficiency of N- CS KOH

AC at different flow rate of 18,20,25 and
28ml/min in 2000 mg / L of NaCl solution at 1.2
V applied Voltage. 29
7.6.1 ADSORPTION ISOTHERM STUDY OF FCDI RESULTS:

Fig 17 Langmuir isotherm graph fig 18 Freundlich isotherm graph

Adsorption isotherm studies were done for the datas obtained from the optimum parameters 1.2 V , 2000 mg/L
feed concentration, 20ml/ min Feed flow rate and 7 % carbon loading.

Langmuir isotherm shows a higher R^2 value (0.9931) compared to the Freundlich isotherm R^2 (0.856), it can
be concluded that the adsorption process follows the Langmuir model more closely

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8. CONCLUSION:

1. Nitrogen-doped, chitosan-functionalized KOH-activated carbon (N-CS KOH AC) bioelectrode synthesized

from sesame oil cake biomass (SCB) offers an environmentally friendly solution for wastewater treatment.

2. Characterization and Electrochemical Properties:

1. High fixed carbon content (71.54%) and functional groups confirmed via UV-Vis spectroscopy.
2. Crystallite size increased from 10.1 nm (KOH AC) to 20.1 nm (N-CS KOH AC) with XRD analysis.
3. Cyclic Voltammetry (CV) showed a specific capacitance of 157.6 F/g.
4. Low resistivity (15.16 Ω·cm) confirmed excellent conductivity via Electrochemical Impedance
Spectroscopy (EIS).
3. Optimal FCDI Performance:
1. Salt adsorption capacity (SAC): 13.7 mg/g, salt adsorption rate (ASAR): 0.63 mg/g/min.
2. Maximum desalination efficiency of 67%.
3. Langmuir isotherm fit (R² = 0.9931) supports monolayer ion adsorption.

4. The N-CS KOH AC bioelectrode demonstrated high efficiency, improved electrochemical performance, and
sustainability, making it a promising candidate for future desalination and wastewater treatment applications.

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THANK YOU

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