This document summarizes the synthesis of nickel nanoparticles and their application in removing malachite green dye from water via adsorption. It discusses synthesizing nickel nanoparticles using a chemical reduction method, characterizing the nanoparticles using various techniques, and applying the nanoparticles to remove malachite green dye from water. Key findings include the nickel nanoparticles having spherical shapes ranging from 50-114 nm in size and being able to remove up to 92.8% of malachite green dye from water. Adsorption kinetics and isotherm experiments showed the process followed pseudo-second order kinetics and was best described by the Langmuir isotherm model.

1. SYNTHESIS OF NICKEL NANOPARTICLES AND
APPLICATION IN MALACHITE GREEN DYE
COLOUR REMOVAL USING ADSORPTION
Presented by
M. Bharath Kumar Naik
M.Tech-2nd year
15001D8117
Under the guidance of :
Dr. T. Bala Narasaiah, Professor
Co-guidance of :
Lt.S.Sharada, Assistant professor
Dept. of Chemical Engineering,
JNTUCEA, Ananthapuramu.

2. Contents
 Introduction
 Objectives
 Experimental protocol
 Results and discussion
 Conclusions
 References
 Publications

3. Introduction
 The most significant method in which humans
damage environmental surroundings is by
emitting harmful chemicals into the air and
water.
 Waste water generated from many industries,
consists of a mixture of various dyes.
 Most dyes are complex aromatic structures
which are difficult to be disposed.
 Furthermore, the color in water resources
poses aesthetic problem.
 They represent a relatively large group of
organic chemicals, non-biodegradable, with a
potential toxicity for the aquatic ecosystem.

4. Objectives
 Synthesis of Nickel nanoparticles in batch reactor using chemical
reduction method.
 Characterization by using different techniques like
 Fourier Transform Infra-red spectroscopy,
 X-ray Diffraction,
 Scanning Electron Microscopy,
 UV-visible spectroscopy and
 Dynamic light scattering.
 Application in dye color removal.

5. Synthesis Procedure
0.03M of Nicl2.6H2O + 4.8g
of PVP, dissolved in 480ml of
DW
1.25M of NaOH + 160ml
N2H4.H2O, dissolved in 160
ml of DW
Solution A Solution B
Stirring for 5 min
Mixing
Green White
Sonication for 15 min at 50ᵒ-60ᵒC
Centrifuged for 30min at 1500rpm
Royal blue
Initial solution grey
Washed with DW several times
Collected sample and dry at room temp.
Petri dish
Mortor and
pestle

6. Cont..
+
sonicated
Fig : synthesis of Nickel nanoparticles

7. Functional
groups
Spectra A
Frequency
cm-1
Spectra B
Frequency
cm-1
C-Cl
Stretching
677.95 680.55
C-O
Stretching
1138.37 1220.26
C-C cross
linked
stret.
1554.53 1587.96
C=O
Stretching
1695.25 1640.86
O-H
Stretching
3649.36 3669.28
Fig : FTIR spectra for (a) Ni and (b) Ni-PVP nanoparticles
Results and Discussion
FTIR (Fourier Transform Infra-red spectroscopy) Analysis :

8. XRD (X-Ray diffraction) analysis :
,” Journal of Nanotechnology, Volume 2014 (2014), Article ID 193162.
Fig : XRD pattern of (a) Nickel-PVP and (b) Nickel nanoparticles.
Ni :
JCPDS number : 04-0850
Crystal structure = FCC;
Planes- (111) and (200)
Estimated Crystallite size
= 13.46 nm
Ni-PVP :
JCPDS number : 04-0850
Crystal structure = FCC;
Planes- (111) and (200)
Estimated Crystallite size
= 11.06 nm

9. UV-visible spectroscopy :
Fig b: UV-Visible spectra for Ni nanoparticlesFig a: UV-Visible spectra for Ni-PVP nanoparticles
 Fig a shows clearly seen that the Surface Plasmon Resonance (SPR) of Ni-PVP
nanoparticles centered at 272 nm with an absorbance of 1.429.
 Fig b shows clearly seen that the Surface Plasmon Resonance (SPR) of Ni
nanoparticles centered at 250 nm with an absorbance of 1.124.

10. SEM(Scanning Electron Microscopy) analysis :
(a) (b)
(d)(c)
Fig a: SEM image for Ni-PVP nanoparticles Fig b: SEM image for Ni nanoparticles
 The prepared nanoparticles were found to be spherical and poly-dispersed with
diameters ranging from 50nm to 114 nm (shown in Figure a and b). The average size
for Ni-PVP and Ni nanoparticles was observed to be 72nm and 96nm.

11. Dynamic light scattering :
 Dynamic Light Scattering (DLS) measures size distribution. The particle size
distribution of Ni-PVP and Ni nanoparticles are diameter range 1-10 nm and 10-100
nm as determine on laser light scattering Particle size.
Fig a: Ni-PVP nanoparticles Fig a: Ni nanoparticles

12. Application (Adsorption)
Calibration curve for Malachite Green :
CONC.
OF
DYE(mg/
L)
%ABS
ORBA
NCE
2 0.089
4 0.252
6 0.482
8 0.612
10 0.726
y = 0.0817x - 0.058
R² = 0.9838
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0 2 4 6 8 10 12
%absorbance
concentration (mg/L)
Fig : Malachite green dye of different concentration

13. Various parameters on % Removal of Malachite Green :
1. Effect of Contact Time
TIME ABSORBAN
CE
(ce) %REMO
VAL
10 0.351 5.00 50
30 0.195 3.09 69.1
50 0.053 1.35 86.5
70 0.003 0.74 92.6
0
10
20
30
40
50
60
70
80
90
100
0 20 40 60 80
%Removal
Time (min)
Effect of time for 10ppm
%Removal
Fig : colour removal progress at different time interval

14. 2. Effect of Adsorbent Dosage
TIME ABSORBAN
CE
(ce) %
REMOVAL
10 0.351 5.00 50
30 0.195 3.09 69.1
50 0.053 1.35 86.5
70 0.003 0.74 92.6
TIME ABSORBAN
CE
(ce) %
REMOVAL
10 0.241 3.65 63.5
30 0.173 2.18 78.2
50 0.051 1.33 86.7
70 0.002 0.73 92.7
Effect of Adsorbent dosage (0.05g) on
equilibrium adsorption
Effect of Adsorbent dosage (0.1g) on
equilibrium adsorption
0
10
20
30
40
50
60
70
80
90
100
0 10 20 30 40 50 60 70 80
%Removal
Time (min)
Effect of Adsorbent dosage
0.05
0.1g

15. 3. Effect of pH
TIME ABSORBANCE (ce) %Removal
10 0.241 3.65 63.5
30 0.173 2.18 78.2
50 0.051 1.33 86.7
70 0.002 0.73 92.7
TIME ABSORBANCE (ce) %Removal
10 0.170 2.79 72.1
30 0.152 2.57 74.3
50 0.014 0.88 91.2
70 0.002 0.73 92.7
TIME ABSORBANC
E
(ce) %Removal
10 0.127 2.26 77.4
30 0.124 2.22 77.8
50 0.012 0.85 91.5
70 0.001 0.72 92.8
pH=4 pH=6
pH=8
0
10
20
30
40
50
60
70
80
90
100
0 10 20 30 40 50 60 70 80
%Removal
Time (min)
pH=4
pH=6
pH=8

16. Adsorption Kinetics :
TIME ABSORBANCE (ce) q
10 0.351 5 5.00
30 0.195 3.09 6.91
50 0.053 1.35 8.65
70 0.003 0.74 9.26
Effect of time on adsorption
When experimental “qe” is closer to theoretical “qe” value, we can say
adsorption process either Pseudo-first-order kinetic model (or) Pseudo-
second-order kinetic model.
Fig : Amount of adsorption (q) Vs time (t) curve

17. Pseudo-first-order kinetic model
ln (qe- qt) = lnqe- k1t
TIME ln (qe - qt)
10 1.44
30 0.85
50 -0.49
70 -1
 Slope gives k1 and intercept
gives qe.
Fig : pseudo first order curve

18. Pseudo-second-order kinetic model
TIME t/qt
10 2
30 4.3
50 5.8
70 7.5
 Slope gives qe and intercept
gives k2.
The R2 value is also very high as compared to the pseudo-first-order model.
Thus it is concluded that pseudo-second-order is the best fitting kinetic model.
Fig : Pseudo-second order curve

19. Adsorption Isotherms
Langmuir isotherm model
Cf Cf/qe
5 0.54
3.09 0.33
1.35 0.14
0.74 0.08
J.Hazard. Mater. 154 (2008) 613-622.
 Slope gives al/kl and intercept gives qe.
Fig : Langmuir isotherm model

20. Freundlich isotherm model :
 Slope gives ‘n’ value and intercept
gives Kf value.
lncf lnqt
1.61 1.61
1.13 1.93
0.30 2.15
0 2.25
J.Hazard. Mater. 154 (2008) 613-622.
Fig : Freundlich isotherm model

21. It is observed that both isotherm curves fit well with the adsorption system as their
R2. For fit of experimental isotherm data to Langmuir equation is more close to
1.000 than freundlich equation.
Therefore, the Langmuir isotherm model represents the experimental data better on
the basis of values of regression coefficient.
Langmuir Isotherm
al kl kl/al Rl
(0<Rl<1)
R2
7.199 333.33 46 0.0137 0.999
Freundlich Isotherm
kf (1/n) R2
9.66 -0.373 0.995

22. Conclusions
 Nickel and Nickel-PVP nanoparticles synthesized by using in chemical reduction
method.
 Thus prepared nanoparticles are spherical and polydispersed , The average size of
Ni-PVP and Ni nanoparticles are 72 nm and 92 nm.
 UV-Vis characterization is done for Ni and Ni-PVP nanoparticles, absorbance peak
is observed at 272 nm and 250 nm respectively.
 FTIR study revealed the bonds(O-H ,C=O ,C-C, C-O and C-Cl).
 XRD shows crystallite size of the 11.06 nm and 13.46 nm for Ni-PVP and Ni
nanoparticles respectively .

23.  The particle size distribution of as determine on laser light scattering Particle
size analyzer is 1-10 nm .
 Malachite green (dye) was removed up to 92.8%.
 In adsorption kinetics, pseudo-second-order model R2 value is also very high as
compared to the pseudo-first-order model. Thus it is concluded that pseudo-
second-order is the best fitting kinetic model.
 In adsorption isotherms model both isotherm curves fit well with the adsorption
system as their R2. For fit of experimental isotherm data to Langmuir equation
is more close to 1.000 than freundlich equation.
 Langmuir model represents better values of regression coefficient.
Cont..

24. Conferences
 Presented a paper on “Synthesis of Nickel nanoparticles particles application
in dye degradation” in the national conference on “Recent advances in
Polymer Technology and Industrial Applications(RAPTIA-2017)”, held
during 17th&18th February 2017, at GNITC Hyderabad.
 Paper presented on “Review on dye degradation using nanoparticles”
in the national conference on “pollution control strategies in chemical &
related industries(PCSCRI-2017)”, held during 10th & 11th March 2017,
at SVU Tirupathi.

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