College of Engineering Studies

Minor Project Presentation

Extraction & Characterization of Silica from Rice Husk Ash

Department of Chemical Engineering

1 Mentor : Dr. Anupama Mishra, Department of Chemical Engineering

Submitted By:
Shreyanshu Agrawal
Nikita Goel
Satyam Dixit
Tanya Kathuria
Shaorya Yadav
 Methodology
2
 Basic steps in the preparation of precipitated Silica are:

1.Obtaining 3.Preparation of
2.Dissolution of Silica from silicate
Silica from rice
Silica in alkali solution
husk
 Methodology
 Silica extraction
3
Rice husk ash
+ Filtration using
Filtrate (Sodium
NaOH Solution Whattman filter
Silicate solution)
(90-95°C) paper

Sodium Silicate
solution titrated
with
4% H2SO4
Titration
(stopped
at 3-4 pH) Centrifugation
(2500 rpm)
Drying in hot
air oven to
produce silica
gel
 Methodology
4

Fig.4 Drying of Rice Husk Fig.5 Washing and Filtering Fig.6 Washed Rice Husk
 Methodology : Proximate Analysis
5

Oven

Fig.7 Sample in Crucible Fig.8 Moisture Approximation

 Methodology : Proximate Analysis
6

Fig.9 Desiccator Fig.10 Volatile Matter

 Methodology : Proximate Analysis
7

Fig.11 Muffle Furnace (Ash Content) Fig.12 Ash Remains

 Result : Proximate Analysis
8

Sample : Rice Husk

Weight : 5 g

Test Percentage
Moisture Content 3%
Volatile Matter 60.2%
Ash Content 25.5%
Fixed Carbon 11.3%

Note : This study was done on dry basis.

• The scaling up of the ash content was done with rice husk
• The ash contains mainly silica along with some other components.
• Our next checkpoint was to dissolve silica(present in ash) in NaOH
solution of optimum concentration.
 Methodology
9

Fig.13 Rice Husk in Muffle Furnace Fig.14 Ash Obtained for further
experiments
 Preparation of Silica Gel
10

Fig.15 Ash Fig.16 NaOH Crystals Fig.17Ash +NaOH Solution

 Preparation of Silica Gel
11

Fig.18 Optimum Solution Fig.19 Filtrate (Na2SiO3) Fig.20 Titration

 Preparation of Silica Gel
12

Gel Formation : Magnetic

Stirring
 Preparation of Silica Gel
13

Starting of Gel Formation Change of pH of Gel Ageing Gel for 18 hours

 Preparation of Silica Gel
14

Fig.21 Centrifugation Fig.22 V-Mix Apparatus Fig.23 Settled Silica Gel

 Preparation of Silica Gel
15

Fig.24 Silica Gel in Petri dish Fig.25 Dried Gel in Hot Air Oven
 Study of Na2SiO3 Preparation
16
S. NaOH concentration (w/v Silica extracted (%)
No. %)
1 1.5 52

P e r c e n t a g e o f S ilic a E x t r a c t e d
2 2 71.83
3 4 76.33

Silica extracted
90
80 76.33
71.83
70
60 52
50
40
30
20
10
0
1 1.5 2 2.5 3 3.5 4 4.5

NaOH Concentration
 Characterization & Expected Outcomes
17
• Characterization and Analysis
 XRD
 FTIR
 SEM
 BET Surface Area
 X-Ray Diffraction Analysis
18 SiO2 gel sample
 X-Ray Diffraction Analysis
19
• Comparison with Literature

Trisyl 300
 X-Ray Diffraction Analysis
20

• Comparison with Literature

 The peaks reveal the formation of particles having the reflection from (100), (110), (102), (111),
(200) and (201 planes, at 2θ values 20.861 39.470°, 40.296°, 42.457°, and 45.800 the sample
synthesized via sol-gel route.
 Colour : Colourless
 a =b= 4.91 Ǻ ; c = 5.40 Ǻ
 Structure : Material formed is having hexagonal crystal structure and is primitive lattice with
lattice parameters a=b=4.913 Å and c=5.405 Å .
 The 2 θ value corresponding to the lattice was found to be 27.17 ° , which was found to be
consistent with the literature.
 FT-IR Study
21 SiO2 gel sample

100.0

95

90 573

85 FT IR
80

75

70

65

60

55
795
50
%T
45

40

35 1641 462

30

25 961

20

15
3461
10 1081

0.0
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0
cm-1
 FT-IR Study
22
Comparison with Literature
 FT-IR Analysis
23

 Comparison with Literature

• The key chemical groups present in Silica sample and Trisyl 300 were identified by respective FTIR spectra.
• In general, the FTIR spectra of Trisyl 300 was sharper, had lower noise and higher intensity when compared to
that of RHSG. A broad band between 2,800 and 3,750 cm -1 indicates surface OH groups (Adhikari et al 1994,
Yates et al 1997).
• This stretch is due to the silanol OH groups and the adsorbed water bound to the silica surface by hydrogen
bonds. A sharper peak or shoulder at »3,700 cm-1 in both spectra is mainly due to the isolated silanol groups
that are not hydrogenbonded to other silanols.
• The bending vibration peak for H-OH is shown at 1,650 cm-1 (Proctor et al 1995) and is more pronounced in
the spectra of Trisyl 300. The bands at 800, 1,080, and 1,220 cm -1 which are more visible in the Trisyl 300
could be attributed to the network vibration modes indicating a highly condensed gel network.
• The peak between 1250-1400 cm-1 in the Trisyl 300 spectra is due to the structural siloxane bonds (Si-O-Si)
and is evident to a lesser degree in the RHSG spectra.
 SEM Analysis
24
 SEM Analysis
25
• Comparison with Literature
 Trisyl 300 particles seemed to be more uniform in appearance
with sizes ranging from <5 to 25 mm.
 These observations are consistent with our pore diameter results
wherein RHSG particles were found to be larger than Trisyl 300
particles.
 The lack of uniformity in the RHSG particle size is a result of the
laboratory grinding process which differs from the industrial
process for commercial silica gel products.
 References
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• Y. Hamzeh, K. P. Ziabari, J. Torkaman, A. Ashori and M. Jafari, J. Environ. Manage., 2013, 117, 263–
267,
• Tribe NCfS. Utilization and recycling of agricultural wastes/byproducts: A country Report. New
Delhi Department of Science and Technology, 1974
• T. Madhiyanon, P. Sathitruangsak, S. Soponronnarit, Co-combustion of rice husk with coal in a
cyclonic fluidized-bed combustor (w-FBC). Fuel 2009; 88:132–8.
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