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E nvironment A sia
The international journal published by the Thai Society of Higher Education Institutes on Environment

Available online at www.tshe.org/EA
EnvironmentAsia 5 (special issue) (2013) 151-155

Effect of operating parameters on the yield of Activated
Carbon prepared from Karanja seed shells
Prof. V.N. Ganvir, Akash Dhobale
Department of Petroleum Refining & Petrochemical Technology,
Laxminarayan Institute of Technology, Rashtrasant Tukdoji Maharaj Nagpur University,
Bharat Nagar, Amravati Road, Nagpur- 440033.
Email: vnganvirlit@gmail.com, aks2015@gmail.com
Abstract
Solid waste disposal has become a major problem in vegetable oil mill / refinery.
Either it has to be disposed safely or use for the recovery of valuable materials. Karanja
oil has medicinal value and widely used in soaps, leather tanning and ‘attar’. Nowadays
Karanja oil is used for preparation of biodiesel. Karanja shells remains as waste.
Therefore, activated carbon was prepared from Karanja shells which are thrown out as
a waste from Karanja oil mill and have no further use after seed removal. A study of the
effect of the preparation conditions on the yield of activated carbon prepared from
Karanja seed shells was made using H3PO4 as an activating agent. The Karanja shells
were washed, dried, digested and carbonized at carbonization temperature varying
from 4000C to 6000C with carbonization time varying from 10 min to 30 min and acid
concentration varying from 0N to 30N. The effects of carbonization temperatures
ranging from 400°C to 600°C and acid concentration ranging from 12N to 20 N with
nitrogen purge rate of 5 lit/Hr were studied. Proximate analysis of feed was done.
Keywords: Activated carbon, Karanja seed shell, yields of activated carbon.

1. Introduction
In the last few years interest &
activity have grown up around the globe
to find a substitute of fossil fuel. According
to Indian scenario the demand of
petroleum product like diesel is increasing
day by day hence there is an urgent need
to find a solution. Biodiesel has become
more
attractive
because
of
its
environmental benefits and fact that it is
made up of renewable resources.
Under Indian condition only nonedible oil can be used as biodiesel which
are produced in appreciable quantity and

can be grown in large scale on noncropped marginal lands and waste lands.
Non-edible oils like Jatropha, Karanja and
Mahua contain 30% or more oil in their
seed, fruit or nut. The Karanja oil has a
bitter taste and a disagreeable aroma, thus
it is not considered edible. [1][2][3]
In India, the Karanja oil is used as a
fuel for cooking and lamps. The Karanja oil
is also used as a lubricant, water-paint
binder, pesticide, and in soap making and
tanning industries. The Karanja oil is
known to have value in herbal medicine
for the treatment of nausea, rheumatism,
as well as human and animal skin

151
E nvironment A sia
The international journal published by the Thai Society of Higher Education Institutes on Environment

diseases. It is effective in enhancing the
pigmentation of skin affected by
Leucoderma. The oil of Pongamia is also
used as a substitute for diesel. [4]
The methods used for activated
carbon synthesis are physical activation
and chemical activation. Furthermore, the
temperature range used in chemical
activation is lower in comparison to that
used in physical activation. Phosphoric
acid is selected as the activating agent
instead of zinc chloride so as not to
aggravate environmental pollution by
contamination with zinc compounds. The
main objective of this research is to
prepare activated carbon from Karanja
seed shells.
2. Experimental
2.1. Pre-treatment
Karanja shells were obtained from
the vegetable oil mill and the seeds were
taken out from the shells. The shells were
repeatedly washed with distilled water to
remove residues and dried at 60°C for 4
hours to reduce moisture content. The
dried shells were crushed with a
commercial miller into small pieces.

Available online at www.tshe.org/EA
EnvironmentAsia 5 (special issue) (2013) 151-155

After drying, the samples were
placed in crucibles and into a high
temperature furnace for carbonization.
The colonization process was carried out
in an inert atmosphere using nitrogen gas
with nitrogen purge rate of 5 lit/hour for
time 10, 15, 20 min. After adjusting the
nitrogen flow, the furnace is started. The
carbonization temperatures used were
4000C, 4500C, 5000C, 5500C and 600°C.
2.4. Proximate analysis of feed
2.4.1. Determination of moisture content.
1.0g of the dried sample was
weighed in a crucible. The crucibles were
placed in an oven and dried at 105ºC to
constant weight for 1 hour as per
(ASTMD-3173). The percentage moisture
content (% MC) was computed as follows:
Moisture content (%) = [(W2-W3) / (W2W1)] x 100
Where,
W1 = weight of crucible, gm.
W2=weight of crucible + sample, gm.
W3=weight of crucible + sample after
heating, gm.
2.4.2 Determination of volatile matter.

2.2. Impregnation
Impregnation of Karanja pods were
done with (4, 8, 12, 16, 20, 24, 28) N
phosphoric acid. 5 gm of sample is
impregnated with appropriate volume of
phosphoric
acid
of
different
concentration. The impregnation process
was performed at temperature 30ºC for
24 hours in a Petri dish. The impregnated
sample was washed with distilled water
till we get 7 pH. The sample was dried in
an oven at 1000C for 2 hrs.
2.3. Carbonization

Loss in weight was reported as
volatile matter on a percentage basis. The
difference in weight due to loss of volatile
was taken as the total volatile matter
present in the biomass.
Volatile matter (%) = [(W5-W6) / (W5W1)] x 100.
Where,
W4 = weight of the crucible + weight of
the sample before oven drying, gm.
W5=weight of the crucible + weight of the
sample before keeping in muffle furnace,
gm.

152
E nvironment A sia

Available online at www.tshe.org/EA
EnvironmentAsia 5 (special issue) (2013) 151-155

The international journal published by the Thai Society of Higher Education Institutes on Environment

W6=weight of the crucible + weight of
sample after keeping in muffle furnace,
gm.
2.4.3. Determination of ash content.
The residual carbon in the crucible
is heated without lid in a muffle furnace at
750ºC for half an hour for (ASTMD-3174).
Heating, cooling and weighing was
repeated, till a constant weight was
obtained. The residue was reported as ash
on a percentage basis.
Ash content, (%) = [(W8-W9) / (W7-W1)]
x 100.
Where,

W7 = weight of the crucible + weight of
the sample before oven drying, gm.
W8= weight of the crucible + weight of the
sample before keeping in muffle furnace,
gm.
W9=weight of crucible + weight of the
sample after keeping in muffle furnace,
gm.
Table 1. Proximate analysis of Karanja
seed shells
Test
Volatile content
Moisture content
Ash content

Karanja seed shell
(%)
60
4.5
3

3. Results and Discussion
3.1. Effect of concentration of phosphoric acid on the yield of activated carbon
Variance of acid concentration by
keeping
carbonization
time
and
carbonization
temperature
constant,
taken for 5 different temperatures 4000C,
4500C, 5000C, 5500C and 600°C. Figure 1
shows that the yield increases as the

concentration of H3PO4 impregnating
solution increases. It approached an
optimum point at 16N of H3PO4 with
75.18 % yield. A further increase in
loading H3PO4 led to a decrease in yield
for all the temperatures considered.

80
70

60
400 deg centi.

40

450 deg cent.

30

500 deg centi.

20

550 deg centi.

10

Yield %

50

600 deg centi.

0
0

5

10

15

20

25

30

H3PO4 Normality

Figure 1. Effect of concentration of phosphoric acid on the yield of activated carbon.
3.2. Effect of carbonization temperature on activated carbon yield

153
E nvironment A sia

Available online at www.tshe.org/EA
EnvironmentAsia 5 (special issue) (2013) 151-155

The international journal published by the Thai Society of Higher Education Institutes on Environment

Carbonization temperature plays a
significant role on the activated carbon
yield. As we increase the temperature
from 4000C to 6000C by keeping
carbonization time and acid concentration
constant, it is taken for 3 different acid
concentrations. The variation of activated
carbon
yield
with
carbonization
temperature is shown in fig 2. For all 3
impregnation concentrations, it was found
that the yield of activated carbon

decreases with increasing temperature
from 4500C onwards.
This was due to the loss of most of the
volatile matter and loss of phosphate
compounds. Under high activation
temperature
yield
decreased
tremendously as a considerable amount of
phosphate compounds volatised when the
carbonization temperature is above
450°C.

80
70

Yield %

60
50
40

12 N H3PO4

30

16 N H3PO4

20

20 N H3PO4

10
0
350

400

450

500

550

600

650

Temp.

Figure 2.Effect of carbonization temperature on the yield of Activated Carbon.
3.3. The effect of carbonization time on activated carbon yield
Variation of carbonization time by keeping
carbonization temperature and acid
.

concentration constant, for three different
temperature
4500C,
5000C,
5500C

80

70

Yield %

60
50
40

400 deg centi.

30

450 deg centi.

20

500 deg centi.

10
0
0

5

10

15

20

25

30

35

Time (min)

Figure 3. Effect of carbonization time on the yield of Activated Carbon.

154
E nvironment A sia
The international journal published by the Thai Society of Higher Education Institutes on Environment

As we increase the carbonization time
from 10 min and onwards for same
temperature the yield of activated carbon
decreases with increasing time. The
optimum carbonization time for the
preparation of the adsorbent was found to
be 10 min.
4. Conclusion
Karanja seed shells can be used as a
precursor in the preparation of activated
carbon with good surface area around 344
m2/gm. However, an attempt has been
made in this work to study the minimum
and optimum carbonization temperature
of Karanja seed shell between the ranges
of 400-6000C. The optimized conditions
(Activation concentration, temperature
and time) were all studied. Optimized
condition for the preparation of activated
carbon is found to be 16N of acid
concentration, carbonization temperature

Available online at www.tshe.org/EA
EnvironmentAsia 5 (special issue) (2013) 151-155

4500C and carbonization time 10 min, as
per yield point of view.
References
1. Subramanian, K.A., Singal, “Utilization of
liquid biofuels in automotive diesel
engines, Biomass and Bio energy”, 2005;
29:65-72.
2. Azam A.M., and Nahar N. M., “Prospects
and potential of fatty acid methyl esters of
some non-traditional seed oil for use as
biodiesel in India”. Biomass and
Bioenergy.2005; 29:293-302.
3. Tiwari S, Saxena M, Tiwari SK “Mahua
oil based resins for the high-temperature
curing of fly ash coatings”. Journal of
applied polymer Science.2003; 87 (2):
110-120.
4. Ashish S. Saksule, “adsorbents from
Karanja seed oil cake and applications”.
International
Journal
of
Chemical
Engineering and Applied Sciences, ISSN
2278 –1366 Original Article, 2012.

Received 16 November 2013
Accepted 3 December 2013
Correspondence to
Mr. Akash Dhobale
Department of Petroleum
Refining & Petrochemical
Technology,
Laxminarayan Institute of
Technology, Nagpur- 440033
E-mail: aks2015@gmail.com

155

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Adsorbent preparation from Karanja seed shells

  • 1. E nvironment A sia The international journal published by the Thai Society of Higher Education Institutes on Environment Available online at www.tshe.org/EA EnvironmentAsia 5 (special issue) (2013) 151-155 Effect of operating parameters on the yield of Activated Carbon prepared from Karanja seed shells Prof. V.N. Ganvir, Akash Dhobale Department of Petroleum Refining & Petrochemical Technology, Laxminarayan Institute of Technology, Rashtrasant Tukdoji Maharaj Nagpur University, Bharat Nagar, Amravati Road, Nagpur- 440033. Email: vnganvirlit@gmail.com, aks2015@gmail.com Abstract Solid waste disposal has become a major problem in vegetable oil mill / refinery. Either it has to be disposed safely or use for the recovery of valuable materials. Karanja oil has medicinal value and widely used in soaps, leather tanning and ‘attar’. Nowadays Karanja oil is used for preparation of biodiesel. Karanja shells remains as waste. Therefore, activated carbon was prepared from Karanja shells which are thrown out as a waste from Karanja oil mill and have no further use after seed removal. A study of the effect of the preparation conditions on the yield of activated carbon prepared from Karanja seed shells was made using H3PO4 as an activating agent. The Karanja shells were washed, dried, digested and carbonized at carbonization temperature varying from 4000C to 6000C with carbonization time varying from 10 min to 30 min and acid concentration varying from 0N to 30N. The effects of carbonization temperatures ranging from 400°C to 600°C and acid concentration ranging from 12N to 20 N with nitrogen purge rate of 5 lit/Hr were studied. Proximate analysis of feed was done. Keywords: Activated carbon, Karanja seed shell, yields of activated carbon. 1. Introduction In the last few years interest & activity have grown up around the globe to find a substitute of fossil fuel. According to Indian scenario the demand of petroleum product like diesel is increasing day by day hence there is an urgent need to find a solution. Biodiesel has become more attractive because of its environmental benefits and fact that it is made up of renewable resources. Under Indian condition only nonedible oil can be used as biodiesel which are produced in appreciable quantity and can be grown in large scale on noncropped marginal lands and waste lands. Non-edible oils like Jatropha, Karanja and Mahua contain 30% or more oil in their seed, fruit or nut. The Karanja oil has a bitter taste and a disagreeable aroma, thus it is not considered edible. [1][2][3] In India, the Karanja oil is used as a fuel for cooking and lamps. The Karanja oil is also used as a lubricant, water-paint binder, pesticide, and in soap making and tanning industries. The Karanja oil is known to have value in herbal medicine for the treatment of nausea, rheumatism, as well as human and animal skin 151
  • 2. E nvironment A sia The international journal published by the Thai Society of Higher Education Institutes on Environment diseases. It is effective in enhancing the pigmentation of skin affected by Leucoderma. The oil of Pongamia is also used as a substitute for diesel. [4] The methods used for activated carbon synthesis are physical activation and chemical activation. Furthermore, the temperature range used in chemical activation is lower in comparison to that used in physical activation. Phosphoric acid is selected as the activating agent instead of zinc chloride so as not to aggravate environmental pollution by contamination with zinc compounds. The main objective of this research is to prepare activated carbon from Karanja seed shells. 2. Experimental 2.1. Pre-treatment Karanja shells were obtained from the vegetable oil mill and the seeds were taken out from the shells. The shells were repeatedly washed with distilled water to remove residues and dried at 60°C for 4 hours to reduce moisture content. The dried shells were crushed with a commercial miller into small pieces. Available online at www.tshe.org/EA EnvironmentAsia 5 (special issue) (2013) 151-155 After drying, the samples were placed in crucibles and into a high temperature furnace for carbonization. The colonization process was carried out in an inert atmosphere using nitrogen gas with nitrogen purge rate of 5 lit/hour for time 10, 15, 20 min. After adjusting the nitrogen flow, the furnace is started. The carbonization temperatures used were 4000C, 4500C, 5000C, 5500C and 600°C. 2.4. Proximate analysis of feed 2.4.1. Determination of moisture content. 1.0g of the dried sample was weighed in a crucible. The crucibles were placed in an oven and dried at 105ºC to constant weight for 1 hour as per (ASTMD-3173). The percentage moisture content (% MC) was computed as follows: Moisture content (%) = [(W2-W3) / (W2W1)] x 100 Where, W1 = weight of crucible, gm. W2=weight of crucible + sample, gm. W3=weight of crucible + sample after heating, gm. 2.4.2 Determination of volatile matter. 2.2. Impregnation Impregnation of Karanja pods were done with (4, 8, 12, 16, 20, 24, 28) N phosphoric acid. 5 gm of sample is impregnated with appropriate volume of phosphoric acid of different concentration. The impregnation process was performed at temperature 30ºC for 24 hours in a Petri dish. The impregnated sample was washed with distilled water till we get 7 pH. The sample was dried in an oven at 1000C for 2 hrs. 2.3. Carbonization Loss in weight was reported as volatile matter on a percentage basis. The difference in weight due to loss of volatile was taken as the total volatile matter present in the biomass. Volatile matter (%) = [(W5-W6) / (W5W1)] x 100. Where, W4 = weight of the crucible + weight of the sample before oven drying, gm. W5=weight of the crucible + weight of the sample before keeping in muffle furnace, gm. 152
  • 3. E nvironment A sia Available online at www.tshe.org/EA EnvironmentAsia 5 (special issue) (2013) 151-155 The international journal published by the Thai Society of Higher Education Institutes on Environment W6=weight of the crucible + weight of sample after keeping in muffle furnace, gm. 2.4.3. Determination of ash content. The residual carbon in the crucible is heated without lid in a muffle furnace at 750ºC for half an hour for (ASTMD-3174). Heating, cooling and weighing was repeated, till a constant weight was obtained. The residue was reported as ash on a percentage basis. Ash content, (%) = [(W8-W9) / (W7-W1)] x 100. Where, W7 = weight of the crucible + weight of the sample before oven drying, gm. W8= weight of the crucible + weight of the sample before keeping in muffle furnace, gm. W9=weight of crucible + weight of the sample after keeping in muffle furnace, gm. Table 1. Proximate analysis of Karanja seed shells Test Volatile content Moisture content Ash content Karanja seed shell (%) 60 4.5 3 3. Results and Discussion 3.1. Effect of concentration of phosphoric acid on the yield of activated carbon Variance of acid concentration by keeping carbonization time and carbonization temperature constant, taken for 5 different temperatures 4000C, 4500C, 5000C, 5500C and 600°C. Figure 1 shows that the yield increases as the concentration of H3PO4 impregnating solution increases. It approached an optimum point at 16N of H3PO4 with 75.18 % yield. A further increase in loading H3PO4 led to a decrease in yield for all the temperatures considered. 80 70 60 400 deg centi. 40 450 deg cent. 30 500 deg centi. 20 550 deg centi. 10 Yield % 50 600 deg centi. 0 0 5 10 15 20 25 30 H3PO4 Normality Figure 1. Effect of concentration of phosphoric acid on the yield of activated carbon. 3.2. Effect of carbonization temperature on activated carbon yield 153
  • 4. E nvironment A sia Available online at www.tshe.org/EA EnvironmentAsia 5 (special issue) (2013) 151-155 The international journal published by the Thai Society of Higher Education Institutes on Environment Carbonization temperature plays a significant role on the activated carbon yield. As we increase the temperature from 4000C to 6000C by keeping carbonization time and acid concentration constant, it is taken for 3 different acid concentrations. The variation of activated carbon yield with carbonization temperature is shown in fig 2. For all 3 impregnation concentrations, it was found that the yield of activated carbon decreases with increasing temperature from 4500C onwards. This was due to the loss of most of the volatile matter and loss of phosphate compounds. Under high activation temperature yield decreased tremendously as a considerable amount of phosphate compounds volatised when the carbonization temperature is above 450°C. 80 70 Yield % 60 50 40 12 N H3PO4 30 16 N H3PO4 20 20 N H3PO4 10 0 350 400 450 500 550 600 650 Temp. Figure 2.Effect of carbonization temperature on the yield of Activated Carbon. 3.3. The effect of carbonization time on activated carbon yield Variation of carbonization time by keeping carbonization temperature and acid . concentration constant, for three different temperature 4500C, 5000C, 5500C 80 70 Yield % 60 50 40 400 deg centi. 30 450 deg centi. 20 500 deg centi. 10 0 0 5 10 15 20 25 30 35 Time (min) Figure 3. Effect of carbonization time on the yield of Activated Carbon. 154
  • 5. E nvironment A sia The international journal published by the Thai Society of Higher Education Institutes on Environment As we increase the carbonization time from 10 min and onwards for same temperature the yield of activated carbon decreases with increasing time. The optimum carbonization time for the preparation of the adsorbent was found to be 10 min. 4. Conclusion Karanja seed shells can be used as a precursor in the preparation of activated carbon with good surface area around 344 m2/gm. However, an attempt has been made in this work to study the minimum and optimum carbonization temperature of Karanja seed shell between the ranges of 400-6000C. The optimized conditions (Activation concentration, temperature and time) were all studied. Optimized condition for the preparation of activated carbon is found to be 16N of acid concentration, carbonization temperature Available online at www.tshe.org/EA EnvironmentAsia 5 (special issue) (2013) 151-155 4500C and carbonization time 10 min, as per yield point of view. References 1. Subramanian, K.A., Singal, “Utilization of liquid biofuels in automotive diesel engines, Biomass and Bio energy”, 2005; 29:65-72. 2. Azam A.M., and Nahar N. M., “Prospects and potential of fatty acid methyl esters of some non-traditional seed oil for use as biodiesel in India”. Biomass and Bioenergy.2005; 29:293-302. 3. Tiwari S, Saxena M, Tiwari SK “Mahua oil based resins for the high-temperature curing of fly ash coatings”. Journal of applied polymer Science.2003; 87 (2): 110-120. 4. Ashish S. Saksule, “adsorbents from Karanja seed oil cake and applications”. International Journal of Chemical Engineering and Applied Sciences, ISSN 2278 –1366 Original Article, 2012. Received 16 November 2013 Accepted 3 December 2013 Correspondence to Mr. Akash Dhobale Department of Petroleum Refining & Petrochemical Technology, Laxminarayan Institute of Technology, Nagpur- 440033 E-mail: aks2015@gmail.com 155