Method

A
B

Carbonization
time / TC
1 hr / 800

Activation
time/ TC
1 hr / 850

Burnoff (%)
-

Surface
Area
248.75
m2/g

Pore
size
2-4
nm

Functional groups

Remarks

Reference

1
2

Aliphatic
Aromatic
Oxygen
Nitrogen
Aromatic
Nitrogen
O-H
Ali, aro, O-H
Ali, aro, O-H, N
-

40-50

2.7 nm

48.5
55.5
73.5
48

85.9
m2/g
366.3
258.9
558.3
-

H2O 9%
Ash 22%
pH 12.7%
Fixed C 43.2
% which
increased at
higher
Carbonization T
H2O 9.15
Ash 8.72

AA CO2
B

1 hr / 800

1 hr/ 850
AA CO2
1 hr/ 850
AA CO2

1 hr / 800

1 hr / 800

1 hr/ 850
AA CO2

40 min/ 500

30 mins
AA - ZnCl2

956

2.0

1549

0.95

7 hr / 550

30 mins/ 80C
AA H3PO4
-

7 hr / 550

190.63

CSAC C
65.88%
Porosity
47.69%

Preparation of activated carbon from cacao shells

Methods:
A. Cocoa shells were dried at 65C during 24h until moisture content was negligible and then sieved. The fraction between 1 and
30 mm was kept at 4C to minimize biodegradation. No other chemical or physical treatments were used prior to adsorption.
B. The heating rate during the process was maintained at 15 C min1. For all the runs, a uniform carbonization time of 1 h was
maintained at the carbonization temperature of 800 C. After this period, the pellets were subjected to activation at 850 C
under a flow of CO2 for several activation times. The product was cooled down again in a stream of flowing N2 until it
reached room temperature. Then the activated carbon was washed with 2 M hydrochloric acid for 1 h at 70 C, followed by a
rinsed with distilled water until it reached pH 7.
C. The residue was impregnated with zinc chloride (Merck, 98%) (1 g agent: 2 g of precursor) under manual agitation for 30 min,
followed by drying at 110 C for 24 h. Carbonization of the material was performed in a muffle furnace (Vulcan 3550) with
nitrogen flow for 40 min at 500 C with a heating rate of 5 Cmin1. The activated carbon obtained was immersed in a
hydrochloric acid solution (Qhemis, 37%) for 20 min and washed with distilled water until reaching a neutral pH. This was
followed by drying the material in an oven at 80 C for 8 h, and storing it in hermetically sealed packages.
D. The residue was impregnated with phosphoric acid (F. Maia, 85%) (1 g agent: 1 g of precursor) and heated to 80 C under
manual shaking for 30 min. Itwas then dried in an oven at 110 C for 24 h. Carbonization of the material was performed in a
muffle furnace (Vulcan 3550) under nitrogen flow for 40 min at 500 C with a heating rate of 5 C min1. The activated
carbon obtained was immersed in a hydrochloric acid solution (Qhemis, 37%) for 20 min and washed with distilled water until
reaching a neutral pH. This was followed by drying the material in an oven at 80 C for 8 h, and storing it in hermetically
sealed packages.
E. Cocoa shell was air dried in sunlight and carbonized with concentrated H2SO4 in the weight ratio of 1:1(w/v). The resulting
product was kept in muffle furnace maintained at 550C for 7 hr. The carbon obtained was washed with distilled water until it
became free from excess acid and dried at 110C for overnight in a hot air oven. The carbonized material was taken out,
grounded to fine powder and sieved to 150 m size and stored in a vacuum desiccator.
F. Cocoa shell was airdried and was added by 50% sulfuric acid with constant stirring (w/v). The resulting product obtained was
kept in muffle furnace maintained at 550C for 7 hours. The carbon obtained was washed with double distilled water and
soaked in 10% sodium bicarbonate solution and allowed to stand overnight to remove the residual acid from pores of the
carbon. The material was washed with distilled water, until the pH of the adsorbent reached 7.0. Then it was dried in a hot air

oven at 100C for 12 hours. The AC was ground and sieved to get the particle size of 150 m and stored in an airtight
container.
References
1. Meunier, N., Laroulandie, J., Blais, J., & Tyagi, R. (2003). Cocoa shells for heavy metal removal from acidic solutions.
Bioresource Technology, 255-263.
2. Ahmad, F., Daud, W., Ahmad, M., & Radzi, R. (2011). Using cocoa (Theobrama cacao) shell-based activated carbon to remove
4-nitrophenol from aqueous solution: Kinetic and equilibrium studies. Chemical Engineering Journal, 461-467.
3. Ahmad, F., Daud, W., Ahmad, M., & Radzi, R. (2012). Cocoa (Theobroma cacao) shell-based activated carbon by CO2
activation in removing of Cationic dye from aqeous solution: Kinetics and equilibrium studies. Chemical Engineering
Research and Design, 1480-1490.
4. Ahmad, F., Daud, W., Ahmad, M., Radzi, R., & Azmi, A. (2013). The effects of CO2 activation, on porosity and surface
functional groups of cocoa (Theobroma cacao) - Shell based activated carbon. Journal of Envonmental Chemical Engineering,
378-388.
5. Ahmad, F., Daud, W., Ahmad, M., & Radzi, R. (2013). The effects of acid leaching on porosity and surface functional groups
of cocoa (Theobroma cacao) - shell based activated carbon. Chemical Engineering Research and Design, 1028-1038.
6. Pereira, R. G., Veloso, C. M., Da Silva, N. M., De Sousa, L. F., Bonomo, R. F., De Souza, A. O., . . . Da Costa Ilheu Fontan, R.
(2014). Preparation of activated carbons from cocoa shells and siriguela seeds using H3PO4 and ZnCl2 as activating agents for
BSA and alpha-lactalbumin adsorption. Fuel Processing Technology, 476-486.
7. Theisavarasu, C., Mylsamy, S., & Sivakumar, N. (2011). Cocoa Shell as Adsorbent for the Removal of Methylene Blue from
Aqueous Solution: Kinetic and Equilibrium Study. Universal Journal of Environmental Research and Technology, 70-78.
8.

Mylsamy, S., & Theivarasu, C. (2012). Adsorption of Reactive Dye Using Low Cost Adsorbent: Cocoa (Theobroma Cacao)
Shell. World Journal of Applied Environmental Chemistry, 22-29.