Activated carbon preparation process

Walnut shell (particle size of 0.1 mm) was heated at a heating rate of 10°C min -1 under CO2
atmosphere to 800◦C and held at this temperature for 1 h before the heat was turned off.
As soon as the system reached ambient temperature, the solid was collected (denoted as
WS-CO2-800) for further functionalisation, tests, and analysis. It is expected that in the CO 2
environment at high temperatures e.g. > 700◦C, the solid obtained will be more porous due
to the Boudouard reaction (C + CO2 → 2CO).

K2CO3 activation: K2CO3 was chosen as an activation agent due to its environmentally
friendly property, allowing K2CO3 to be used in food products [37]. At high temperatures
(800°C), K2CO3 reacted with walnut shell and enhanced the porosity and morphology of
carbons [38]. The walnut shell was impregnated directly with 100 mL DI water containing 40
g of K2CO3 to create activating ratio mass ratio of K2CO3 to walnut shell of 4:1 and then dried
overnight in oven at 60°C. The dried mixture was transferred into a Vecstar furnace and
carbonised at 800°C for 2 h at a heating rate of 10°C min-1 under N2 atmosphere and then
left cooled down overnight under N2 until it reached ambient temperature. The walnut shell
activated carbon was collected and washed in hot DI water until pH reached 7 to remove
remaining potassium compounds in carbons. The walnut shell carbon was denoted as WS-
K2CO3-800.

KOH activation: KOH was used as the activating agent. 40 g of KOH was mixed with 10 g of
walnut shells to create the mass ratio of KOH to walnut shell 4:1 and then dried overnight in
oven at 60°C. The dried mixture was transferred into a Vecstar furnace and carbonised at
800°C for 2 h at a heating rate of 10°C min-1 under N2 or CO2 atmosphere and then left
cooled down overnight until it reached ambient temperature. This will give two different
carbons WS-KOH-N2-800 and WS-KOH-CO2-800.

Fe(NO3)3 activation: It is expected that Fe(NO3)3 reacts with biomass at high temperatures
e.g.  800°C to create carbon with mesoporous structure and highly ordered graphitic
carbon structure [35,39]. 40 g of walnut shell was impregnated in 100 mL Fe(NO3)3 1 M
(mass ratio Fe(NO3)3/ walnut shell 3:5) solution overnight. The mixture was then dried in the
oven at 60°C overnight and the dried mixture was then carbonised at 800°C for 2 h under N 2
atmosphere, and the furnace was left cooling down overnight under N 2 flow. The carbon
sample was washed with HCL 0.1 M to remove all iron particles and then with hot DI water
until it reaches neutral pH (6-7). This carbon is denoted as WS-Fe(NO 3)3-N2-800. Another
sample was prepared and activated under CO2 instead of N2 to give WS-Fe(NO3)3-CO2-800.