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placed in a furnace under a nitrogen atmosphere, heated to 8008C
(ramp rate: 28Cminꢀ1), and held at that temperature for 2 h.
(0.09 g) and H2O (5 g). Carbonization was completed by pyrolysis
at 9008C under vacuum. The carbon-silica composite obtained
after pyrolysis was washed with HF solution to remove the silica
template.
Sample C (Jute-derived carbon #2): Jute (1 g) was ground with a
mortar and pestle into tiny fibrous pieces and then washed three
separate times with acetone, ethanol, and water. The sample was
placed in a furnace under nitrogen, heated to 8008C (ramp rate:
28Cminꢀ1), and held at that temperature for 2 h. The sample was
activated by grinding it together with KOH (1:1 mass ratio), after
which it was heated to 7008C (ramp rate: 28Cminꢀ1) and held at
that temperature for 2 h. The final sample was washed with HCl
and water prior to use.
Sample J (Soft-templated mesoporous carbon #1): According to
a previous paper,[23] phenol (0.61 g) was melted in a flask at 40–
428C and mixed with NaOH aqueous solution (0.13 g; 20 wt%)
under stirring. After 10 min, formalin (1.05 g; 37 wt% formalde-
hyde) was added dropwise and the sample was held below 508C.
Upon further stirring for 1 h at 70–758C, the mixture was cooled to
RT and the pH was adjusted to approximately 7.0 with HCl solu-
tion. The water was removed by vacuum evaporation below 508C,
and the final product was dissolved in ethanol (20 wt% resol-etha-
nol solution). Pluronic F127 (0.5 g) was added to this resol-ethanol
solution (5.0 g; 20 wt%). After stirring at RT for 10 min, the sample
was dried under ambient conditions for 4 h; this was followed by
thermal treatment at 1208C for 24 h. The resulting samples were
obtained after pyrolysis for 3 h at 3508C (ramp rate: 18Cminꢀ1).
Mesoporous carbon was obtained after carbonization under nitro-
gen at 8008C (ramp rate: 18Cminꢀ1) and holding at that tempera-
ture for 2 h.
Sample D (Jute-derived carbon #3): Jute (1 g) was ground with a
mortar and pestle into tiny fibrous pieces and then washed three
separate times with acetone, ethanol, and water. The sample was
placed in a furnace under nitrogen, heated to 8008C (ramp rate:
28Cminꢀ1), and held at that temperature for 2 h. Finally, the ob-
tained carbon was activated by grinding it together with KOH (1:1
mass ratio) and then heating at 8008C for 2 h. The final sample
was washed with HCl and water prior to use.
Sample E (Porous carbon nanosheets): The preparation of this
sample followed an existing method.[19] Zinc nitrate hexahydrate
(11.9 g) was dissolved in distilled water (200 mL) and the pH was
changed gradually to 7.0 with 0.5m NaOH solution. The resulting
precipitate was dried overnight. The precipitate (1 g) was suspend-
ed in 0.5m gallic acid (250 mL) and then stirred vigorously for 2 h
at room temperature (RT) under nitrogen. Next, the sample was
heated (again under nitrogen) to 9508C (ramp rate: 58Cminꢀ1) and
held at that temperature for 2 h. The final sample was washed
with HCl and water prior to use.
Sample K (Soft-templated mesoporous carbon #2): According to
a previous paper,[24] the mesoporous carbon was prepared through
a simple method using atom-transfer radical polymerization. Typi-
cally, the resol precursor (2.0 g, containing 0.25 g phenol and
0.15 g formaldehyde) was added to tetrahydrofuran (THF) solution
(5.0 g, containing 0.1 g PEO125-b-PS230 copolymer) and then stirred
to form a homogeneous solution. The solution was poured into a
dish to evaporate ethanol at RT in ꢁ5–8 h, then heated in an oven
at 1008C for 24 h. The product was removed from the dish and
ground into a fine powder. The obtained sample was calcined at
8008C for 3 h under nitrogen to obtain the mesoporous carbon.
Sample F (MXene-derived carbon): According to
a previous
paper,[20] Ti3AlC2 powder (2 g) was suspended in HF solution
(25 mL; 40 wt%) at RT for 24 h. The resulting precipitate was
washed thoroughly with deionized water to form the MXene, then
dried under vacuum at RT for two days. The dried MXene was
placed into a horizontal quartz tube furnace, which was then
purged with argon and heated to 9008C. Subsequently, it was ex-
posed to dry chlorine gas for 2 h. After chlorination, the samples
were held at 6008C for 2 h under flowing ammonia gas to remove
residual chlorine and chlorides trapped in the pores.
Sample L (Ordered mesoporous carbon prepared from carbon-
silica nanocomposite #1): According to a previous paper,[25] block
copolymer F127 (1.6 g) was dissolved in ethanol (20.0 g, containing
1.0 g of 0.1m HCl solution). The sample was stirred for 1 h at 408C
to make a clear solution. Then, tetraethoxysilane (TEOS; 2.0 g) was
dissolved in this solution. Next, resol-ethanol solution (5.0 g,
20 wt%) was added to the solution, which was then stirred for 1 h
at RT. All three components of the sample were assembled during
this one-step process. The assembled mixture was transferred to a
dish and dried for 1 h at RT. After evaporation of the ethanol, ther-
mal polymerization was conducted at 1008C for 24 h in an oven.
The resulting thin film was removed from the dish, carbonized
under nitrogen at 3508C (ramp rate: 18Cminꢀ1), and held at that
temperature for 3 h, then at 8008C (ramp rate: 58Cminꢀ1), holding
at that temperature for 2 h. The resulting carbon-silica composites
were immersed in HF solution (10 wt%) for 24 h to remove the
silica, and then washed with water.
Sample G (Porous carbon prepared from CaCO3 #1): According
to a previous paper,[21] Na2CO3 solution (0.33m) and CaCl2 solution
(0.033m) were dissolved in deionized water (100 mL). Dopamine
hydrochloride was dissolved in tris(hydroxymethyl)aminomethane
solution (10 mm) and the pH was adjusted to 8.5. This solution was
stirred vigorously for 24 h. The sample was separated by centrifu-
gation, and the resulting CaCO3-polydopamine composite was
heated under nitrogen at 8008C (ramp rate: 28Cminꢀ1) and held at
that temperature for 2 h. The final sample was washed with HCl
and water prior to use.
Sample M (Ordered mesoporous carbon prepared from carbon-
silica nanocomposite #2): The synthetic approach was similar to
that for Sample L. Block copolymer F127 (1.6 g) was dissolved in
ethanol (8.0 g, containing 1.0 g of 0.2m aqueous HCl). The sample
was stirred for 1 h at 408C to make a clear solution. Next, TEOS
(2.0 g) and resol-ethanol solution (5.0 g; 20 wt%) were added se-
quentially to the solution, which was then stirred for 2 h. The mix-
ture was transferred to a dish and dried for 1 h at RT. After total
evaporation of the ethanol, thermal polymerization was conducted
at 1008C for 24 h in an oven. The resulting thin film was removed
from the dish and carbonized under nitrogen at 3508C (ramp rate:
18Cminꢀ1), holding at that temperature for 3 h, then at 9008C
(ramp rate: 58Cminꢀ1), holding at that temperature for 2 h. The re-
sulting carbon-silica nanocomposites were immersed in HF solu-
Sample H (Porous carbon prepared from CaCO3 #2): The synthe-
sis method was similar to that of Sample G except that the CaCO3-
polydopamine composite was heated under nitrogen at 8008C
(ramp rate: 58Cminꢀ1) and held at that temperature for 2 h.
Sample I (Hard-templated mesoporous carbon CMK-3): The prep-
aration of mesoporous carbon CMK-3 has been reported previous-
ly.[22] SBA-15 (1 g) was added to a mixture of sucrose (1.25 g) and
H2SO4 (0.14 g) dissolved in H2O (5 g). The mixture was placed in a
drying oven for 6 h at 1008C, and then for 6 h at 1608C. The
sample turned dark brown or black during the treatment in the
oven. The silica powders containing partially polymerized and car-
bonized sucrose were treated again at 100 and 1608C using the
same drying technique after the addition of sucrose (0.8 g), H2SO4
Chem. Eur. J. 2018, 24, 1 – 7
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