03-KC2017-049 Rev[1] File[1398].hwpClean Technol., Vol. 23, No. 4,
December 2017, pp. 364-377
* To whom correspondence should be addressed. E-mail:
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doi: 10.7464/ksct.2017.23.4.364 pISSN 1598-9712 eISSN 2288-0690
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1, 2, 3, 3, 3,* 1
46241 63 2 2
46241 63 2 3
51518 51-88
(2017 10 25 ; 2017 11 5 ; 2017 11 5 )
Characteristics on Chemical Activation and VOCs Adsorption of
Activated Carbon according to Mixing Ratio of Anthracite and
Lignite
Joon-Hyung Cho1, Sung-Kyu Kang2, Min-Kyoung Kang3, Kuk Cho3, and
Kwang-Joong Oh3,* 1Division of Creative Low Impact Development and
Management for Ocean Port City Infrastructures, Pusan National
University
2, Busandaehak-ro 63beon-gil, Geumjeong-gu, Busan, 46241, Republic
of Korea 2Department of Civil and Environmental Engineering, Pusan
National University
2, Busandaehak-ro 63beon-gil, Geumjeong-gu, Busan, 46241, Republic
of Korea 3Department of Environmental Chemistry, Korea Polytachnic
VII Collage
51-88, Oedongballim-ro, Seongsan-gu, Changwon-si, Gyeongsangnam-do,
51518, Republic of Korea
(Received for review October 25, 2017; Revision received November
5, 2017; Accepted November 5, 2017)
·
, , ,
. , ,
. · , , , ,
1,154 ~ 1,420 m2 g-1 ,
, . , ,
5,640 kcal kg-1 , > >
.
: , , , ,
Abstract : In this study, to improve the low surface area of
domestic anthracite as raw materials of activated carbon,
characteristics on chemical activation and VOCs adsorption of
activated carbon according to mixing ratio of anthracite and
lignite. For these, properties of raw materials, parameter
characteristics of preparation processes for activated carbon, and
VOCs adsorption characteristic of the prepared activated carbon are
analyzed. The experimental results showed that, the domestic
anthracite had disadvantages of high contents for ash and lead,
arsenic, which were exceeded for the heavy metal limits, in the
properties of raw materials. To improve these diadvantages, using
the mixing ratio of anthracite and lignite, and the optimum
conditions for pretreatment, activation, washing, and pellitization
process, the activated carbon had a range of BET
(Brunauer-Emmett-Teller) surface area of 1,154 ~ 1,420 m2 g-1 with
mesopore development and hydrophobic surface property. The carbons
were satisfied
364
365
with the quality standard for granular activated carbon, and had
similar physicochemical properties with the commercial activated
carbon. The minimum mixing condition for commercial VOCs activated
carbon performance must have the caloric value of above 5,640 kcal
kg-1, and the carbon had higher adsorption capacity with order of
xylene > toluene > benzene according to more higher molcular
weight and hydrophobic property.
Keywords : Activated carbon, Chemical activation, Anthracite,
Lignite, Volatile organic compounds
1.
,
. , , ,
,
[1]. 2015
, , ,
[2],
,
,
. ,
50 ,
10 1,000
· ,
19 ~ 36% [1]. ( , , ) 50,767
99.6%
, , ,
79.8%
[3].
, , , , , ,
4, 5,000
[4]. 3 M, DuPont
,
Calgon, Norit
[5].
, 15 [6], , ,
, 20 .
, 24,300/
38%
, 2014 115,429 2006 13%
[7].
. ,
, , ,
,
.
2 . ,
, 936 2,381
94,600 ~ 197,490
[8,9].
(62 ~ 70%) (33~35%)
.
.
2 ,
,
. ,
, (phosphoric acid), (zinc chloride), (potassium carbonate),
(sodium hydroxide), (potassium hydro- xide) [12-14].
, ,
, , ,
[10-12].
,
, Kong et al. [13]
, 920 m2 g-1 . Kim,
366
Figure 1. Schematic diagram of activation process reactor.
et al. [14] 2 , 900 ~ 1,000 m2 g-1 .
1,000 m2 g-1
.
, Yoon et al. [15]
1,014 ~ 1,093 m2 g-1
, Kim et al. [16]
1,039 ~ 1,232 m2 g-1
, Choi et al. [17] ·
1,084 m2 g-1 .
,
,
.
, , ,
, , ,
,
BET (Brunauer–Emmett–Teller) ,
, FTIR (Fourier Transform Infrared) .
.
2.
2.1.
, .
8 ~ 35 mesh .
(Nitric acid, Samchun, KOR, purity 60%), (Hydro- chloric acid,
Samchun, KOR, purity 35 ~ 37%), (Phophoric acid, Samchun, KOR,
purity 85%), (Sulfuric acid, Junsei, JPN, purity 95%) ,
(Potassium hydroxide, Samchun, KOR, purity 85%) . CMC (Car-
boxylmethyl cellulose sodium salt, Samchun, KOR), PVA (Polyvinyl
alcohol, Samchun, KOR), (Starch, Samchun, KOR), (Gum arabic,
Samchun, KOR) .
2.2.
, , , , , .
(OV-11/CTB-10, Jelo Tech, KOR) -0.1 MPa, 90 , 24 h
,
(SH-820F, Seyoung Scientific, KOR)
, (0.5 ~ 16 M)
(1 ~ 5 mL g-1), (6 ~ 48 h) .
367
Table 1. Proximate, element, caloric value, heavy metal analysis
for low-grade anthracite, anthracite, and ligniet as raw material
of activated carbon
Items Analyzed items Unit
Ash % 43.0 31.13 14.55 - Fixed carbon % 49.10 60.99 76.28 -
Element
C % 26.20 62.50 80.1 - H % 1.10 0.80 3.00 - O % 1.10 2.00 4.30 - N
% 0.40 0.40 1.70 - S % 0.08 0.24 0.43 - Cl % 0.08 0.01 0.00 -
Caloric value
Lower heating value
Heavy metal
Hg mg kg-1 0.00 0.04 0.00 - Cd mg kg-1 0.00 0.61 1.62 1 Pb mg kg-1
39.90 33.90 9.00 10 As mg kg-1 2.20 7.60 0.00 2 Cr mg kg-1 33.20
57.80 47.3 - Co mg kg-1 5.50 8.20 12.9 - Cu mg kg-1 5.20 28.60 0.0
- Mn mg kg-1 24.50 74.50 693 - Ni mg kg-1 11.40 45.30 31.70 - Tl mg
kg-1 0.00 0.00 0.00 - V mg kg-1 47.80 20.10 7.40 -
(25 ~ 90 ) (6 ~ 48 h) ,
115 . 24 h . Figure 1 (STF-15/
75/610, Carbolite Ltd., UK) , (Euro- therm 2408CP, Carbolite Ltd.,
UK) 1,500
, 16
,
. 1,000 mm, 500 mm , 6
. 1,000 mm, 50 mm, 5 mm,
, , 0.5 ~ 5.0 L min-1
.
20 ,
,
. , ,
30 g
,
99.9% (0.5 ~ 2 L min-1)
10 min-1 (700 ~ 900 )
, (2 ~ 5 h)
. ,
,
.
(0.1 ~ 5 M) (1 ~ 4 mL g-1), (0.5 ~ 4 h)
, pH
, ,
-0.1 MPa, 90 , 24 h .
, (5 ~ 15%)
-0.1 MPa, 90 , 24 h .
BET , , FTIR . BET
(Micromeritics ASAP 2020, USA)
90 , 10 min-1, 350 , 4 h
-196 ,
0.05 ~ 0.15 P/P0 5
0.9999 , C . KSM 1802 , , , , FTIT
(IRAffinity-1 Shimadzu, Japan) .
(ASTM D6646-03)
,
,
(50 ppm), (5,000 ppm),
, , (10,050 ppm)
,
(ppbRAE 3000, REA systems, Inc., USA)
. 3
.
368
Figure 2. BET surface area and ash content of activated carbon
according to (a) pretreatment agents, (b) HNO3 concentration, (c)
HNO3/ anthracite ratio, and (d) pretrement time in pretreatment
process.
, , ,
,
. , (%) (8.9) > (6.1)
(6.1)
, (%)
(43.0) > (31.1) > (14.6)
11.9 ~ 28.4% , (%)
(76.3) > (61.0) > (49.1)
.
,
,
. , C (%) (80.1) > (62.5) >
(26.2)
, H (%) 3%
. O (%) 5%
, N, S, Cl 0.5%
. (kcal kg-1) , (7,086) > (5,162) > (2,360) .
7,400 kcal kg-1 30.2 ~ 68.1%
, C
. , (mg kg-1) (802.9) >
(276.7) > (169.7) , Pb
(mg kg-1) (39.9) > (33.9) > (9.0) 10 mg kg-1 , As (mg kg-1)
(7.6) >
(2.2) > (0.0)
2 mg kg-1 , Cd (mg kg-1) (1.62) > (0.61) > (0.0)
1 mg kg-1 .
, Cd, Pb, As 3
.
3.2.
.
,
.
3.2.1.
Figure 2 (a) , (b)
369
Table 2. Coagulation properties of anion and cation in aqueous
solution
Anion→ Cl- NO3 - SO4
Cation↓
Ag+ I S S I Hg+ I S VSS I Ba2+ S S I I Ca2+ S S VSS I Cu2+ S S S I
Cd2+ S S S I Co2+ S S S I Fe2+ S S S I Hg2+ S S VSS I Mg2+ S S S I
Mn2+ S S S I Ni2+ S S S I Pb2+ I S I I Sr2+ S S VSS I Zn2+ S S S I
Al3+ S S S I As3+ S X X X Cr3+ S S S I Fe3+ S S S I V3+ S S S
I
Note : S = soluble (>5000 mg L-1), SS = slightly soluble
(2000-5000 mg L-1), VSS = very slightly soluble (20-2000 mg L-1), I
= insoluble (< 20 mg L-1), X = not compound.
, (c) , (d)
25 24 h, ,
900 , 4 h, 1 L min-1, (KOH/ anthracite, wt% wt%-1) 4 , 0.5 M , , 4
mL g-1, 2 h
. Figure 2(a) , (m2
g-1) (1685.4) > (539.9) > (210.4) > (39.7) .
(SiO2) 49 ~ 57%, (Al2O3) 27 ~ 31%, (Fe2O3) 4 ~ 10%, (CaO) 2 ~ 6%,
(MgO) 0.4 ~ 1.3%
[18]. Equation (1)~(13)
, ,
[19-23], Table 2
[24,25]
, , , . ,
, , ,
.
.
Al2O3(s) + 6HCl(aq) → 2AlCl3(aq) + 3H2O (5)
Fe2O3(s) + 6HCl(aq) → 2FeCl3(aq) + 3H2O (6)
CaO(s) + 2HCl(aq) → CaCl2(aq) + H2O (7)
Al2O3(s) + 3H2SO4(aq) → Al2[SO4]3(aq) + 3H2O (8)
Fe2O3(s) + 3H2SO4(aq) → Fe2[SO4]3(aq) + 3H2O (9)
CaO(s) + H2SO4(aq) → CaSO4(s) + H2O (10)
Al2O3(s) + H3PO4(aq) → 2Al[PO4](s) + 3H2O (11)
Fe2O3(s) + H3PO4(aq) → 2Fe[PO4](s) + 3H2O (12)
3CaO(s) + 2H3PO4(aq) → Ca3[PO4]2(s) + 3H2O (13)
(%) , (28.1) >
(26.8) > (22.5) > (21.6) 3
.
.
. Figure 2(b) ,
(m2 g-1) 16 M (1830.0) > 10 M (1829.9) > 5 M (1565.4) > 1
M (1194.5) > 0.1 M (1027.0)
, 10 M .
,
.
, 0.5 M (28.6) > 1 M (27.2) > 5 M (23.8) > 10 M (21.6) 16
M (21.6)
.
10 M .
370
Figure 3. BET surface area of activated carbon according to (a)
mixing temperature, and (b) mixing time in mixing process.
Figure 2(c) , (m2 g-1) 5 mL g-1 (1832.1) > 4 mL g-1 (1829.9)
> 3 mL g-1 (1687.3) > 2 mL g-1 (1431.8) > 1 mL g-1
(423.8)
, 4 mL g-1
.
,
. (%) , 1 mL g-1 (31.55) > 2 mL g-1 (25.0) > 3 mL g-1 (22.5)
> 4 mL g-1 (21.6) 5 mL g-1 (21.6) .
4 mL g-1 . Figure 2(d) , (m2
g-1) 48 h (1708.7) 24 h (1685.4) 12 h (1685.4) > 6 h (1156.5) 6
h 12 h . 12 h ,
.
(%) 6 h (30.8) > 12 h (21.6) 24 h (21.5) 48 h (21.3) .
12 h .
3.2.2.
Figure 3 (a) , (b)
10 M , 4 mL g-1, 12 h,
, 900 , 4 h, 1 L min-1, (KOH/anthracite, wt% wt%-1) 4
, 0.5 M , , 4 mL g-1, 2 h .
Figure 3(a) , (m2 g-1) 90 (1685.4) > 55 (1675.2) > 25
(1662.8)
.
,
1.4%
.
25 . Figure 3(b) , (m2 g-1)
48 h (1686.2) > 24 h (1685.4) > 12 h (1495.4) > 6 h
(1256.5) , 24 h .
24 h
, 24 h .
3.2.3.
Figure 4 (a) , (b) , (c) , (d)
Figure 4(d)
.
10 M , 4 mL g-1, 12 h, 25 24 h,
0.5 M , , 4 mL g-1, 2 h
. Figure 4(a) , (KOH/anthracite,
wt% wt%-1) (m2 g-1) 4 (1829.9) > 5 (1435.5) > 3 (1329.3) >
2 (791.1)
4
,
. Equation (14) C KOH
1 : 3 [11,26,27],
1 : 4
,
.
4
.
371
Figure 4. BET surface area of activated carbon according to (a)
KOH/anthracite ratio, (b) activation temperature and time, (c)
nitrone flow rate, and (d) caloric value in activation process
[note : the analysis results for ash and carbon content were
included in Figure 4(d)].
6KOH + 2C → 2K + 3H2 + 2K2CO3 (14)
Figure 4(b) , 4 h (m2 g-1) 900 (1829.9) > 800 (1740.5) > 700
(1500.5)
, 900 . Equation (14)
Equation (15) ~ (18) 800
[27],
. 900
(m2 g-1) 4 h (1829.9) > 3 h (1685.4) > 5 h (1450.5) > 2 h
(1136.4) > 1 h (1025.4)
4 h ,
. 4 h
.
900 , 4 h .
K2CO3 → K2O + CO2 (at 700 ~ 800 ) (15)
CO2 + C → 2CO (16)
Figure 4(c) ,
(m2 g-1) 2.0 L min-1 (1875.9) 1.5 L min-1 (1864.5)
1.0 L min-1 (1829.9) > 0.5 L min-1 (1155.4) 0.5 L min-1
1.0 L min-1
.
, , .
1.0 L min-1 . Figure 4(d) ,
(m2 g-1) 7,086 kcal kg-1 (2073.1) > 6,124 kcal kg-1 (1915.0)
> 5,162 kcal kg-1 (1,685.4) > 3,761 kcal kg-1
(1,230.6) > 2,360 kcal kg-1 (633.5)
, . 1,000 m2 g-1
3,300 kcal kg-1 , 39% .
3.2.4.
Figure 5 (a) , (b) , (c) , (d)
372
Figure 5. BET surface area of activated carbon according to (a)
washing agents, (b) HCl concentration, (c) HCl/anthracite ratio,
and (d) washing time in washing process.
Figure 6. BET surface area and hardness of activated carbon
according to (a) binder kinds, and (b) binder content in
pelletization process.
HW (hot water), CW (cold water) . 10 M ,
4 mL g-1, 12 h,
25 24 h, ,
900 , 4 h, 1 L min-1, (KOH/anthracite, wt% wt%-1) 4 .
Figure 5(a) , (m2 g-1) HCl-HW-CW (1829.9) HW-CW (425.3) > CW
(280.8)
1,400 m2 g-1
. Equation (14) ~ (18)
, ,
,
. ,
85
.
--
.
Figure 6 (a) , (b)
373
Table 3. BET surface area, pore volume, and average pore width of
pelletized activated carbons
Sample Low-grade anthracite
Low-grade anthracite + Anthracite
activated carbon
BET surface area (m2 g-1) 433.8 842.7 885.1 1154.2 1191.9 1419.7
1522.3
Micropore area (m2 g-1) 367.4 453.3 437.7 758.8 598.6 827.5
1314.2
External area (m2 g-1) 66.5 389.4 447.4 395.4 593.3 592.2
208.1
Total pore volume (cm3 g-1) 0.242 0.523 0.593 0.608 0.654 0.753
0.692
Micropore volume (cm3 g-1) 0.158 0.208 0.205 0.326 0.271 0.361
0.55
Mesopore volume (cm3 g-1) 0.084 0.314 0.388 0.282 0.383 0.392
0.142
Average pore width () 22.3 24.8 26.7 21.0 21.9 21.2 18.2
10 M , 4 mL g-1, 12 h, 25 24 h,
, 900 , 4 h, 1 L min-1, (KOH/anthracite, wt% wt%-1) 4,
0.5 M , , 4 mL g-1, 2 h
. Figure 6(a) ,
(m2 g-1) CMC (1250.4) > Starch (1173.6) > Guargum (1120.9)
> PVA (1040.7) . Lozano-Castello et al. [28] CMC
, PVA
.
. (%) , CMC (94) > PVA (67) > Guargum (51) > Starch
(36)
, KSM 1802 90%
-25.8% , CMC
.
CMC , CMC
. Figure 6(b) , (m2
g-1) 0% (1685.5) > 5% (1541.1) > 10% (1379.9) > 15%
(1250.4)
. (%)
, 15% (94) > 10% (84) > 5% (77) 0% (10) 5% , 5% 15%
. KSM 1802
90%
15% .
3.4.
,
BET , , FTIR .
3.4.1. BET
BET
(m2 g-1) , Commercial AC (1522.3) > Lignite (1419.7) >
Anthracite + Lignite (1191.9) > Anthracite (1154.2) > Low-
grade anthracite + Lignite (885.1) > Low-grade anthracite +
Anthracite (842.7) > Low-grade anthracite (433.8)
.
31.5%, 33.1%, 30.6% . (m2 g-1) Commercial AC (1314.2) > Lignite
(827.5) > Anthracite (758.8) > Anthracite + Lignite (598.6)
> Low-grade anthracite + Anthracite (453.3) > Low-grade
anthracite + Lignite (453.3) > Low-grade anthracite (367.4) 1.5
~ 3.5
, (m2 g-1) Anthracite + Lignite (592.2) > Lignite (593.3) >
Low-grade anthracite + Lignite (447.4) > Anthracite (395.4) >
Low-grade anthracite + Anthracite (389.4) > Commercial AC
(208.1) > Low-grade anthracite (66.5)
1.8 ~ 2.9 . , (cm3 g-1) Lignite (0.753)
> Commercial AC (0.692) > Anthracite + Lignite (0.654) >
Anthracite (0.608) > Low-grade anthracite + Lignite (0.593) >
Low-grade anthracite + Anthracite (0.523) > Low-grade anthracite
(0.242)
. (cm3 g-1)
, (cm3/g) Lignite (0.392) > Low-grade anthracite + Lignite
(0.388) > Anthracite + Lignite (0.383) > Low-grade anthracite
+ Anthracite (0.314) > Anthracite
374
Figure 7. Fourier-transform infrared spectra of (a) powdered
activated carbons, and (b) pelletized activated carbons.
Table 4. Physical property of pelletized activated carbons
Physical property
Density (g mL-1)
Low-grade Anthracite 1.5 99.2 98.2 0.55 Low-grade Anthracite +
Anthracite 1.8 99.5 97.9 0.40
Low-grade Anthracite + Lignite 1.6 99.2 97.9 0.39
Anthracite 1.7 99.6 97.7 0.38 Anthracite + Lignite 1.6 99.1 97.5
0.36 Lignite 1.4 99.4 97.0 0.33 Commercial AC 2.0 95.8 97.1
0.41
Standard (KSM 1802) under 10
above 90
above 90
under 0.56
(0.282) > Commercial AC (0.142) > Low-grade anthracite
(0.084) 34.1% ,
2.0 ~ 2.8 . () , Low-grade anthracite + Lignite
(26.7) > Low-grade anthracite + Anthracite (24.8) > Low-grade
anthracite (22.3) > Anthracite + Lignite (21.9) > Lignite
(21.2) > Anthracite (21.0) > Commercial AC (18.2)
1.8% , 20
,
.
,
.
. ,
, 1.4 ~ 1.8%
,
. 99%
.
,
,
.
,
,
.
Figure 7 (a) , (b) FTIR
. Figure 7(a) , O-H (3,700 ~ 3,800 cm-1), C=O (1,550 cm-1), C-H
(1,430 cm-1), C-O (978 cm-1) [29],
.
,
,
. Figure 7(b) , CMC
O-H (3,000 ~ 3,500 cm-1), -COOH (1,600 cm-1), C-H (1,430 cm-1),
-CH2 (1,320 cm-1), C-O (1,000 cm-1)
[29],
. 15%
.
,
,
.
375
Figure 8. Breakthrough curve of activated carbon for (a) single
benzene, (b) single xylene, and (c) combined benzene, toluene, and
xylene.
3.5.
(a) , (b) , (c) ,
,
short term exposure limit (STEL) , . ,
. Figure 8(a) , (STEL 5 ppm)
(min) Lignite (320) > Anthracite (254)
Commercial AC (252) > Anthracite + Lignite (240) > Low- grade
anthracite + Anthracite (207) > Low-grade anthracite + Lignite
(207) > Low-grade Anthracite (100) ,
1.3 . Table 3
. , STEL 5 ppm ,
.
,
. Figure 8(b) , (STEL 150 ppm)
Lignite (160) > Anthracite + Lignite (133) > Anthracite (120)
> Low-grade anthracite + Lignite (79) > Commercial AC (70)
> Low-grade anthracite + Anthracite (60) > Low-grade
Anthracite (22) ,
1.1 ~ 2.3 .
Table 3
, ( >
> ),
. Figure 8(c) , , ,
(STEL 305 ppm) (min) Lignite (115) > Anthracite + Lignite (70)
> Commercial AC (67) > Anthracite (65) > Low-grade
anthracite + Anthracite (56) > Low-grade anthracite + Lignite
(55) > Low-grade Anthracite (31)
, ,
1.7
.
,
, , ,
.
4.
376
,
, . , (%) (43.0) >
(31.1) > (14.6)
,
(kcal kg-1) (7,086) > (5,162) >
(2,360) 30.2 ~ 68.1%
.
, 3.3 ~ 3.9, 1.1 ~ 3.8 .
,
,
. , 10
M , 4 mL g-1, 12 h,
25 24 h,
4, 900 , 4 h, 1 L min-1,
0.5 M --, 4 mL g-1, 2 h,
CMC 15% .
4,290 kcal kg-1 , 35%
, 1,154 ~ 1,420 m2 g-1
. ( 1,000 m2 g-1) 15 ~ 42% .
, BET
0.8 ~ 0.9 , 0.6 ,
1.9 ~ 2.8 ,
. FTIR ,
,
.
.
,
1.0 ~ 1.3, 1.1 ~ 2.3, 1.0 ~ 1.7 , (87.5%) > (11.2%) > (-9.3%)
. , ,
5,640 kcal kg-1 , > >
.
.
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