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Fibers and Polymers 2015, Vol.16, No.

3, 543-549 ISSN 1229-9197 (print version)


DOI 10.1007/s12221-015-0543-6 ISSN 1875-0052 (electronic version)

Effects of Powder Activated Carbon Particle Size on Adsorption Capacity and


Mechanical Properties of the Semi Activated Carbon Fiber
Navid Saeidi* and Mohammad Nader Lotfollahi*
Faculty of Chemical, Gas and Petroleum Engineering, Semnan University, Semnan 35195-363, Iran
(Received August 22, 2014; Revised November 1, 2014; Accepted November 11, 2014)

Abstract: Effects of activated carbon particle size on adsorption and mechanical properties of the semi activated carbon fiber
(SACF) were studied. Four types of powder activated carbons including powders with particle size less than 150, 90, 50 µm
and powder without any screening were used to prepare the coater adsorbent mixture for coating on E-glass fiber. Iodine
number and BET surface area of the coated fibers were measured. The results showed that arrangement and screening of the
powder activated carbon had positive effect on the adsorption capacity and surface area of the produced samples. Also,
arrangement and decrease of activated carbon particle size led to improve mechanical properties of the produced samples.
Keywords: Semi activated carbon fiber, Adsorption property, Mechanical property, Surface area, Particle size

Introduction Economy et al. [12] have developed a relatively low cost


procedure in which phenolic resin as precursor was coated
Activated carbons are well-known adsorbents extensively on glass fibers. However their work had a few vulnerable
used for purification and separation in many industrial spots, but using of low cost glass fiber was a good idea to
processes and for effluent treatment, owing to their ability to prepare SACF. After the above work, a few researchers
adsorb a large variety of compounds from both gaseous and studied on preparation of SACF and tried to increase the
liquid streams [1-3]. Activated carbons are applied in quality of the fibers, including adsorption capacity and
various shapes, suchas powder, granular, pellet, honeycomb mechanical strength, and decrease the cost of the products.
and activated carbon fiber (ACF), and each type has its Jeong et al. [11] evaluated the possibility of using coal tar
specific application [3-5]. ACFs have very wide applications pitch instead of phenolic resin for coating on the glass fiber
in industries, particularly, for removal of pollutants from because of its lower cost than phenolic resin. In other reported
water or air. The applications of ACF have been widely work [10] a procedure was described for coating glass fiber
extended, not only as an adsorbent but also as a catalyst by a mixture of coal tar pitch and phenolic resin. In such
support and as an electronic material [3,6-9]. Various methods works, the glass fibers after coating by precursors (pitch and
were proposed to produce ACF [6,10-15]. Eom et al. [6] phenolic resin) were treated under high temperature (500-
prepared the ACF through differently shaped of spinnerets 1000 oC). The treatment includes carbonization and activation.
from pitch precursor. They activated the carbon fiber in These treatments may negatively affect on shape and
steam media. To attain ACFs with good adsorption capacity, mechanical strength of the products. Also, as mentioned
they performed the treatments under high temperature earlier, SACF can be used as a catalyst support. Therefore,
(around 1000 oC). Vilaplana-Ortego et al. [13] prepared treating under high temperature may damage the loaded
activated carbon fibre monoliths by physical activation of material on the catalyst support.
carbon fiber monolith rived from two kinds of pitch-based By using powder activated carbon instead of phenolic
carbon fibre (CF). resin in coating the glass fiber, it does not need any thermal
In another reported work, Im et al. [14] prepared ACF by treatments on the coated glass fiber at high temperature any
electro-spinning method. To activate the ACF, they attached more. To our knowledge ethe possibility of coating glass
silica nanoparticles to the ACF before electro-spinning. After fiber by powder activated carbon have not been examined
stabilization, the silica nanoparticles were extracted by HF yet.
acid. They did not treat the fibers under high temperature. In some reported works, the authors studied effects of
However, the obtained ACF in the mentioned work did not activated carbon particle size on the quality of their products
have proper surface area. Kim et al. [15] also used the [16-23]. For instance, Jae-Woo Lim et al. [16] reported a
electro-spinning method to prepare activated carbon fiber. In method to manufacture honeycomb activated carbon. They
their work, stabilization step was done under high temperature, studied effect of activated carbon particle size on the prepared
700 to 1000 oC. The stabilized fibers were activated by honeycomb’s adsorption and mechanical properties. They
steam at temperature 650 to 850 oC. All above mentioned improved the product properties by changing and arranging
works are expensive and time-consuming. the size of the powder activated carbon. Thus, it could be
inferred that it is possible the mechanical and adsorption
*Corresponding author: Navid_Saeedi13@yahoo.com properties of the shaped activated carbon to be promoted by
*Corresponding author: mnlotfollahi@semnan.ac.ir changing and arranging powder activated carbon particle

543
544 Fibers and Polymers 2015, Vol.16, No.3 Navid Saeidi and Mohammad Nader Lotfollahi

size used in the manufacture process. Table 1. Iodine numbers, surfaces area and mean pore diameter of
In the present work, a procedure was described for coating the samples
powder activated carbon on glass fibers for applying in gas Particle size Iodine Surface Mean pore
phase. In addition, the effects of powder activated carbon Run no. of activated number area diameter
particle size on surface area and adsorption and mechanical carbon (µm) (mg/g) 2
(m /g) (N)
properties of SACF were studied. For this purpose, four 1 Various @
1360 1155 2.3
types of powder activated carbon having certain particle size
2 150 1353.554 1040 2.1
were prepared and applied.
3 90 1368.862 1195 1.9
Experimental 4 50 1387.871 1240 1.75
@
Activated carbon with mean particle size up to 109 µm.
Materials and Reagents
Methyl cellulose was obtained from BDH Company (UK)
as a binder. The methyl cellulose has a gelation temperature of nitrogen at -196 oC. Table 1 shows iodine numbers, mean
(around 45 oC) and below this gelation temperature the pore diameters and surfaces area of the samples.
methyl cellulose is completely soluble in water. Powder As can be seen in Table 1, by decreasing activated carbon
activated carbon was obtained from Jacobi Company particle size from 150 µm to 50 µm, both iodine number and
(Sweden). Choloridric acid, iodine, potassium iodide, starch, surface area are changed by an ascendant trend, but mean
sodium thiosulfate were obtained from Merck Company pore diameters were decreased. These behaviors are consistent
(Germany), all with mass fraction purity greater than 0.99. with the reported work by Lim et al. [16]. To study effect of
All chemicals were used without any further purification. activated carbon particle size on adsorption capacity and
The E-glass fiber with about 0.5 mm thickness was provided mechanical properties of the coated fibers, the sieved activated
from Qingdao strong M&E Co. Ltd. (China). carbon powders were individually applied in preparing the
Characteristics of the Powder Activated Carbon and adsorbent coater mixture.
Screening
The purchased activated carbon was sieved to obtain three Coating the Fibers
activated carbon types including particles with less than 50, The coating procedure was carried out by dip-coating
90 and 150 µm by standard sieves equipped with a shaker method [26] with several alterations. For this, a mixture
(E.L.M, SIE. 35). Figure 1(a), (b) and (c) show SEM images including powder activated carbon, methyl cellulose and
of the screened activated carbon powders with less than 50, water was mixed by a mechanical mixer with about 300 rpm
90 and 150 µm and Figure 1(d) shows the activated carbon at temperature 50 oC for 15 min. Actually, the temperature
powder without any screening. The SEM images were recorded was increased over 45 oC, which under the temperature
using XL30 Philips. Iodine number of the samples was methyl cellulose was completely soluble in the water, until
obtained by ASTM D4607-94 [24]. In this work, all the methyl cellulose partly precipitated and a mixture having
iodine number measurements were performed three times suitable viscosity for dip-coating was attained. Then, the
and the average values were reported. The nitrogen adsorption fibers (1.92 g and 12 cm2) were simply dipped in the prepared
and desorption isotherms for all samples were measured at mixture, allowed to soak for a few minutes. In order to drain
−196 oC on a Belsorp 18 (BEL Japan, Ltd.). The samples the excess mixture, the fibers are subjecting under a force 15
were heated at 200 oC for 2 hours and degassed overnight. Newton for one minute. Then, the prepared fibers were dried
The specific surface area and mean pore diameter were by an oven at temperature 60 oC for 3 hours. In the above
determined by the Brunauer-Emmet-Teller (BET) method mentioned step for preparation of the coated mixture, the
[25] using am (N2=16.2 Å2), where, am, is the molecular area temperature was regulated by a thermostatic bath (Grant

Figure 1. SEM images of the activated carbon (250×), (a) particle size less than 50 µm, (b) particle size less than 90 µm, (c) particle size less
than 150 µm, and (d) various particle size (mean particle size up to 109 µm).
Improvement of Semi Activated Carbon Fiber’s Properties Fibers and Polymers 2015, Vol.16, No.3 545

instruments (Cambridge) Ltd. (type SE 15, England)), accurate this case. It can be concluded that the minimum composition
to ±0.2 oC. Also, the components were weighed on an analytical of methylcellulose is 3 wt%. Figure 2 shows SEM images of
balance (A&D Company, GF-600, Japan) accurate to 0.001 g. the coated fibers by mixtures containing 3 wt% of methyl
It is important to note that the mixing of the binder with cellulose and various contents of activated carbon (15, 20
powder activated carbon using high-speed mixer prevents and 25 wt% in Figure 2(a), (b) and (c), respectively). As it
blocking of the activated carbon pores and improves the can be seen in Figure 2(a), the adsorbent mixture did not
adsorption capacity of the prepared mixture [27]. well fill the voids between the fibers. Figure 2(c) shows that
the SEM image of the produced activated carbon fiber
Results and Discussion demonstrated better coating with respect to the prior cases
(in Figure 2(a) and (b)). The experiments with more wt% of
Adsorption Capability activated carbon (30 wt%) in the coater adsorbent mixture
In this work, a set of experiments was performed to attain showed that the coater adsorbent mixture was viscose and
appropriate adsorbent mixture for good quality of coating. coating by dip-coating method was impossible. For the
We first coated the fibers by various compositions of the adsorbent mixture containing of 4 wt% methyl cellulose and
adsorbent mixture and then the quality of coating was various wt% of activated carbon, the obtained results were
examined by SEM images. The experiments were started the same as the results obtained by the adsorption mixture
with the minimum composition of methyl cellulose (1 wt%) containing 3 wt% methyl cellulose. By increasing the wt%
as organic binder. The produced activated carbon fibers did of methyl cellulose from 4 wt% to 5 wt%, the coater adsorbent
not have good coverage with the adsorbent mixture in this mixture was semi-plastic and the coating was impossible.
composition of methyl cellulose. On the other word, the To compare the adsorption properties of the coated fibers,
adsorbent mixture in this case could not fill the voids the parameter of “adsorption capability” was defined to
between the fibers and the coating quality was poor. The show the effects of both adsorption and coating quality of
experiments were continued for the adsorbent mixture produced fibers. Adsorption capability parameter depends
containing 2 wt% for methyl cellulose and various wt% of on both iodine number of the adsorbent mixture and the
activated carbon. Poor coating quality was also observed in weight percent of the adsorbent mixture coated on the fibers.

Figure 2. SEM images of the coated fibers, (a) 3 wt% methyl cellulose and 15 wt% activated carbon, (b) 3 wt% methyl cellulose and
20 wt% activated carbon, and (c) 3 wt% methyl cellulose and 25 wt% activated carbon.
546 Fibers and Polymers 2015, Vol.16, No.3 Navid Saeidi and Mohammad Nader Lotfollahi

Actually, adsorption capability was defined to identify the than 50, 90 and 150 µm, and activated carbon particles
adsorption properties of the finished products and raw without any screening with particle sizes up to 109 µm was
material. It means that the parameter determines what the also used. Then, SACFs were prepared using these different
adsorption capacity of the coater mixture is and how many types of powder activated carbon. To prepare the coater
grams of the mixture are coated on a certain surface of the E- adsorbent mixture (activated carbon, methylcellulose and
glass fiber. Therefore, the adsorption properties of finished water), four types of powder activated carbon were individually
products are determined using a relation depending on applied. Adsorption capacity, surface area, and mechanical
adsorption properties of the coater adsorbent mixture, which properties of the prepared SACFs were measured and
can be called raw material, weight of the coated adsorbent compared with the products reported in the literature.
mixture and a certain surface of the E-glass fiber. The Table 2 shows iodine numbers of different adsorbent
adsorption capability (mg/cm2) is defined as follows: mixtures. As can be seen in Table 2, for the adsorbent mixture
containing 3 wt% methylcellulose and 25 wt% activated
(a × b)
Adsorption capability = --------------- (1) carbon, the iodine number of the coater adsorbent mixture
c
was increased from 1316.211 mg/g to 1335.621 mg/g by
where a denotes iodine number of the coater adsorbent decreasing activated carbon particle size from 150 µm to
mixture (mg/g), b denotes weight of the coated adsorbent 90 µm. However, when activated carbon particle size was
mixture (g) and c denotes surface of the fiber (cm2). decreased from 90 µm to 50 µm, iodine number of the coater
To this work, the powder activated carbon was screened to adsorbent mixture was decreased from 1335.621 mg/g to
obtain three types of activated carbon including particles less 1308.897 mg/g. In brief, the coater adsorbent mixture

Table 2. Iodine number and adsorption capability of the coated fibers


Activated carbon Iodine number of the Weight of the coated Adsorption
wt% wt% a
Sample particle size adsorbent mixture adsorbent mixture capability
methyl cellulose activated carbon 2
(µm) (mg/g) (g) (mg/cm )
1 3 25 150 1316.211 1.834 201.161
2 3 25 90 1335.621 1.843 205.129
3 3 25 50 1308.897 1.848 201.570
@
4 3 25 Various 1324.551 1.829 201.883
5 4 25 150 1310.347 1.919 209.546
6 4 25 90 1322.235 1.929 212.549
7 4 25 50 1294.886 1.941 209.447
@
8 4 25 Various 1314.892 1.916 209.944
9 3 20 150 1305.452 1.442 156.871
10 3 20 90 1319.276 1.461 160.621
11 3 20 50 1290.231 1.447 155.580
@
12 3 20 Various 1308.762 1.439 156.942
13 4 20 150 1289.742 1.581 169.923
14 4 20 90 1311.445 1.588 173.547
15 4 20 50 1269.121 1.601 169.321
@
16 4 20 Various 1297.711 1.578 170.649
17 3 15 150 1305.322 1.043 113.454
18 3 15 90 1309.623 1.127 122.995
19 3 15 50 1290.762 1.031 110.897
@
20 3 15 Various 1295.234 1.029 111.066
21 4 15 150 1271.198 1.164 123.306
22 4 15 90 1275.445 1.211 128.713
23 4 15 50 1263.112 1.215 127.890
@
24 4 15 Various 1283.342 1.199 128.227
a @
Weight of the coated adsorbent mixture (g)=Weight of the coated fiber (g)−Weight of the fiber before coating (g), Activated carbon with
mean particle size up to 109 µm.
Improvement of Semi Activated Carbon Fiber’s Properties Fibers and Polymers 2015, Vol.16, No.3 547

Table 3. Surface area of the samples synthesized in this work and


other works
BET surface area
Sample 2 Synthesis method
(m /g)
1 810 Present work
2 910 Present work
3 780 Present work
4 867 Present work
5 785 Present work
6 870 Present work
7 720 Present work
8 796 Present work
[10] 430 Coating inorganic fibers
Figure 3. Comparison between iodine numbers of the sieved [10] 730 Coating inorganic fibers
activated carbon and the adsorbent mixtures.
[14] 450 Electrospinning
[14] 550 Electrospinning
containing activated carbon with 90 µm particle size has the [15] 622 Electrospinning
largest iodine number. The same trends were obtained about [28] 340 Molding process
the coater adsorbent mixture containing 4 wt% methyl [28] 482 Molding process
cellulose and 25 wt% activated carbon. In addition, decrease
[28] 576 Molding process
of activated carbon content from 25 wt% to 20 and 15 wt%
didn’t affect on the observed behaviors of the samples [29] 280 Spinning
containing 3 and 4 wt% methylcellulose and 25 wt% activated [30] 675 Activation of PAN fiber
carbon (Table 2). [30] 536 Activation of PAN fiber
Figure 3 illustrates a comparison between iodine numbers [31] 458 Activation of kevlar fiber
of the sieved activated carbon (Table 1) and the coater [31] 251 Activation of kevlar fiber
adsorbent mixtures (Table 2). As can be seen in Figure 3, the [31] 403 Activation of kevlar fiber
iodine number of the activated carbon has an ascendant
[32] 527 Activation of oil-based pitch
trend by decreasing the powder activated carbon particle
size. But in both the adsorbent mixtures (containing 3 and [33] 718 Activation of pitch-based fiber
4 wt% methyl cellulose, and 25 wt% activated carbon), [34] 750 Activation of a kind of sponge
iodine number was increased with decreasing the activated
carbon particle size from 150 µm to 90 µm, and when the
activated carbon particle sizewas decreased from 90 µm to screening (samples 4 and 8). The highest surface area is
50 µm, it was also decreased. obtained as sample 2 prepared by the coater adsorbent
Table 2 also shows weight of the coated adsorbent on the mixture containing 3 wt% methyl cellulose and 25 wt%
fibers and the adsorption capability. As can be seen in table powder activated carbon having particle sizes less than
2, the weight of coated adsorbent mixture was increased by 90 µm. Recently, some researchers used oil-based pitch to
decreasing activated carbon particle size. The obtained synthesize activated carbon fibers [32]. However, the
results showed that a decreasing effect of activated carbon surface area of their produced sample, 527 m2/g, is much
particle size on iodine number was higher than its effect on lower than the samples produced here. In other reported
the weight of coated adsorbent mixture. The highest fiber’s work, Wang et al. [33] synthesized ACF using a pitch-based
adsorption capability was attained in the coated fiber with fiber. The reported surface area of their sample is up to
the adsorbent mixture containing 4 wt% methyl cellulose 718 m2/g, which is lower than the produced fibers in the
and activated carbon (25 wt%) with 90 µm particle size. In present work. The nearest surface area, which is up to
other hand, the adsorption capability of the coated fibers was 750 m2/g, to the sample which is named 2, having surface
improved by using the sieved activated carbon in preparing area equal to 910 m2/g, is regarding a fiber produced using
the coater adsorbent mixture. activation of a kind of sponge [34]. Totally, it can be said
Table 3 compares surface area of the coated fibers with that the surface area of the samples prepared in the present
other produced fibers reported in the literature. The surfaces work is higher than that of other compared works. Finally, it
area of the fibers coated by screened activated carbon are is obvious that the proposed SACF in the present work
higher than that of coated by activated carbon without any performed better than the existing one.
548 Fibers and Polymers 2015, Vol.16, No.3 Navid Saeidi and Mohammad Nader Lotfollahi

Table 4. Weight loss of the coated fibers after 20 minute flowing of content. Therefore, the coated fiber with the adsorbent
air (165 lit/min) mixture containing methylcellulose 4 wt% and activated
wt% wt% Activated Weight loss after carbon 15 wt% with particle sizes less than 50 µm had no
Sample methyl activated carbon particle 20 minutes weight loss. Also, the coated fiber by the coater adsorbent
a
cellulose carbon size (µm) flowing of air (g) mixture containing 3 wt% methylcellulose and 25 wt%
1 3 25 150 0.011 activated carbon with various particle sizes (mean particle
2 3 25 90 0.009 size up to 109 µm) had the highest weight loss. Briefly, the
weight loss of the coated fibers was decreased by using the
3 3 25 50 0.005
@
sieved activated carbon in preparing the coater adsorbent
4 3 25 Various 0.012
mixture.
5 4 25 150 0.009
6 4 25 90 0.008 Conclusion
7 4 25 50 0.002
8 4 25 Various @
0.010 In this work, the effects of activated carbon particle size
9 3 20 150 0.008 on adsorption and mechanical properties of SACFs were
studied. The SACF coated by the adsorbent mixture containing
10 3 20 90 0.007
4 wt%methylcellulose and 25 wt% activated carbon with
11 3 20 50 0.006 particle sizes less than 90 µm had the highest adsorption
@
12 3 20 Various 0.010 capability and surface area. Therefore, the adsorption capability
13 4 20 150 0.007 and surface area of the prepared SACFs were promoted by
14 4 20 90 0.007 sieving the powder activated carbon. In addition, it was
15 4 20 50 0.005 found that the weight loss of the SACFs after 20 minutes
16 4 20 Various @
0.008
flowing of air (165 lit/min) was decreased by decreasing
activated carbon particle size. Also, decreasing of activated
17 3 15 150 0.007
carbon content and increasing of methylcellulose content led
18 3 15 90 0.005 to decrease the weight loss. Therefore, the SACF coated by
19 3 15 50 0.004 adsorbent mixture containing 4 wt% methyl cellulose and
20 3 15 Various @
0.007 15 wt% activated carbon with particle sizes less than 50 µm
21 4 15 150 0.004 had the lowest weight loss (equal to zero).
22 4 15 90 0.002
23 4 15 50 0.000
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@
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