CHAPTER - 3 ADSORBENT CHARACTERISTICS
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1 CHAPTER - 3 ADSORBENT CHARACTERISTICS In the present work five categories of activated carbon were prepared from Ananas Comosus L by different methods. Out of five activated carbons, one superior quality carbon was selected for the adsorption studies of four classes of dyes namely acid dye ( Acid Green 25), basic dyes (Basic Yellow 2 and Ethyl Violet), reactive dye (Reactive Orange 16) and direct dye (Direct Brown 2) through batch and column mode. Effluent samples from fabric dyeing industry were also treated using the selected activated carbon and cost of effluent treatment was also analyzed General Physico-Chemical Properties The various physico chemical properties of the five activated carbon prepared from Ananas Comosus L leaves by various methods are presented in Table 3.1. In chemical activation, different activating agents are expected to significantly affect the extent of activation [1]. In the present study, activation with H 2 SO 4, ZnCl 2, H 3 PO 4, H 2 SO 4 & H 2 O 2 and KOH were evaluated and compared. The ph values of the carbon prepared by acid processes ACC1 and ACC3 were less than 7.0 (i.e acidic). This may be due to the introduction of acidic groups on the surface of activated carbon. ACC5 was basic in nature. The acid or basic nature of an activated carbon depends on its preparation, inorganic matter and chemically active oxygen groups on its surface as well as the kind of treatment to which the activated carbon was subjected. Generally, neutral ph is preferred for the wastewater treatment as higher or lower ph affects the adsorption process and influences the ph of the treated water. The ph of the activated carbon affects the adsorptive property of the carbons, as highly acidic or basic carbons are undesirable for processing. 77
2 The details of functional groups present in the surface of carbon is not clear, however, the possible reactions during chemical activation of pistochio-nut shells using KOH were reported by Yang [2]. Radhika and Palanivelu [3] have reported the ph of the activated carbon above 7.0 during the activation of coconut shell carbon by KOH. The activated carbons ACC2, ACC4 and ACC5 show higher conductivity and ACC1 shows moderate conductivity. Conductivity measures the water leachable minerals. These minerals are generally not desirable in any application because, it may cause specific problems with catalysis of adverse reactions or interference by competitive adsorption [4]. In order to improve the adsorption performance, the activated carbon with higher conductivity will have to be pre-washed, making the treatment process cumbersome and expensive. Therefore, it is desirable to use activated carbon with low conductivity. Comparatively, ACC3 has very low conductivity than other activated carbon, which is being preferred to use as adsorbent for the removal of dyes. High content of volatile matter, fixed carbon (64-68% ) and low ash were also reported as favourable properties of the precursors for the production of activated carbon [5]. The ph of the granular activated carbon is influenced by the ash content. Ash content is the measure of minerals as impurities present in the carbon. They are the residues, which remain upon the burn off of the carbonaceous portion during pyrolysis. The ash content of the activated carbon depends on the precursor and is positively correlated to ph [6]. Among the five varities of activated carbon prepared except ACC3, all have more than 15% ash content, which may be incorporated by the activating agents. Therefore, materials with lowest ash content precursor are 78
3 preferred in order to have the most active sites on the surface of the activated carbon. High ash content ultimately reduces the fixed carbon percentage. The agricultural by-products could thereby be used as renewable resources, as they are desirable for carbon precursors because of their low ash content and high bulk density [7]. Activated carbon derived from most of the naturally occuring plants and agro products have high percentage of volatile matter. This is due to the presence of more volatile organic compounds in the precursor. Solubility studies of carbon in water and acid were performed separately to evaluate the amount of impurities present in the carbon prepared by different carbonization processes, this may affect the quality of treated water during the process. From the data, it is clear that all the carbons have very low level of water soluble matter and acid soluble matter. Generally, an adsorbent bulk density is an important parameter. The American Water work Association has set a lower limit of bulk density at 0.25 mg/ml for granular activated carbon to be of practical use [8]. The bulk density values of all carbons are found only in a narrow range, indicating that activating agents have a least role in altering the bulk density and more over, it depends on the nature of precursor. An adsorbent with high bulk density need not be regenerated frequently because it can hold more adsorbate per unit weight [9]. The bulk density of the prepared sample used for this work is within that limit, which is 0.43 mg/ml Adsorptive properties are directly related to the porosity of activated carbon, as the highly porous carbon adsorb relatively large amount of organic compounds. ACC3 is one of the highly porous carbon among the five varieties. The above said 79
4 factor was supported by fact that H 3 PO 4 activated carbon has highest surface area of 808 m 2 /g. The iodine value of the activated carbons changed significantly with activating agents. Iodine number can be correlated with the ability of a carbon to adsorb low molecular weight substance. As I 2 molecule is relatively small, it provides a measure of surface area or capacity to adsorb small adsorbates. Iodine number for commercial adsorbent ranges from 300 to 1200 mg/g (10). Moreover, the H 3 PO 4 activated carbon has the highest Iodine value of 948 mg/g indicating that its pore surface and structure are the best developed. The activation with H 3 PO 4 gave the highest yield of 54.6%. Thus, H 3 PO 4 activated carbon (ACC3) was chosen for the subsequent experiments. Methylene blue number and phenol number give an indication of ability of a carbon to adsorb high molecular weight substance like dye molecule, ACC2 and ACC3 shows methylene blue number of greater than 200, indicates that the carbon is good for dye adsorption. The level of sodium is low in all types of carbon. High level of potassium was noticed in carbons prepared by KOH,H 2 SO4 and H 2 O 2 impregnation method. This can be taken as advantage for ion exchange process and for the removal of cations in wastewater Surface characteristics studies (SEM analysis) The SEM was used to get proper images of samples at the microscopic level. These images are primarily used to determine the structure and distribution of the pores that are present on the surface of the activated carbon. It also determines the nature and the size of the pore, depending on the magnification of the image taken. 80
5 The SEM images of activated carbon produced using sulphuric acid (ACC1), zinc chloride (ACC2), phosohoric acid (ACC3), sulphuric acid & hydrogen peroxide (ACC4), potassium hydroxide (ACC5) are depicted in Figs 3.1 to 3.5. It is evident from the SEM images that a wide variety of pores are present in activated carbons along with fibrous structure in ACC1 to ACC4. Small cavities, pores and more rough surface on the carbon sample indicate the presence of interconnect network. Tubular pores and cavities will increase the surface area of the adsorbent. ACC3 with 2500x & 5000x magnification clearly shows relatively porous with wide ranging cracks. The macropores are clearly visible, which helps the easy diffusion of dye molecules to the pore structure. Conversely, the surfaces of other carbons are smooth with limited macropores. This supports the results of iodine number of ACC3 being more than the other chemically activated carbons Sturctural Analysis FTIR Studies The IR spectra of Ananas Comosus L leaves activated carbon (ACC1 to ACC5) (Figs ) show the presence of the following groups. Absence of C-H and N-H peaks in most of the activated carbons proves that the solid surface of carbon is homogeneous. The activated carbon ACC1, ACC2 and ACC4 show a broad peak around 3313 cm -1 ; ACC2 and ACC5 show a broad peak around 3396 cm -1 and ACC3 shows a broad peak around 3422 cm -1 which are responsible for OH stretching vibration [11-13]. The position of the band is characteristic of the stretching vibration of hydroxy group while broadening of the band is indicative of high degree of association because of extensive hydrogen bonding. Thus, it is expected that the investigated carbons contain hydroxyl groups from carboxyl, phenol or alcohols. The existence of phenol is supported by O- H bending (1400 cm -1 ) vibrations. 81
6 The spectra of all activated carbons except ACC3 show a strong wide absorption band at 3200 cm -1 due to N-H symmetric stretching. Except ACC1 and ACC4, other carbons show a peak around cm -1 for C-H stretching vibrations. The peak corresponding to C-H bending at 1400 cm -1 and C-C stretching vibrations at 1040 cm -1 are exhibited by ACC3. The peak around cm -1 may be attributed to the carbon halogen vibrations (C-X). The peak at 598 and 680 cm -1 are assigned to the out of plane C-H bending mode. Except ACC4, C-H deformation is noticed between cm -1 in all the four activated carbons. The peak around 1580 cm -1 observed in ACC3 should be the characteristic of the C=O strtching vibration of lactonic and carbonyl groups. The peak appearing around 1338 cm -1 in all carbons is due to C-H deformation vibration in methyl group. A peak at 1670 cm -1 for all activated carbons except ACC3 is the characteristic peak for carboxylic C=O group. The C-H out of plane bending at 811cm -1 supports the presence of aromatic groups in the carbon structure. The region between cm -1 shows two bands at around 460 and 465 cm -1 which are associated with the in-plane and out of plane aromatic ring deformation vibrations [14]. ACC3 shows a charcteristic bands at 3787 cm -1 due to O-H stretching, the band at 3428 cm -1 represents O-H stretching vibrations of the carboxylic acid, the peak at cm -1 represents the C C stretching, peaks at cm -1 represents the C=C stretching, peaks appearing at 1441 cm -1 shows the C-H bond in CH 3. The presence of C-O stretching is indicated by the peaks at cm -1, cm -1 and 1022 cm -1. The peak at cm -1 is due to C-H deformation. The peak appearing at 598 cm -1 is assigned to C-P bonding. The broad peak around 1099 cm -1 in ACC3 can be assigned to stretching vibrations of P=O groups. 82
7 Based on the collective FT-IR data, the carbon prepared from H 3 PO 4 (ACC3) has high surface heterogenity which is useful for the multilayer adsorption of dye molecules. The surface heterogenity is due to the presence of the functional groups like C=O aromatic C=C, aromatic C-H, hydrogen bonded OH group, -P=O & C- P bonds. The results of characterization studies indicate that Ananas Comosus L leaves is a good precursor material for the production of activated carbon of high efficiency. Especially ZnCl 2 and H 3 PO 4 impregnation methods give more porous and high surface area carbon which is suitable for waste treatment. ACC3 carbon was selected as an adsorbent for all further adsorption experiments. The point of zero ph was estimated for the ACC3 and it was found to be X-Ray diffraction Studies X- ray diffraction pattern of the sample did not show any peak, thereby indicating the amorphous nature of the product. It does not give any major peaks which could be due to lack of inorganic and crystalline substance in the activated carbon Pore Characteristics of ACC3 Based on the physico-chemical characteristics, ACC3 (activated carbon prepared from H 3 PO 4 impregnation method) was selected for further adsorption studies. The N 2 adsorption-desorption isotherm studies were carried out only for ACC3 to find the pore size distribution characteristics and the results are presented in Table 3.2 A qualitative information on the adsorption process and the extent of surface area available to the adsorbate is given by the shape of the adsorption/desorption 83
8 curve. The N 2 adsorption/desorption isotherm of the activated carbon prepared from Ananas comosus leaves at ºC is shown in Fig.3.12.The adsorption isotherm is classified as type I isotherm indicating that the carbon is mainly microporous [15] in nature. The hysteresis indicates the presence of mesopores on the surface of the carbon. The amount of nitrogen adsorbed on the adsorbent gradually increases in the whole relative pressure range, implying that this carbon contains a small amount of mesopores. The prepared carbon exhibits a moderately developed porosity with a specific surface area of m 2 /g and the single point adsorption total pore volume of pores (< Å) is cm 2 /g. The BJH average pore radius (2V/A) is 8.5Å and median pore width determined by Horvath and Kawazoe is Å. The presence of micropores and mesopores in the activated carbon prepared from Ananas comosus leaves is given by pore size distribution calculated by Horvath and Kawazoe method and the differential pore volume plot is given in the Fig Effect of ph of adsorption of dyes onto ACC3 The ph of the system exerts profound influence on the adsorptive uptake of adsorbate molecule presumably due to its influence on the surface properties of the adsorbent and ionization/ dissociation of the adsorbate molecules. On the other hand, ph strongly influence the specifiation and adsorption availability of the dyes [16]. The effect of ph for the adsorption of the selected five dyes onto ACC3 over a ph range of 2 to 11 and the respective data are given in Table 3.3. The uptake of anionic dyes decreases and cationic dye increases when the solution ph was increased from 2 to 11. The effect of dye sorption by ACC3 strongly depends on the electrostatic attraction between dye and surface of the sorbent. 84
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