INTERNATIONAL JOURNAL OF SCIENTIFIC & TECHNOLOGY …...Neza Rahayu Palapa, Suheryanto, Risfian...

INTERNATIONAL JOURNAL OF SCIENTIFIC & TECHNOLOGY RESEARCH VOLUME 9, ISSUE 09, SEPTEMBER 2020 ISSN 2277-8616

154 IJSTR©2020 www.ijstr.org

Utilization Of Biochar Derived Indonesian Rice Husk As Adsorbent Of Malachite Green Removal

In Aqueous Solution

Neza Rahayu Palapa, Suheryanto, Risfian Mohadi, Addy Rachmat, Aldes Lesbani

Abstract: In this work, biochar (BC) was obtained from rice husk (RH) local paddy field and prepared by pyrolysis method as adsorbent of malachite green (MG). The characterization of BC was conducted by XRD, FTIR, BET, SEM-EDX analyses and TGDTA. BC was applied as adsorbent of MG from aqueous solution. BC was confirmed by X-ray diffractograms with broad reflection (002) at 24

o and the presents of organic bonds vibration from FTIR

spectra. Surface area analysis showed rice husk after pyrolysis was increases to 72.25 m2/g from 7.08 m

2/g. The TGA showed two step oxidation and

DTA presents the exothermic process. The result of the adsorption study indicated the BC follows pseudo-second-order (PSO) after equilibrium state at 90 min with dye uptake 89.48 mg/L. The isotherm model follows Langmuir with the maximum adsorption capacity of MG using BC uptake is 105.263 mg/g higher than raw material 31.419 mg/g. The thermodynamic analysis indicates that the MG adsorption is spontaneous, endothermic and based on XRD and FTIR characterization, no obvious changes after MG adsorption. Index Terms: Rice Husk, Biochar, Adsorbent, Malachite Green, and Adsorption

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1. INTRODUCTION SYNTHETIC dyes wastewater has been considered as an environmental problem and contaminates water for long time [1]. The main source of synthetic dyes wastewater is textile, paper, pulps, paints, and cosmetic industries [2]. Commonly, synthetic dyes have high resistance against oxidizing agents, hardly biodegradable, high toxicity and irritant substance to eye and skin contact [3]. The elimination of malachite green (MG) in wastewater therefore become a necessity and had to be done. Several techniques such as adsorption [4], bioremediation [5], chemical decomposition and also membrane fluctuation have been used to remove dyes from aqueous solution [6]. Due to economically, easy to operate, and high effectivity to remove toxic pollutants, the adsorption is considered as a recommended technique to remove pollutants in water [7]. The uses of bio-sorbent of natural material may have prospect as generous sorbents [8]. Due to their affordable, after these materials have been escalated. However, generally, these inexpensive sorbents have commonly low adsorption capacities and oblige large quantity of adsorbents. Therefore, there is a special demand to discover new, low budget, easily obtainable and effective adsorbents for useful application [9]. The use of activated carbon has been found to be effective, although these materials was expensive and perhaps because it is obtained from not able to be renewed material sources such as coal, and also because of the manufacturing process needs a prominent count of energy [10]. The production of

activated carbon called biochar from agricultural organic waste has been investigated such as rice husk [11], sawdust [12], coffee husk [13], cassava peel [14], coconut shell [15], nut shell [16], bamboo [17], orange peel [18], and crab shell [9] have been widely examined for the removal of dye. Biochar of Pomelo peel had been studied for methyl orange adsorption by Zhang et al. [19] which is has maximum adsorption capacity 163 mg/g. Liu et al. [20] also reported the wheat straw biochar was conducted into methylene blue solution with adsorptive capacity 16.92 mg/g. The MG adsorption studied by Hameed and El-Khaiary [21] using rice straw biochar and obtained maximum adsorption capacity 148 mg/g. On the other hand, MG has been studied by groundnut biochar and obtained 94% adsorbed after 15 minutes from 100 mg/L [22]. Sewu and co-workers [23] also investigated that woodchip biochar was adsorbed crystal violet in aqueous solution with adsorption capacity 195 mg/g. Zazycki and others [16] reported that biochar from pecan nutshell was examined as adsorbent of reactive dye with adsorption capacity approx. 130 mg/g. In agricultural countries such as Indonesia, where greatly provenance of biomass is available biosorption is prospering more and more appealing. Rice husk can demonstrate to be a preferable alternative to adsorption process because it is straightly available where agriculture is surrounded by major business. It is inexpensive and represents great adsorption capacity as properly handled [24]. In a research experiment, all of the important variables are examined. The main interaction variables with adsorbent and adsorbate to determine the adsorption process for example, time adsorption, dye concentration and temperature. The regeneration of adsorbent was identified in order to economic point of view for the industrial and larger scale practical applications.

2 EXPERIMENTAL SECTION 2.1 Preparation and characterization of biochar derived

Indonesian rice husk The rice husk (RH) was obtained from Indonesian local production in Central Java, Bukata Organic. The raw material was dried at 60

oC prior pyrolysis treatment. The pyrolysis

treatment was conducted in furnace at constant N2 flow for two

———————————————— Neza Rahayu Palapa is doctoral students in Department of Mathematic

& Natural Science, Universitas Sriwijaya, Indonesia. E-mail:, [email protected]

Tarmizi Taher and Bakri Rio Rahayu are analyses team member of Research Center of Inorganic Materials and Complexes, Universitas Sriwijaya, Indonesia. E-mail: [email protected] and [email protected]

Risfidian Mohadi, Suheryanto and Addy Rachmat are senior Lecturer in Department of Mathematic & Natural Science, Universitas Sriwijaya, Indonesia. E-mail: [email protected], [email protected], [email protected]

Aldes Lesbani as Corresponding Author is Professor in in Department of Mathematic & Natural Science, Universitas Sriwijaya, Email:

[email protected]

mailto:[email protected]:[email protected]:[email protected]:[email protected]:[email protected]:[email protected]:[email protected]



hours at 500oC with reactor heating rate 10

oC/min. Then, the

reactor was cooled down to room temperature. Biochar (BC) was characterized by XRD Rigaku Miniflex-600, FTIR Shimadzu Prestige-21, morphology analysis by SEM Quanta-650 Oxford instrument, surface area analysis and thermal analysis by Shimadzu DTG-60H instrument. 2.2 Batch Adsorption Experiments The adsorption experiments were studied through adsorption kinetics, adsorption isotherm, and adsorption thermodynamics. The various of initial concentration, adsorption time and temperature batch system were studied. The concentration of MG on solutions after adsorption was measured by a UV–vis spectrophotometer Bio-Base BK-UV 1800 PC at 619 nm.

3 RESULTS AND DISCUSSION 3.1 Characterization of rice husk and biochar The FTIR spectra and XRD pattern of RH, BC before and after adsorption of MG were shown in Fig.1. The absorption from vibration bands of RH and BC indicated these materials before adsorption and after adsorption had no obvious changes. Fig.1.A showed broad band at 3448/cm presents of O-H vibration and Si-O vibration from silica band at 470/cm. The low vibration at 794/cm presented the ring C-H deformation or C-H wagging. Other vibrations at 1103/cm assigned the symmetrical C-O band; 1620/cm denotes the formation of oxygen function group such as carboxylic C=O stretching and aromatic C=C stretching. According to [25], the presents of low vibration at 1434 and 2924/cm indicated the asymmetric of C-H. After adsorption of MG, the similar peaks were observed. However, the intensity of O-H vibration and C-H asymmetric was slow decreased and appeared a new peak at 1382/cm denotes C-N vibration. The XRD pattern of RH and BC are shown in Fig 1.B. The pattern of before and after adsorption has no significant changes and all samples indicated are completely amorphous by the featureless diffractograms and

the appearance of a diffuse maximum 23° at 2 reflection 002 typical for amorphous silica and did not show crystalline structure.

Fig. 1 FTIR spectra and X-ray diffraction pattern of RH, BC

before and after adsorption of MG

The characterization of materials’ morphologies was presented in Fig. 2. The appearance of rice husk before and after pyrolysis was investigated in Fig. a and b. Fig. 2c showed the morphology of rice husk before pyrolysis which is the rice husk had uniform globular structure with lemma and palea is the main components. [26] confirm the main composition of RH is lemma and palea with prominent globular predominate morphologies. Fig. 2.d showed the morphology of BC had small pore with cylindrical holes interconnected by some large holes. In other hands, the morphology of BC in low

temperature pyrolysis (300-350o) caused the pores were not

fully developed and de-uniform of pore structure of rice husk biochar. The composition of RH and BC was described by EDS (Fig. 2.e and f). According to [27], the main contain of RH is silica in combination with a large amount of the lignin and after pyrolysis the silica properties were increased. Fig. 2 Morphology images and composition of rice husk and

rice husk biochar The surface area analysis of RH and BC was listed in Table 1. The BET surface area of BC was 72.25 m

2/g with the pore size

is 3.33 nm indicated the mesopore characterization. Nitrogen adsorption desorption of RH and BC were presents in Fig. 3. The nitrogen adsorption-desorption curve indicates type IV, indicating a mesoporous material. The hysteresis loop of the materials is H3-type, consistent with a cavitation-induced desorption branch lower limit of (P/P0) > 0.42. The H3 hysteresis explains the binding strength of anions located in the interlayer. However, Fig.3.b the presents of characteristic of step-down (shoulder) observed at 0.8-0.85 (P/P0) as similar reported as [28] indicated to the complexity of capillary condensation in pore networks with the cavitation induced evaporation effect. Table 1. The surface area analysis results of rice husk biochar

Adsorbent Surface Area Pore Size Pore Volume m

2/g nm cm

3/g

Rice Husk Biochar 72.25 3.33 0.060 Rice Husk 7.08 3.14 0.011



Fig. 3 Adsorption-desorption of nitrogen plot into (a) rice husk

biochar and (b) rice husk

Fig. 4 TGDTA curve of a) rice husk and b) rice husk biochar

Thermogravimetric of RH and BC has been investigated the loss-mass of lignin-cellulose by TGA as presents in Fig.4. Firstly, the loss-mass of rice husk is up to 100

oC due to

moisture content and hemicellulose decomposition at 200-350

oC and appearance of indentation after 380

oC attributed

the lignin-cellulose maximum decomposition. Similar reported by [29] the material had decomposition of hemicellulose, cellulose and lignin at 270-385

oC. The TGA curve of BC also

has two steps, the first steps denote oxidation of organic compounds and DTA curve shows exothermic process. The second peak may be attributed to the oxidation of cellulose and bonding of organic molecules. 3.2 The effect of time adsorption and kinetics adsorption

study Next, the effect of contact time between MG solution and adsorbent was investigated. According to the obtained result that is displayed in Fig.5.a it is evident to the adsorption process was extremely affected by the contact time. The MG removal efficiency gradually increased by increasing contact time before eventually reached it maximum adsorption capacity after 90 min with dye adsorbed was 56.21 mg/L and 89.48 mg/L. Moreover, it can also be observed that in the initial state, the adsorption process was conducted rapidly within the first 50 min. Afterward, it was slightly conducted before reached equilibrium time. The kinetics of MG adsorption onto RH and BC were determined using the two most studied kinetics model called the pseudo-first-order (PFO) and pseudo-second-order (PSO) model. This investigation was attended to examine the mechanism that controls the adsorption process weather a mass transfer, chemical reaction, or diffusion [30]. The linear plot of the

employed model, as well as the fitted model against the experimental data, are presented in Fig.6. and the calculated kinetics parameter of MG adsorption is presented in Table 2. It was observed that both models exhibited a good linear regression against the experimental data. However, the PSO model showed a much better correlation coefficient (R

2) that

very close to one. The predicted adsorption capacity of the adsorbent based on the PSO model also indicated much closer to the real experimental value as well as the graph of the fitting model against the experimental data as can be seen in Fig.5b. These findings suggested that the adsorption of MG by RH and BC was described and followed the PSO model rather than the PFO. Regarding this result, assumed that the adsorption process was mainly governed by chemisorption or chemical interaction [31].

Fig. 5 The effect of contact time adsorption and kinetic fitted

model adsorption of rice husk and rice husk biochar

Fig. 6 The plot of a) RH pseudo-first-order, b) RH pseudo-second-order, c) BC pseudo-first-order and d) BC pseudo-

second-order kinetics model

Table 2. Adsorption kinetics parameter of MG using RH and BC

Adsorbent Pseudo-first-

order Value

Pseudo-second-

order Value

RH 𝑘 (1/min) 0.024 𝑘 (g/mg min)

0.014

𝑞 (mg/g) 43.260 𝑞 (mg/g) 61.958 𝑅 0.935 𝑅 0.996

BC 𝑘 (1/min) 0.023 𝑘 (g/mg min)

0.0030

𝑞 (mg/g) 31.975 𝑞 (mg/g) 97.390 𝑅 0.876 𝑅 0.999



3.3 Equilibrium study, isotherm adsorption,

thermodynamic parameter and regeneration study The adsorption isotherm equilibrium was investigated at different initial MG concentration. Two adsorption isotherm models namely Langmuir and Freundlich's isotherm were applied to the obtained experimental data. The Langmuir isotherm model was designed for describing monolayer adsorption that occurred in the homogenous surface. This model is provided as [32]:

=

+

⋅

(1)

Where 𝑞 is the maximum adsorption capacity conducted in the monolayer (mg/g), b is the Langmuir adsorption equilibrium constant (1/mg), and 𝐶 is the equilibrium MG concentration (mg/L). The isotherm parameter based on the Langmuir model was determined from the slope and intercept values of the 1/qe vs 1/Ce plot. Next, the Freundlich adsorption isotherm model was employed. This model basically was used to describe an adsorption phenomenon that occurred in the heterogeneous surface in which the adsorption capacity is related to the used dye concentration [4]. The linear form of the Freundlich model can be written as follow:

ln 𝑞 = ln𝐾 + (

) ln 𝐶 (2)

Where 𝐾 and n is the Freundlich constant corresponds to the

adsorption capacity and adsorption intensity, respectively. These parameters can be described from the plot ln 𝑞 against ln 𝐶 as slope and intercept. The adsorption isotherm parameters of MG using RH and BC are presented in Table 3. From the value of the regression coefficient (R

2), it can be

concluded that the adsorption mechanism was best described the Langmuir model rather than the Freundlich model. This result indicated that the adsorption process was conducted in the monolayer surface. Moreover, this finding also in accordance with the predicted kinetics model that assumed that the adsorption process was conducted chemically [33]. Table 3 also shown the maximum adsorption capacity of BC increased slightly to 105.263 mg/g from 31.419 mg/g for RH.

Table 3. Isotherm parameters of MG adsorption using RH and

BC Adsorbent

Langmuir Freundlich

𝑞 𝐾 𝑅 𝐾 n 𝑅

RH 31.419 0.728 0.999 12.246 3.582 0.975 BC 105.263 0.508 0.994 21.591 9.104 0.971

The thermodynamic was calculated in this research such as enthalpy (ΔH), entropy (ΔS) and Gibbs energy (ΔG). Thermodynamic parameter was calculated in order to determine and examine the adsorption process which is spontaneous or not. the tendency of the spontaneous of chemic reaction was studied by ΔG. According to [34], both, ΔH and ΔS parameters were evaluated so as define ΔG from adsorption process. Reactions take place spontaneously at a specified temperature if ΔG is a negative quantity. The characteristic denomination of the thermodynamic parameters for adsorption of MG onto BC are listed in Table 4. The result of thermodynamic study, the reduced in the negative value of ΔG with a rise in temperature exhibit that the favorable state from adsorption process is on high temperature. These

occurrences were developed because of the movability of MG molecules liven up with an increase in temperature and that the resemblance of sorbate on the sorbent is higher at high temperatures. Concluded, a reduction of the negative ΔG value with an increase in temperature interprets that higher temperature causes the adsorption easier. Table 4 also represents the value of ΔH is positive and presents an endothermic adsorption process. A positive value of ΔS describes the affinity of the adsorbent to the adsorbate molecules. Futhermore, positive value of ΔS indicates increased randomness at the solid/solution interface with some structural changes in the adsorbate-adsorbent and this phenom corresponds to an increase in the degree of freedom of the adsorbed molecules [35].

Table 4. The thermodynamic parameter of MG adsorption using BC

Adsorption Temperature

∆H (kJ/mol) ∆S (kJ/mol) ∆G (kJ/mol)

30 C 8.916 33.441 -1.216

40 C -1.551

50 C -1.718

The regeneration study was determined in order to economic point of view for the industrial and larger scale practical applications [36]. The main characteristic of an efficient adsorbent is the reusability of adsorbent with significant adsorption capacity and restoration of original characteristic properties of adsorbent before reuse. Thus, an expeditious adsorbent should be showed an excellent performance in the adsorption-desorption process. The desorption study was conducted using ethanol as eluents of MG dye desorption process.

Fig. 7 Reusability of rice husk and rice husk biochar The results shown in Fig.7. presents BC has stronger and higher effectivity to adsorb significant amount of MG molecule than RH when applied in repeated cycles. The efficiency of BC decreases in the second cycle to 46.17%, third 18.39% and fourth 3.90%. Furthermore, the fourth regeneration of RH was not determined because of a very small amount of MG was adsorbed in the third cycle, probably due to small amount could easily be removed from the surface and identified RH cannot adsorb MG molecule anymore. However, the overall regeneration ability of BC is relatively higher and sustainable than RH.



4 CONCLUSION Rice husk biochar were successfully prepared by pyrolysis method and applied as adsorbent for MG removal. The ability of RH and BC to adsorb MG from water has been explored. The extent of removal depended on time adsorption, initial concentration and temperature adsorption. The kinetic parameter was described by PSO with qeexperiment and qecalculation are closed after equilibrium state at 90 min with dye uptake 89.48 mg/L. The adsorption process followed the Langmuir isotherm with the maximum adsorption capacity of MG using BC uptake is 105.263 mg/g higher than raw material 31.419 mg/g. The process was endothermic in nature and more favorable at higher temperatures. The results showed that BC has been successfully used as an adsorbent for the removal of MG in wastewater even regeneration ability of BC is relatively high and sustainable.

ACKNOWLEDGMENT This study was supported ―Hibah Profesi‖ Universitas Sriwijaya in fiscal year 2019-2021 by the financial support program for research with contract number 0014/UN9/SK.LP2M.PT/2019. Authors also thank Research Center of Inorganic Materials and Complexes FMIPA Universitas Sriwijaya for instrumental and analysis support.

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