Title Science and Technology Indonesia e-ISSN:2580-4391 p-ISSN:2580-4405 Vol. 7, No. 4, October 2022 Research Paper Green Synthesis of Nickel Aluminum Layered Double Hydroxide using Chitosan as Template for Adsorption of Phenol Hasja Paluta Utami1, Nur Ahmad2, Zaqiya Artha Zahara3, Aldes Lesbani2,4, Risfidian Mohadi1,4* 1Magister Programme Graduate School of Mathematics and Natural Sciences, Sriwijaya University, Palembang, South Sumatera, 30139, Indonesia2Graduate School of Mathematics and Natural Sciences, Faculty of Mathematics and Natural Sciences, Sriwijaya University, Palembang, South Sumatera, 30139, Indonesia3Magister Programme in Environment Management, Sriwijaya University, Palembang, South Sumatera, 30139, Indonesia4Research Center of Inorganic Materials and Coordination Complexes, Faculty of Mathematics and Natural Sciences, Sriwijaya University, Palembang, South Sumatera, 30139, Indonesia *Corresponding author: risfidian.mohadi@unsri.ac.id AbstractIn present study, a modification of the NiAl LDH composite with chitosan was successful. Characterization was carried out usingX-rays, The results obtained show that there is an angle of 2\ at 11.57°(003); 22.91°(006); 35.04°(012); 39.73°(015); and 61.9°(110).The FT-IR spectrum of the Chitosan@NiAl LDH at Wavenumber 3448, 1635, 1543, and 601 cm−1. The NiAl LDH and chitosan have asurface area of 3.288 m2/g and 8.558 m2/g, respectively. An increase in the surface area of the composite Chitosan@NiAl LDH 9.493m2/g, all of adsorbents follow type IV isotherm based on the classification according to IUPAC. The optimum pH of the NiAl LDH atpH 3. The optimum pH for chitosan and chitosan@NiAl LDH material is at the optimum pH of 5. The kinetic and isotherm model inthe adsorption process is pseudo-second-order and Freundlich model, respectively. The maximum adsorption capacity of NiAl LDH,chitosan, and chitosan@NiAl LDH is 25.445, 23.753, and 33.223 mg/g, respectively. The increase in regeneration cycles causes adecrease in the percentage of adsorbed; sequentially, the percentage adsorbed during the fifth regeneration reaches 3.545, 1.966,4.309%, respectively. KeywordsLayered Double Hydroxide, Chitosan, Phenol, Adsorption Received: 15 August 2022, Accepted: 24 October 2022 https://doi.org/10.26554/sti.2022.7.4.530-535 1. INTRODUCTION Along with the increasing population and technological devel- opments, water pollution is one of the severe problems faced and has become a concern of manyparties. One of the harmful pollutants in the environment is phenol (Alves et al., 2019). Phenol waste can come from production processes in various industries such as metal smelting, plastics, polymers, pharma- ceuticals, paints, wood processing, organic pesticides, pulp, and paper (Dehmani et al., 2021b; Wang et al., 2022; Zhang et al., 2022). The presence of phenol in the environmenst, especially wa- ters, can disrupt aquatic ecosystems and human health (da Silva et al., 2022). United State Environmental Agency (USEPA) has limit concentration of phenol in water is 1 `g/L (de Farias et al., 2022). Therefore, to overcome the problem of envi- ronmental pollution, a solution is needed, one of which is the adsorption method (Khan et al., 2022). Adsorption has several advantages compared to other methods, including the rela- tively straightforward process, relatively high eectiveness, and eciency (Jain et al., 2022). The adsorbent dramatically determines the success of the adsorption process, which is characterized bya large adsorption capacity. Researchers have used many adsorbents to overcome environmental pollution problems, such as humic acid, zeolite, clay, activated carbon, chitosan, and layered double hydrox- ide (Lesbani et al., 2021). Layered double hydroxide (LDH) is an anionic clay material and hydrotalcite with the ability to exchange ions between layers, which has the general for- mula [M2+1−xM3+x(OH)2]x+[(An−)x/n·yH2O]x−, where M is divalent and trivalent metal cations (Bouteraa et al., 2020). Layered double hydroxides have been widely developed into adsorbents because they have good adsorption and uniqueness (Taher et al., 2021). The development of LDH composites was also carried out on a hydrochar basis. Research by Juleanti et al. (2022) compared the adsorption ability of Mg/Al, Ca/Al, and Zn/Al composites based on hydrochar on the absorption of direct https://crossmark.crossref.org/dialog/?doi=10.26554/sti.2022.7.4.530-535&domain=pdf https://doi.org/10.26554/sti.2022.7.4.530-535 Utami et. al. Science and Technology Indonesia, 7 (2022) 530-535 green dyes. The ability of these hydrochar-based compos- ites to have adsorption capacities of 94.34 mg/g on Mg/Al- hydrochar, 128.20 mg/g on Ca/Al-hydrochar, and 89.29 mg/g on Zn/Al-hydrochar. In addition, layered double hydroxide can be composited with chitosan. Chitosan is known to have theabilityasanadsorbent, so it canbeused toabsorbhazardous materials in some wastewater. According to Barbusiński et al. (2018), chitosan is a natural biopolymer that is well-known and good for water treatment. Chitosan has physical and chemical characteristics, chemical stability, high reactivity, high chela- tion properties, and high selectivity to pollutants (Seedao et al., 2018). In present study, a modication of the NiAl LDH compos- ite with chitosan will be carried out. The prepared composite materials were characterized using X-Ray Diraction (XRD), Fourier Transform Infra-Red (FTIR), and Brunauer Emmet Teller (BET). The resulting composite material will be applied as an adsorbent of organic compounds in the form of phe- nol. The adsorption parameters to be determined are kinetics, isotherms, and adsorbent regeneration. Determination of the adsorption parameters will be studied through variations in contact time, concentration, and temperature, as well as the desorption process. 2. EXPERIMENTAL SECTION 2.1 Chemicals and Instrumentation All chemicals; nickel hexahydrate (Ni(NO3)2.6H2O), alumi- num nitrate nonahydrate (Al(NO3)3.9H2O), sodium carbonate (Na2CO3) , chitosan, hydrogen chloride (HCl), distilled wa- ter (H2O), sodium hydroxide (NaOH), phenol (C6H5OH), 4-aminoantipyrine (C11H13N3O), potassium hexacyanofer- rate(III) (K3[Fe(CN)6]) , and acetate buersolution (CH3COO Na) pH 10. All instrumentation; X-Ray Diraction (XRD), spectrophotometerUV-Visible,BrunauerEmmetTeller(BET), and Fourier Transform Infra-Red (FTIR). 2.2 Synthesis of NiAl-LDH A total of 100 mL of a solution containing 0.75 M Ni(NO3)2. 6H2O was mixed with 100 mL of a solution containing 0.25 M Al(NO3)3.9H2O and then stirred for 30 min. Furthermore, the pH of the mixture was adjusted to reach pH 10 with the addition of 2 M NaOH. The resulting mixture was then stirred at a temperature of 65◦C for 24 h. The samples were ltered and washed with distilled water and then dried in an oven at a temperature of 100◦C. 2.3 Preparation Chitosan@NiAl LDH A total of 30 mL of 0.75 M Ni(NO3)2.6H2O were mixed into 30 mL of 0.25 M Al(NO3)2.9H2O solution, then stirred and added 3 gram chitosan. The NaOH solution with a concentra- tion of 2 M was slowly added to the mixture until it reached a pH of 10. Solids were formed after 3 days of stirring at a tem- perature of 80°C. Then the solid was ltered and washed with distilled water. The composite material obtained was dried at a temperature of 100°C. 2.4 Adsorption of Phenol Adsorption parameters were studied through pH, contact time, concentration, temperature, and regeneration process varia- tions. 0.02 g of adsorbent was put into an Erlenmeyer con- taining 20 mL of phenol. Adsorption was carried out with variations in pH (2-11), contact time (0-180 min), initial con- centration (10-30 mg/L), temperature (30-60°C), and regen- eration 5 cycles times. After that, the phenol solution was complex. The phenol complex process was conducted to Xie et al. (2020) by adding 1 mL of 5 mg/L phenol solution into a beaker. Then 0.1 mL of 2% 4-aminoantipyrine reagent was added, 0.1 mL of hexacyanoferrate (III) 8%, 1 mL of pH 10 buer solution and 3 mL of distilled water were added. Then the mixture was homogenized and allowed to stand for 5-10 minutes. Afterward, the phenol concentration was measured using a UV-Visible spectrophotometer at 505.2 nm. 3. RESULT AND DISCUSSSION CharacterizationwascarriedoutusingX-rays toproduceaNiAl LDH diractogram, as shown in Figure 1. The results obtained show that there is an angle of 2\ at 11.57°(003); 22.91°(006); 35.04°(012); 39.73°(015); and 61.9°(110). The success of the NiAl LDH synthesis can be proven by the research of Ahmad et al. (2022) according to JCPDS No.15-0087. The diraction pattern of chitosan at an angle of 2\= 7.93° and 19.35°. The 19.35° has a higher intensity than the peak of 7.93°. According to Billah et al. (2020), the angle is 2\ at= 10° and 20°, indicating that the chitosan material is classied as semi-crystalline by JCPDS data No.039-1894. The results of the characterization of Chitosan@NiAl LDH composites showed that the typical peaks of double-layer hydroxyl were shown at angles of 2\= 11.45° and 60.93°, while the typical peaks of chitosan were at angles of 2\= 22.5°. Figure 1. X-Ray Diractogram of Adsorbents Figure 2 shows the FT-IR spectrum of the Chitosan@NiAl © 2022 The Authors. Page 531 of 535 Utami et. al. Science and Technology Indonesia, 7 (2022) 530-535 Table 1. Brunauer Emmet Teller of Adsorbents Parameter NiAl LDH Chitosan Chitosan@NiAl LDH Surface Area (m2/g) 3.288 8.558 9.493 Pore Volume (cm3/g), BJH 0.006 0.018 0.031 Pore Size (nm), BJH 16.983 19.102 17.057 LDH composite material. Wavenumber 3448 cm−1 vibrations occur in the -OH group from water molecules. The O-H bending vibration in the NiAl composite is at a wavenumber of 1635 cm−1. The aromatic C=C group derived from chitosan is shown at the wavenumber 1543 cm−1. The nitrate group is at a wavenumber of 1543 cm−1, and the vibration for metal oxide is at a wavenumber of 601 cm−1. According to Cardinale et al. (2020), the NiAl LDH is in the wavenumber region of 3600 cm−1. The O-H bonds in each layer are at 1632 cm−1. The wavenumber of 1348 cm−1 has nitrate groups, and the wavenumbers of 749 and 652 cm−1 have metal groups. Figure 2. Fourier Transfer Infra-Red Spectrum of Adsorbents The graph nitrogen adsorption-desorption isotherms of NiAl LDH, chitosan, and chitosan@NiAl LDH can be seen in Figure 3. The graph shows that each material belongs to the type IV isotherm based on the classication according to IUPAC. Adsorption can be said to be a type IV isotherm if the adsorbent used has pores in the range of 2-50 nm, and there is an increase in adsorber absorption when the pores are lled with nitrogen (Asnaoui et al., 2022; Cao et al., 2022). The NiAl LDH and chitosan have a surface area of 3.288 m2/g and 8.558 m2/g, respectively. An increase in the surface area of the composite Chitosan@NiAl LDH 9.493 m2/g. Thus, from the data in Table 1, it can be conrmed that the LDH modication process with chitosan material was successfully carried out, characterized by an increase in surface area. Figure 3. Graph Nitrogen Adsorption-Desorption Isotherms of Adsorbents The eect of pH plays an essential role in the adsorption process (Qu et al., 2022). Figure 4 shows the optimum pH of the NiAl LDH at pH 3, with the adsorbed concentration reaching 13.355 mg/L. The optimum pH for chitosan and chitosan@NiAl LDH material is at the optimum pH of 5, with the adsorbed chitosan concentration of 10.414 mg/L, while chitosan@NiAlLDHof14.663mg/L.AccordingtoAl-Ghouti et al. (2022), when the solution’s pH is smaller or in an acidic solution state, the graphite oxide is positively charged, while in an alkaline solution or an alkaline solution, the surface of adsorbent is negatively charged. Therefore, the eciency of phenol adsorption decreases at alkaline pH conditions; this is due to the electrostatic repulsion between phenol and the negatively charged surface of graphite oxide. Figure 4. Eect of pH on Adsorption of Phenol © 2022 The Authors. Page 532 of 535 Utami et. al. Science and Technology Indonesia, 7 (2022) 530-535 Table 2. Pseudo-First Order and Pseudo-Second Order Parameter Adsorbents Qeexp PFO PSO (mg/g) Qecalc (mg/g) k1 (min−1) R2 Qecalc (mg/g) k2 (g/mg.min) R2 NiAl LDH 12.274 7.224 0.030 0.9719 12.804 0.010 0.9997 Chitosan 9.774 7.511 0.029 0.9452 10.311 0.008 0.9967 Chitosan@NiAl LDH 13.722 14.997 0.048 0.8676 14.556 0.007 0.9987 Table 3. Langmuir and Freundlich Parameter Adsorbent T (◦C) Langmuir Freundlich Qmax kL R2 n kF R2 NiAl LDH 30 25.445 0.438 0.845 1.395 1.456 0.9478 40 25.063 0.055 0.8827 1.466 1.801 0.9447 50 23.041 0.079 0.9392 1.653 2.469 0.9516 60 24.155 0.088 0.9451 1.685 2.820 0.9548 Chitosan 30 23.753 0.026 0.6276 1.270 6.703 0.9292 40 22.472 0.031 0.5671 1.295 2.078 0.8803 50 20.704 0.041 0.6888 1.362 4.248 0.8859 60 17.668 0.064 0.8866 1.581 7.579 0.9074 Chitosan@NiAl LDH 30 29.851 0.037 0.662 1.366 1.472 0.9343 40 32.468 0.040 0.8074 1.348 1.652 0.9645 50 33.223 0.044 0.8483 1.357 1.828 0.9687 60 26.596 0.076 0.9052 1.609 2.685 0.9654 Pseudo-rst order and pseudo-second order were used to determine the adsorption rate using the results of the data on the eect of phenol adsorption time in Figure 5. The kinetic model in the adsorption process can be determined by looking at the value of the coecient of determination (R2) which is close to 1, the smallest value of the kinetic rate (k), and the similarity between the experimental Qe value and the calcu- lated Qe. Based on Table 2, all adsorbent materials follow the pseudo-second-order kinetic model. This can be proven by the data of the coecient of determination (R2) which is close to 1, and the value of the kinetic rate (k2) in the pseudo- second-order kinetic model is smaller than the value of the pseudo-rst-order kinetic rate (k1), so it can be concluded that the reaction proceeds faster in the model pseudo-second order kinetics. Pseudo-second order implied adsorption of phenol was chemisorption (Gao et al., 2022). The Langmuir isotherm equation is used if the adsorp- tion process is in the form of a single layer or monolayer and there is an interaction between the adsorbate molecules. The Freundlich isotherm equation applies to adsorption processes that occur in several layers or multilayers so that there is no association and dissociation of the adsorbate molecules (Liu et al., 2021). The results of the NiAl LDH, chitosan, and chitosan@NiAl LDH adsorption isotherm data can be seen in Table 3. All adsorbents followed the Freundlich equation adsorption isotherm model, seeing the correlation coecient (R2) value closer to the value of 1. The maximum adsorption capacity of NiAl LDH, chitosan, and chitosan@NiAl LDH is 25.445, 23.753, and 33.223 mg/g, respectively. Comparison maximum capacities this work with other research in adsorp- tion shown in Table 4. Table 4. Comparison Maximum Capacities Adsorption of Phe- nol with Other Research Adsorbent Qmax (mg/g) Reference Bentonite 23.64 (Ahmadi and Igwegbe, 2018) 𝛼-Fe2O3 21.93 (Dehmani et al., 2020) Claried sludge 1.052 (Mandal and Das, 2019) SWNTO 30.864 (De la Luz-Asunción et al., 2015) GEO 28.986 (De la Luz-Asunción et al., 2015) Lignite 6.216 (Liu et al., 2021) Natural Clay 10.1 (Dehmani et al., 2021a) ZnCl2-BFAC 17.02 (Sathya Priya and Sureshkumar, 2020) Tea waste 7.62 (Gupta and Balomajumder, 2015) Zn4Al-LDH 7.73 (Lupa et al., 2018) NiAl LDH 25.445 This work Chitosan 23.753 This work Chitosan@NiAl LDH 33.223 This work © 2022 The Authors. Page 533 of 535 Utami et. al. Science and Technology Indonesia, 7 (2022) 530-535 Figure 5. Pseudo-First Order and Pseudo-Second Order for Adsorption of Phenol Figure 6. Regeneration Study of Adsorbent Based on Figure 6, it can be seen that the adsorbent re- generation process decreased during the third regeneration. The percentage of phenol adsorbed using NiAl LDH, chitosan, and chitosan@NiAl LDH during the rst regeneration reached 47.821, 38.844, 48.859%, respectively. The increase in regen- eration cycles causes a decrease in the percentage of adsorbed; sequentially, the percentage adsorbed during the fth regener- ation reaches 3.545, 1.966, 4.309%, respectively. 4. CONCLUSION Modication of the NiAl LDH composite with chitosan was successful by characterization XRD, FTIR and BET. The op- timum pH of the NiAl LDH at pH 3, the optimum pH for chitosan and chitosan@NiAl LDH material is pH 5. The ki- netic and isotherm model in the adsorption process is pseudo- second-order and Freundlich model, respectively. The max- imum adsorption capacity of NiAl LDH, chitosan, and chi- tosan@NiAlLDHis25.445,23.753,and33.223mg/g, respec- tively. 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Liu, H. Gong, Q. Chen, and H. Liu (2022). Hydroxyl-Functionalized Hypercrosslinked Polymers with Ultrafast Adsorption Rate as an Ecient Adsorbent for Phe- nol Removal. Microporous and Mesoporous Materials, 336; 111836 © 2022 The Authors. Page 535 of 535 INTRODUCTION EXPERIMENTAL SECTION Chemicals and Instrumentation Synthesis of NiAl-LDH Preparation Chitosan@NiAl LDH Adsorption of Phenol RESULT AND DISCUSSSION CONCLUSION ACKNOWLEDGMENT