Science and Technology Indonesia

e-ISSN:2580-4391 p-ISSN:2580-4405
Vol. 8, No. 2, April 2023

Research Paper

Facile Fabrication of Layered Double Hydroxide-Lignin for Efficient Adsorption of

Malachite Green
Neza Rahayu Palapa1* , Nur Ahmad2,3 , Alfan Wijaya3 , Zaqiya Artha Zahara3
1 Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Sriwijaya, Ogan Ilir 30662, Indonesia
2 Graduate School, Faculty of Mathematics and Natural Sciences, Sriwijaya University, Ogan Ilir, 30662, Indonesia
3 Research Center of Inorganic Materials and Complexes, Faculty of Mathematics and Natural Sciences, Sriwijaya University, Palembang, 30139, Indonesia

*Corresponding author: [email protected]

Abstract
Preparation of layered double hydroxide-lignin (lignin-Zn/Al) carried out by coprecipitation method. The FTIR spectra of lignin-Zn/Al
displayed at 3448, 2939, 1620, 1381, 1118, 1041, and 601 cm −1 . The characteristic peaks are located at 10.1°, 19.1°, 20.1°, 29.4°, 33.9°,
and 60.4°. The lignin-Zn/Al nitrogen adsorption-desorption isotherm showed a Type-IV curve, indicating that it had a mesoporous
structure. The H3 kind of hysteresis loop also provides evidence for the presence of mesopores within the lignin-Zn/Al complex.
Lignin-Zn/Al, lignin, and Zn/Al had pHpzc values of 6.09, 3.01, and 6.09, respectively. Lignin-Zn/Al, lignin, and Zn/Al are positively
charged when the pH of the solution is less than pHpzc, and they are negatively charged when the pH of the solution is more than
pHpzc. The Langmuir and pseudo-second-order model best represented the MG adsorption onto all adsorbents. The lignin-Zn/Al,
lignin, and Zn/Al were shown to have maximum Langmuir adsorption capacities of 83.034, 78.740, and 36.364 mg/g, respectively.
Zn/Al adsorption capacity increased 2.28 times after being composited with lignin.
Keywords
Layered Double Hydroxide, Adsorption, Lignin, Malachite Green

Received: 20 January 2023, Accepted: 8 April 2023

https://doi.org/10.26554/sti.2023.8.2.305-311

1. INTRODUCTION garnered the most attention among these due to its straightfor-
The contamination brought on by the wastewater discharge of ward functioning, design flexibility, practical recyclability, and
organic dyes has become a more prominent issue because of excellent reliability. For the purpose of removing MG from an
the industry’s rapid development (Tang et al., 2022) . In many aqueous solution, numerous sophisticated adsorption materi-
als have been developed recently, including Costus woodsonii
industries, including papers, tannery, printing inks, clothing,
(Van Tran et al., 2022) , modified metal-organic frameworks
and others, dyes are widely utilized. As a result, a lot of colorful
wastewater is produced, and many organic dyes will have a (Dahlan et al., 2023) , biowaste garlic peel (Pathania et al., 2022) ,
major harmful impact on the environment and human health and layered double hydroxide (Ahmad et al., 2023a) . Layered
(Giri et al., 2022; Vigneshwaran et al., 2021). Malachite green double hydroxides (LDHs) are a type of 2D anionic clay that
(MG), a triphenylmethane cationic dye, is frequently used in is composed of layers (Nazir et al., 2022) . LDH has a struc-
ture similar to brucite with a large surface area, where M(II)
the textile industry (Jin et al., 2022) . However, even at low
is surrounded by six hydroxide ions, for instance, and forms
concentrations, MG has been discovered to have numerous
toxicological side effects on human bodies, such as mutagenic, an octahedral array that is connected to form an infinite 2D
teratogenic, and cancerous consequences (Buvaneswari and structure (Ahmed and Mohamed, 2022) .
Singanan, 2022; Sarkar et al., 2021). These adsorbents have excellent MG molecule adsorption
Several cutting-edge methods, such as extraction (Raval performance, but for this purpose, sustainable, cost-effective
adsorbents made from biomass are still required (Wang et al.,
et al., 2022) , photodegradation (Puthukkara et al., 2022) , mem-
2018) . Also, when compared to several previously described
branes (Iqbal et al., 2022) , oxidation combining ultrasonic and
electrochemical (Ren et al., 2021) , and adsorption (Moradi adsorbents, biomass-based adsorbents appear to be more envi-
and Panahandeh, 2022) , have been used to remove MG from ronmentally friendly, cost-effective, and sustainable (Juleanti
aqueous medium over the past few decades. Adsorption has et al., 2021) . Designing biomass-derived adsorbents to remove
MG from aqueous media is therefore appealing. Lignin, an
Palapa et. al. Science and Technology Indonesia, 8 (2023) 305-311

amorphous high-molecular aromatic polymer, is the second Where q is adsorption capacity at t time (mg/g); C0 and C
most prevalent biomass component on the planet after cellu- are initial concentration and concentration for t time of MG,
lose (Zong et al., 2023) . The pulp and paper industry currently respectively (mg/L); V is the volume of MG (L); m is the mass
produces about 50 million tons of lignin as a byproduct each of lignin-Zn/Al (g).
year. The vast majority of lignin that has been burned up to
this point has been done so to create energy, which has re- 3. RESULTS AND DISCUSSION
sulted in significant lignin resource waste (Du et al., 2023) . FT-IR spectra of Zn/Al, lignin, and lignin-Zn/Al were pre-
The use of inexpensive, readily available industrial waste lignin sented in Figure 1. The FTIR spectra of lignin-Zn/Al displayed
to produce effective functional materials for environmental re- at 3448, 2939, 1620, 1381, 1118, 1041, and 601 cm−1 . The
mediation is a great solution when taking into account greater stretching vibration of -OH from Zn/Al is responsible for ap-
lignin usage and water remediation (Wang et al., 2022) . A pearing of the broad bandwidth 3448 and 1620 cm−1 (Ahmad
three-dimensional network structure and the abundance of et al., 2023b) . The band at 2939 cm−1 is stretching vibration of
functional groups that include oxygen in lignin give it more aliphatic -CH from lignin and the distinctive peak at bandwidth
potential for functionalization (Hamad et al., 2022) . 1381 cm−1 is anion interlayer NO3 − from Zn/Al (Zubair et al.,
In this work, the coprecipitation technique was used to pre- 2022) . The peak at 1118 and 1041 cm−1 are ascribable to
pare the lignin-Zn/Al. Many cutting-edge characterization C-O and C-O-C from lignin, respectively (Sun et al., 2022) .
techniques were used to examine the physicochemical charac- The metal oxide bond vibration is attributed to the band at 601
teristics of lignin-Zn/Al. Also, the potential of lignin-Zn/Al cm−1 (Chen et al., 2022) .
was examined, as well as its application to simulated textile
wastewater.

2. EXPERIMENTAL SECTION
2.1 Materials
All chemicals were used without any further purification. Sodium
chloride, sodium hydroxide, aluminum nitrate nonahydrate,
chloride acid, and zinc nitrate hexahydrate were purchased
from Sigma Aldrich and Merck. Lignin and distilled water
were purchased from Tokyo Chemical Industry and Brataco,
respectively.

2.2 Preparation Lignin-Zn/Al and Characterization

Lignin-Zn/Al was prepared by the coprecipitation method.
Both 0.25 M aluminum nitrate nonahydrate and 0.75 M zink
nitrate hexahydrate were dissolved in 30 mL of distilled water,
respectively. The solutions were added sodium hydroxide 2 M
to pH 8 and stirred at 70°C for 4 h. Afterward, the Zn/Al added
3 g lignin was under continuous stirring for 3 days, filtered,
and dried. The characterization of lignin-ZnAl using Fourier
Transfer Infra-Red (FTIR) (Shimadzu), X-Ray Diffractometer Figure 1. Fourier Transfer Infra-Red Results of Adsorbents
(XRD) (Rigaku), and Surface Area Analyzer (Quantachrome).

2.3 Adsorption Process of MG The usual Zn/Al XRD pattern can be seen in Figure 2,
Batch adsorption tests were conducted in a shaker. Investiga- where the characteristic peaks are located at 10.1° and 20.1°,
tions were into the effects of temperature (30–60°C), initial dye respectively, and correspond to the basal spacings of d003 and
concentration (60–100 mg/L), contact time (10–180 min), and d006, respectively (Yuliasari et al., 2023) . The 101 and 110
pHpzc (2–11). Usually, 100 mL of beaker glass was filled with planes are responsible for two further linked peaks at 29.4°
30 mL of MG solution and 30 mg of lignin-Zn/Al. Liquid and 60.4°, respectively. The XRD of the lignin is depicted in
aliquots were obtained after adsorption and centrifuged. Then, Figure 2 and displays the distinctive peak of carbon material
the supernatant was examined using a UV-Vis spectrophotome- at 19.1° and 33.9° (Sturgeon et al., 2014) . The XRD results
ter set to the maximum wavelength of 617 nm. Equation 1 of the lignin-Zn/Al mixture reveal the presence of distinctive
was used to determine the concentration of MG. Zn/Al and lignin reflections.
When evaluating the lignin-Zn/Al structure, the specific
surface area and pore size are important factors. Table 3 quan-
(C0 -C) ×V titatively displays the lignin-Zn/Al, lignin, and Zn/Al pore’s
q= (1)
m structure (d), surface area (SBET ), and pore volume (VP). The

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Palapa et. al. Science and Technology Indonesia, 8 (2023) 305-311

Table 1. The Surface Area of Adsorbents

Adsorbent SBET (m2 /g) d (nm) VP (cm3 /g)

Lignin-Zn/Al 7.125 1.960 0.007
Lignin 4.079 2.255 0.009
Zn/Al 1.968 27.687 0.006

Table 2. Kinetic Data of Adsorbents

Pseudo-First-Order Pseudo-Second-Order
Adsorbent Qeexp Qecalc k1 R2 Qecalc k2 R2
(mg/g) (mg/g) (min )−1 (mg/g) (g/mg.min)
Lignin-Zn/Al 45.642 17.527 0.024 0.850 47.170 0.002 0.999
Lignin 39.892 29.336 0.036 0.941 44.053 0.002 0.993
Zn/Al 36.148 39.455 0.037 0.995 39.683 0.002 0.996

Figure 2. X-Ray Diffractometer Results of Adsorbents Figure 3. Nitrogen Adsorption-Desorption Results of

Adsorbents

results show that lignin-Zn/Al has an average surface area of

7.125 m2 /g and pore sizes of 1.9620 ≈ 2 nm. The surface area When the pH of the solution is low, shaking causes H+ to
of Zn/Al increase after combining with lignin. Our findings migrate from the solution to the surface of the lignin-Zn/Al,
demonstrate the presence of mesopores in the lignin-Zn/Al lignin, and Zn/Al, raising the pH. When the solution has a high
structure, which have IUPAC-recommended diameter ranges pH, H+ diffuses into the solution from the surface of lignin-
of 2–50 nm (Heo et al., 2022) . The N2 adsorption/desorption Zn/Al, lignin, and Zn/Al. This reduces the pH of the solution.
curves and BJH (Barrett, Joyner, Halenda) pore size distri- H+ ions do not migrate at the point where the initial and final
butions of lignin-Zn/Al are shown in Figure 2. The lignin- pHs meet, indicating that pHpzc is the point of convergence.
Zn/Al nitrogen adsorption-desorption isotherm, as reported Lignin-Zn/Al, lignin, and Zn/Al had pHpzc values of 6.09,
by IUPAC, showed a Type-IV curve, indicating that it had a 3.01, and 6.09, respectively, as illustrated in Figure 4. Lignin-
mesoporous structure. The H3 kind of hysteresis loop also Zn/Al, lignin, and Zn/Al are positively charged when the pH of
provides evidence for the presence of mesopores within the the solution is less than pHpzc, and they are negatively charged
lignin-Zn/Al complex. when the pH of the solution is more than pHpzc .
The pHpzc of is the point when there is no charge at all. Table 2 lists the resulting parameters after the experimental

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Palapa et. al. Science and Technology Indonesia, 8 (2023) 305-311

Table 3. Isotherm Data of MG Adsorption

Freundlich Langmuir
Adsorbent T (°C) n kF R2 Qmax kL R2
Lignin-Zn/Al 30 5.230 1.431 0.828 78.125 0.233 0.994
40 5.959 1.452 0.781 79.365 0.341 0.995
50 7.930 1.490 0.645 83.333 0.723 0.996
60 1.101 1.506 0.668 84.034 1.469 0.999
Lignin 30 1.978 1.228 0.878 67.568 0.076 0.955
40 2.033 1.244 0.882 71.942 0.075 0.917
50 2.439 1.291 0.928 72.464 0.093 0.985
60 2.475 1.309 0.947 78.740 0.102 0.981
Zn/Al 30 0.876 2.037 0.880 23.310 0.121 0.982
40 1.071 1.903 0.763 26.954 0.155 0.954
50 1.388 1.789 0.732 30.675 0.203 0.956
60 1.916 1.684 0.778 36.364 0.342 0.980

Table 4. Several Adsorbents to the Adsorption of MG

Adsorbent Qmax (mg/g) References

Lignin-Zn/Al 84.034 This study
Lignin 78.740 This study
Zn/Al 36.364 This study
Avena sativa 83 Banerjee et al. (2016)
Pine cone 111.1 Kavci (2021)
Graphene oxide aminated lignin aerogels 113.5 Chen et al. (2020)
Halloysite nanotube 74.95 Altun and Ecevit (2022)
Active carbons 58 Hijab et al. (2021)
Chitosan-zink oxide 11 Muinde et al. (2020)
PACT@𝛾-Fe2 O3 62.89 Hasan et al. (2020)

Figure 4. pHpzc of Lignin-Zn/Al, Lignin, and Zn/Al Figure 5. Contact Time Between Adsorbents and Adsorbate

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Palapa et. al. Science and Technology Indonesia, 8 (2023) 305-311

data are fitted to the kinetics models. The pseudo-second-order Environmental Remediation of Heavy Metals and Dye Pol-
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