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A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane
Alexandria Engineering Journal (2019) xxx, xxx–xxx
H O S T E D BY
Alexandria University
Alexandria Engineering Journal www.elsevier.com/locate/aej www.sciencedirect.com
ORIGINAL ARTICLE
A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane Noor Hafizah Mohd Amin a, Faizatul Shimal Mehamod b, Faiz Bukhari Mohd Suah a,c,* a
School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Pulau Pinang, Malaysia School of Fundamental Science, Universiti Malaysia Terengganu, 21030 Kuala Terengganu, Malaysia c Department of Chemistry, Imperial College London, Exhibition Road, London SW7 2AZ, United Kingdom b
Received 7 May 2019; revised 18 July 2019; accepted 19 August 2019
KEYWORDS Batch reactor; Malachite green; Methylene blue; Polymer inclusion membrane; Simultaneous extraction
Abstract A novel approach in simultaneous extraction of two basic dyes, malachite green (MG) and methylene blue (MB) from an aqueous solution was performed by using a batch reactor consisting a polymer inclusion membrane (PIM). The PIM is made up of poly(vinyl) chloride (PVC) as the base polymer, bis-(2-ethylhexyl) phosphate (B2EHP) as an extractant and dioctyl phthalate (DOP) as the plasticizer. The optimized extraction conditions for both dyes were identified by varying the composition of the PIM. It was found that the optimum PIM composition for simultaneous extraction was PIM with a composition of PVC 35% wt% (m/m): B2EHP 60% wt% (m/m): DOP 5% wt% (m/m). It shows that the average percent extraction efficiency achieved is more than 97% for the mixture of MG and MB (100 mg L1) within 4 h of extraction process. The batch reactor consisting PIM prepared in this study is highly capable in performing simultaneous extraction of MG and MB in an aqueous solution. Ó 2019 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
1. Introduction Malachite green (MG) and methylene blue (MB) are among the basic dyes commonly used in textile industry, even knowing that they affect our ecosystem [1,2]. It was reported that * Corresponding author at: School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Pulau Pinang, Malaysia. E-mail addresses: [email protected], [email protected] (F.B. Mohd Suah). Peer review under responsibility of Faculty of Engineering, Alexandria University.
MG dye could harm living things from various fish to mammals due to its detrimental characteristics as teratogenic, carcinogenic and reproductive abnormalities [3]. Moreover, it also has been reported that these dyes can cause chronic health problems at very high concentrations, such as cyanosis, jaundice and tissue necrosis when humans are exposed [4]. Hence, the treatment of these dyes from wastewater is an important issue to examine as the effluents produce a negative impact on living things. Over the years, many physico-chemical methods have been developed, such as adsorption, photocatalytic process, coagula-
https://doi.org/10.1016/j.aej.2019.08.007 1110-0168 Ó 2019 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/). Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
2 tion, oxidative process, electrochemical process and membrane separation for the treatment of these dyes [5–12]. Among these methods, membrane separation is considered as a green method because there is no requirement of a large amount of volatile organic compounds as well as energy saving because it operates without using a thermal heating process. Furthermore, the operation is hassle-free because the operation is a continuous process, which does not require a regeneration process [12]. Membrane technology is an effective system for the removal and recovery of dye materials [12]. There are several types of membranes generally use in the membrane-based separation process. Among these membranes, polymer inclusion membrane (PIM) has a better mechanical properties, good chemical resistance and low cost of preparation. In addition, PIM has excellent capabilities in enhancing the selectivity of an extraction process, fast permeation rate, possesses a high interfacial surface area, high transport flux, high flexibility in membrane composition, prominent separation efficiency and is highly versatile in terms of applications [13,14]. In a recent study, PIM was successfully applied to remove MG from wastewater sample with an average extraction efficiency achieved of more than 98% [15]. In addition, a study also showed that PIM has the capability to remove MB from the aqueous solution, achieving 93% extraction efficiency [16]. In many developing countries, not much improvement has been made in the terms of developing new methods for recovering and removing dyes, classical processes such as adsorption and coagulation are still utilized [5]. The only improvement is in use of new materials but not a new method. Thus, this paper aims to establish a new method for simultaneous removal of basic dyes by using a batch reactor consist of PIM. The unique idea of this research is authors try to extract two basic dyes by using a single PIM. To our knowledge, this is the first report showing the use of a batch reactor consist of PIM in removal of MG and MB simultaneously from an aqueous solution. Previously, authors have proved that PIM was excellent in extracting a single dye in an aqueous solution [15]. Thus, authors would like to explore the feasibility of PIM as an extractant in extracting two dyes simultaneously. Our results demonstrated that PIM was able to recover most of MG and MB (>97%) from an aqueous solution. In addition, PIM shows excellent physical and chemical properties that have a massive potential to be applied on a large scale for wastewater treatment. 2. Experimental 2.1. Chemicals and instrument Poly(vinyl chloride) (PVC) (high molecular weight), bis-(2ethylhexyl)phosphate (B2EHP), dioctyl phthalate (DOP) and nitric acid (HNO3) (65%) were obtained from Sigma (St. Loius, MO, USA). Tetrahydrofuran (THF), MG and MB were obtained from QRe¨C Chemicals (Auckland, New Zealand). The instrument used for the analysis was an ultraviolet–visible (UV–Vis) spectrophotometer (Perkin Elmer Lambda 35) (Waltham, MA, USA). 2.2. Membrane preparation PIMs were prepared similarly to the procedure used in the previous study [15]. The PVC solution is prepared by dissolving
N.H. Mohd Amin et al. the PVC powder in 10 mL THF while for the B2EHP and DOP solution are prepared separately by dissolving them in 5 mL of THF. The mixture of these three solutions were stirred for 4 h until homogenous casting solution is formed. The solution was poured into a 9.0 cm diameter flat bottom glass petri dish which was set horizontally and covered by using a filter paper to slow the evaporation of the solvent and drying evenly. The PIM solution was allowed to evaporate over 24 h and it was peeled off from petri dish by moistening the membrane with distilled water. Lastly, PIM was washed using distilled water for several times before using it for the extraction process. All of the PIMs were prepared at room temperature. 2.3. Membrane preparation The determination of the concentration of the dye solution are determined by using UV/Vis spectrophotometer at wavelength of 617 nm for MG and 662 nm for MB, respectively. The morphology and characterization of the membrane were investigated by using Fourier Infrared Spectroscopy (FTIR) (Perkin-Elmer model L1280034, Boston, MA, USA) in the range of 4000–600 cm1 to observe the functional group. Scanning Electron Microscopy (SEM) (Zeiss model Leo Supra 50 VP, Oberkochen, Germany) was used to study the surface morphology and Thermal gravimetric analysis (TGA) (Mettler Toledo, Columbus, Oh, USA) were carried out in the range in between 0 °C and 900 °C at heating rate of 30 °C min1 to determine the thermal stability of the composition of the membrane. 2.4. Extraction process The extraction of the dyes was conducted by using a batch reactor consisting of two electrolyte compartments. The compartments of the reactor are separated by the PIM. The dimensions of the reactor are 4.7 cm 5.3 cm 9.3 cm. The reactor compartments were then screwed together. The feeding solution used was MG, MB and the mixture of both dyes (all volume are set to 100 mL) while the receiving solution used was HNO3 (100 mL and 1.0 M). A magnetic stirrer is put in the feeding phase to stir the dye solution for homogeneous extraction. Initially, the optimization of the PIM for each dye was determined based on the highest percentage extraction efficiency. A sample of 2.50 mL of the feeding solution was pipetted into a 25 mL volumetric flask every 30 min for 4 h to observe the removal of the dye by each of the PIMs prepared. The concentration of each dye was determined by using the UV–Vis spectrophotometer at a wavelength of 617 nm for MG and 662 nm for MB [15,16]. This procedure was then continued for the mixed dyes solutions of MG and MB (20– 80 mg L1) by using the optimized PIM. The volume ratio of the mixed dyes solutions was fixed at 1:1. 2.5. Determination of per cent dyes removal The concentration of the removed dyes from the aqueous solution was determined based on the absorbance of the light quantified by using the UV–Vis spectrophotometer. The per cent extraction of the dye, E% is calculated using the following equation:
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
Simultaneous extraction of basic dyes by using PIM E% ¼ ð½dyei ½dyef Þ=½dyei 100;
3 ð1Þ
where [dye]i is the initial dye concentration in the aqueous solution (mg L1) and [dye]f is the final dye concentration after the extraction process in the aqueous solution (mg L1).
Table 1 The values of the wavenumbers (cm1) and the types of molecular vibrations in each materials and membrane. Materials
Wavenumbers (cm1)
Type of molecular vibrations
PVC
2912.20 1427.10 691.57 2959.11–2930.08 2861.03 1223.32 1011.23 2958.27–2929.07 2860.10 1723.82 1600.01–1461.29 1380.24 1267.26 900.0–675.0 2959.84–2930.22 2861.09 1724.95 1462.85 1380.55 1230.96 1021.30 692.72
CAH stretching CAH bending CACl stretching Csp3AH Csp2AH P‚O PAO Csp3AH Csp2AH C‚O CAC in ring CAO stretching OAC CAH Csp3AH Csp2AH C‚O CAC stretching in ring CAO P‚O PAO CACl
3. Results and discussion B2EHP
3.1. Characterization of membrane composition 3.1.1. Identification of spectral membrane
DOP
In this study, the FTIR is used to study the vibrations of molecular bonds that present in the membrane (PIM V). Fig. 1 represents the FTIR absorption spectra of PIM V with composition of PVC 35 wt% (m/m): B2EHP 60 wt% (m/m): DOP 5 wt% (m/m) in 650–4000 cm1 region. As stated in Table 1, the wavenumbers of the membrane surfaces matched with the raw materials of the membrane compositions. The obtained results showed that the two weak peaks at 2959.84–2930.08 cm1 attributed to CAH stretching in the PVC and Csp3AH in B2EHP and DOP. Whereas, the two weak bands at 2861.09 cm1 correspond to Csp2AH in B2EHP and DOP. Weak band at 1724.95 cm1 arises from the C‚O group of DOP while the sharp and weak band at 1462.85 cm1 indicating the CAC stretching in the ring of DOP structure. The very weak band at 1380.55 cm1 results from stretching of CAO group of DOP. The medium peak at 1230.96 cm1 assigned to P‚O group of B2EHP, whereas, the strong and intense peak at 1021.30 cm1 attributed to PAO group of B2EHP. Lastly, the weak band at 692.72 cm1 occurs due to CACl stretching of PVC. Thus, it shows that the intermolecular interactions correlated between the base polymer and extractant in the membrane. This implies that only weak interaction of Van der Waals forces is present between the compositions of PIM.
Fig. 1
Membrane
3.1.2. Morphological properties of PIM membrane SEM is a technique to provide information on extractant and plasticizer distributions within the base polymer. Fig. 2 showed the morphology of the polymeric composition of the membrane. It was observed that a smooth, less porous and high dense membrane was formed. This suggested that the membrane become more homogenous and the changes of the microstructure of PIM shall increase the rate of movement of ions across the membrane [17,18].
FTIR spectrum of PIM V (PVC: B2EHP: DOP).
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
4
N.H. Mohd Amin et al.
Fig. 2
SEM image of PIM V (PVC: B2EHP: DOP) surface morphology.
3.1.3. TGA analysis As shown in Fig. 3, thermogram of PIM indicates the occurrence of three major steps of weight loss. First weight loss occurred at around 170 °C which was due to weight loss of DOP with a weight loss of 39% of the original weight. Then, at a temperature of around 285 °C, weight loss of B2EHP occurred. Lastly, at a temperature of 388 °C, the decomposition of polymer chains happened (a loss of 17% of the original weight). 3.2. Optimization of the PIM Each MG and MB with a concentration of 100 mg L1 was extracted using a PIM with a different composition. Different
Fig. 3
compositions of PIM were studied to optimize the extraction capability as given in Table 2. In general, the purpose of optimizing the condition is to increase the absorption and uniformity of membrane surfaces towards the cationic dye from the aqueous solution. It is known that a transparent, selfsupporting and homogeneous membrane is crucial for yielding high extraction capability [15]. Here, B2EHP acts as a complexing agent that combines with the cationic dye and assists the transport of the dye across the membrane from the feeding phase to the receiving phase. DOP’s function is to promote a better extraction capability by improving the flexibility of the membrane and the solubility of the extractant species in the liquid phase. The positive charge existing on the cationic dyes, MG and MB atoms attracted to the negatively charged B2EHP of PIM to form dye-B2EHP neutral ion complex.
Thermogram of PIM V (PVC: B2EHP: DOP).
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
Simultaneous extraction of basic dyes by using PIM Table 2
5
The composition of PIM with the total mass of 500 mg.
Membrane
PVC (mg)
B2EHP (mg)
DOP (mg)
Composition (wt%)
I II III IV V
250 250 275 200 175
200 225 200 250 300
50 25 25 50 25
50:40:10 50:45:05 55:40:05 40:50:10 35:60:05
þ Dyeþ aq: þ ½RH2 org $ ½DyeðRHRÞorg þ Haq:
ð2Þ
where, RH2 is an extractant and [Dye (RHR)]org is a neutral ion pair complex. To choose the PIM for simultaneous extraction of MG and MB dyes from aqueous solution, an initial individual extraction experiment was carried out. The results in Table 3 show that the highest extraction of MG and MB dye by an individual extraction process was obtained by using PIM II and V with values for E% of 99.13% and 99.22%, respectively. The suitable ratio of B2EHP and DOP in the polymeric membrane has been found to allow the best extraction efficiency of each dye. Interestingly, these PIMs also produced a satisfactory calculated value at 95% confidence limit which are 98.11 ± 0.9% for MG and 96.35 ± 4.1% for MB. So, it shows there is no significantly error observed from these PIMs at 95% confidence level. Thus, those PIM compositions were considered for further study. The effect of initial concentration on the extraction efficiency of each individual dye at optimum condition was studied in the range of 20–100 mg L1 as illustrated in Figs. S1 and S2. The results revealed that the E% increase with increasing time for various initial dye concentration. However, after at certain stage of analysis, E% for each different initial concentration become constant. This phenomena is probably attributed to the membrane saturation and lower efficiency membrane area after prolonged exposure to the dyes solutions. The obtained results were comparable with the previously reported experiments [19–21].
the concentration of the dye extracted by the PIM. In this study, PIM is able to extract MG and MB dyes from the aqueous solution by complexing the positive ions of the dyes with negatively charged B2EHP. This indicated that there is an electrostatic attraction between the cationic dye and B2EHP during the extraction process. The comparison made in Figs. 4–8 shows that PIM V achieved a slightly better extraction efficiency than PIM II. The maximum E% was observed at 100 mg L1 of initial dyes where the extraction of the dyes mixture approaching 100%. This can be explained by the presence of an optimum amount of B2EHP in the PIM V compared with PIM II, providing microchannels in the membrane structure for speeding up the movement of ions. However, it cannot achieve exactly 100% 120 Av. percentage extraction (E%)
Then, the cationic dye is extracted across the hydrophobic PIM with high extraction efficiency. The reaction is as stated in Eq. (2) below:
100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 4 Simultaneous extraction of MG and MB dyes with initial concentration of 100 mg L1 for PIM II and PIM V.
3.3. Simultaneous extraction of MG and MB dyes
Table 3 The comparison of percent extraction of an individual dye (MG and MB) for each different PIM composition. PIM
I II III IV V
Percent extraction of dye (E%) MG
MB
97.95 99.13 98.46 97.99 97.03
93.11 97.98 92.32 99.11 99.22
120 Av. percentage extraction (E%)
The simultaneous extraction of the dyes was conducted based on the optimized PIM for each individual extraction. The per cent extraction efficiency of each dye was calculated based on
100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 5 Simultaneous extraction of MG and MB dyes with initial concentration of 80 mg L1 for PIM II and PIM V.
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
6
N.H. Mohd Amin et al.
Av. percentage extraction (E%)
120 100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 6 Simultaneous extraction of MG and MB dyes with initial concentration of 60 mg L1 for PIM II and PIM V.
The fast uptake of basic dyes at the beginning of extraction process as shown in Figs. 4–8 may be attributed to the rapid complexation of dye molecules with the extractant. The different uptake of dye also may be affected by their molecular weight of dye [22–26]. The dye with lower molecular weight (MB) will diffuse faster into the membrane and forming the complex of dye-B2EHP and followed by dye with higher molecular weight (MG). The average percentage extraction of PIM V is higher than PIM II at an optimum pH 5.0 due to the complexation of positively charged dyes with negatively charged B2EHP. From the result showed in Figs. 4–8, the time taken for the simultaneous extraction process for PIM V is faster than PIM II, which is achieving more than 92% starting from 90 min for concentrations of 20–40 mg L1 and 120 min for 60–100 mg L–1, even though there was competition between extraction of MG and MB dyes. In addition, the extraction process for PIM V is faster than for PIM II due to the optimum concentration of B2EHP to extract the dyes rapidly.
Av. percentage extraction (E%)
120
4. Conclusion 100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 7 Simultaneous extraction of MG and MB dyes with initial concentration of 40 mg L1 for PIM II and PIM V.
A batch reactor consisting a PIM was successfully developed to extract MG and MB dyes simultaneously from an aqueous solution. The extraction of the dyes is influenced by three main parameters, the membrane composition, the initial dyes’ concentrations and the pH of the feeding solution. The PIM prepared is highly capable of performing simultaneous extraction of two dyes in an aqueous solution due to its extraction capability and membrane properties (mechanically and chemically stable). In order to explore the potential application of this dyes recovery system, additional studies are currently been carried such as optimizing the PIM in terms of stability and size, increasing the concentration of dyes and testing the system with real wastewater samples. Declaration of Competing Interest
Av. percentage extraction (E%)
120
None.
100
Acknowledgement
80 60
PIM II
Authors would like to acknowledge Universiti Sains Malaysia for providing financial assistance through Bridging grant scheme (304.PKIMIA.6316215).
PIM V
40
Appendix A. Supplementary material
20 0 0
50
100
150 200 Time (min)
250
300
Fig. 8 Simultaneous extraction of MG and MB dyes with initial concentration of 20 mg L1 for PIM II and PIM V.
due to the saturation of the membrane area, which does not allow any further extraction. Nevertheless, this limitation can be overcome by utilizing a PIM with a higher surface area or using a different cell arrangement (e.g. flow-through cell) for the extraction process.
Supplementary data to this article can be found online at https://doi.org/10.1016/j.aej.2019.08.007. References [1] J. Oliva, A.I. Martinez, A.I. Oliva, C.R. Garcia, A. MartinezLuevanos, M. Garcia-Lobato, R. Ochoa-Valiente, Flexible graphene composites for removal of methylene blue dye– contaminant from water, Appl. Surf. Sci. 436 (2018) 739–746. [2] G.A. Borges, L.P. Silva, J.A. Penido, L.R.D. Lemos, A.B. Mageste, A method for dye extraction using an aqueous two– phase system: Effect of co-occurrence of contaminants in textile industry wastewater, J. Environ. Manage. 183 (2016) 196–203.
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ORIGINAL ARTICLE
A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane Noor Hafizah Mohd Amin a, Faizatul Shimal Mehamod b, Faiz Bukhari Mohd Suah a,c,* a
School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Pulau Pinang, Malaysia School of Fundamental Science, Universiti Malaysia Terengganu, 21030 Kuala Terengganu, Malaysia c Department of Chemistry, Imperial College London, Exhibition Road, London SW7 2AZ, United Kingdom b
Received 7 May 2019; revised 18 July 2019; accepted 19 August 2019
KEYWORDS Batch reactor; Malachite green; Methylene blue; Polymer inclusion membrane; Simultaneous extraction
Abstract A novel approach in simultaneous extraction of two basic dyes, malachite green (MG) and methylene blue (MB) from an aqueous solution was performed by using a batch reactor consisting a polymer inclusion membrane (PIM). The PIM is made up of poly(vinyl) chloride (PVC) as the base polymer, bis-(2-ethylhexyl) phosphate (B2EHP) as an extractant and dioctyl phthalate (DOP) as the plasticizer. The optimized extraction conditions for both dyes were identified by varying the composition of the PIM. It was found that the optimum PIM composition for simultaneous extraction was PIM with a composition of PVC 35% wt% (m/m): B2EHP 60% wt% (m/m): DOP 5% wt% (m/m). It shows that the average percent extraction efficiency achieved is more than 97% for the mixture of MG and MB (100 mg L1) within 4 h of extraction process. The batch reactor consisting PIM prepared in this study is highly capable in performing simultaneous extraction of MG and MB in an aqueous solution. Ó 2019 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
1. Introduction Malachite green (MG) and methylene blue (MB) are among the basic dyes commonly used in textile industry, even knowing that they affect our ecosystem [1,2]. It was reported that * Corresponding author at: School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Pulau Pinang, Malaysia. E-mail addresses: [email protected], [email protected] (F.B. Mohd Suah). Peer review under responsibility of Faculty of Engineering, Alexandria University.
MG dye could harm living things from various fish to mammals due to its detrimental characteristics as teratogenic, carcinogenic and reproductive abnormalities [3]. Moreover, it also has been reported that these dyes can cause chronic health problems at very high concentrations, such as cyanosis, jaundice and tissue necrosis when humans are exposed [4]. Hence, the treatment of these dyes from wastewater is an important issue to examine as the effluents produce a negative impact on living things. Over the years, many physico-chemical methods have been developed, such as adsorption, photocatalytic process, coagula-
https://doi.org/10.1016/j.aej.2019.08.007 1110-0168 Ó 2019 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/). Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
2 tion, oxidative process, electrochemical process and membrane separation for the treatment of these dyes [5–12]. Among these methods, membrane separation is considered as a green method because there is no requirement of a large amount of volatile organic compounds as well as energy saving because it operates without using a thermal heating process. Furthermore, the operation is hassle-free because the operation is a continuous process, which does not require a regeneration process [12]. Membrane technology is an effective system for the removal and recovery of dye materials [12]. There are several types of membranes generally use in the membrane-based separation process. Among these membranes, polymer inclusion membrane (PIM) has a better mechanical properties, good chemical resistance and low cost of preparation. In addition, PIM has excellent capabilities in enhancing the selectivity of an extraction process, fast permeation rate, possesses a high interfacial surface area, high transport flux, high flexibility in membrane composition, prominent separation efficiency and is highly versatile in terms of applications [13,14]. In a recent study, PIM was successfully applied to remove MG from wastewater sample with an average extraction efficiency achieved of more than 98% [15]. In addition, a study also showed that PIM has the capability to remove MB from the aqueous solution, achieving 93% extraction efficiency [16]. In many developing countries, not much improvement has been made in the terms of developing new methods for recovering and removing dyes, classical processes such as adsorption and coagulation are still utilized [5]. The only improvement is in use of new materials but not a new method. Thus, this paper aims to establish a new method for simultaneous removal of basic dyes by using a batch reactor consist of PIM. The unique idea of this research is authors try to extract two basic dyes by using a single PIM. To our knowledge, this is the first report showing the use of a batch reactor consist of PIM in removal of MG and MB simultaneously from an aqueous solution. Previously, authors have proved that PIM was excellent in extracting a single dye in an aqueous solution [15]. Thus, authors would like to explore the feasibility of PIM as an extractant in extracting two dyes simultaneously. Our results demonstrated that PIM was able to recover most of MG and MB (>97%) from an aqueous solution. In addition, PIM shows excellent physical and chemical properties that have a massive potential to be applied on a large scale for wastewater treatment. 2. Experimental 2.1. Chemicals and instrument Poly(vinyl chloride) (PVC) (high molecular weight), bis-(2ethylhexyl)phosphate (B2EHP), dioctyl phthalate (DOP) and nitric acid (HNO3) (65%) were obtained from Sigma (St. Loius, MO, USA). Tetrahydrofuran (THF), MG and MB were obtained from QRe¨C Chemicals (Auckland, New Zealand). The instrument used for the analysis was an ultraviolet–visible (UV–Vis) spectrophotometer (Perkin Elmer Lambda 35) (Waltham, MA, USA). 2.2. Membrane preparation PIMs were prepared similarly to the procedure used in the previous study [15]. The PVC solution is prepared by dissolving
N.H. Mohd Amin et al. the PVC powder in 10 mL THF while for the B2EHP and DOP solution are prepared separately by dissolving them in 5 mL of THF. The mixture of these three solutions were stirred for 4 h until homogenous casting solution is formed. The solution was poured into a 9.0 cm diameter flat bottom glass petri dish which was set horizontally and covered by using a filter paper to slow the evaporation of the solvent and drying evenly. The PIM solution was allowed to evaporate over 24 h and it was peeled off from petri dish by moistening the membrane with distilled water. Lastly, PIM was washed using distilled water for several times before using it for the extraction process. All of the PIMs were prepared at room temperature. 2.3. Membrane preparation The determination of the concentration of the dye solution are determined by using UV/Vis spectrophotometer at wavelength of 617 nm for MG and 662 nm for MB, respectively. The morphology and characterization of the membrane were investigated by using Fourier Infrared Spectroscopy (FTIR) (Perkin-Elmer model L1280034, Boston, MA, USA) in the range of 4000–600 cm1 to observe the functional group. Scanning Electron Microscopy (SEM) (Zeiss model Leo Supra 50 VP, Oberkochen, Germany) was used to study the surface morphology and Thermal gravimetric analysis (TGA) (Mettler Toledo, Columbus, Oh, USA) were carried out in the range in between 0 °C and 900 °C at heating rate of 30 °C min1 to determine the thermal stability of the composition of the membrane. 2.4. Extraction process The extraction of the dyes was conducted by using a batch reactor consisting of two electrolyte compartments. The compartments of the reactor are separated by the PIM. The dimensions of the reactor are 4.7 cm 5.3 cm 9.3 cm. The reactor compartments were then screwed together. The feeding solution used was MG, MB and the mixture of both dyes (all volume are set to 100 mL) while the receiving solution used was HNO3 (100 mL and 1.0 M). A magnetic stirrer is put in the feeding phase to stir the dye solution for homogeneous extraction. Initially, the optimization of the PIM for each dye was determined based on the highest percentage extraction efficiency. A sample of 2.50 mL of the feeding solution was pipetted into a 25 mL volumetric flask every 30 min for 4 h to observe the removal of the dye by each of the PIMs prepared. The concentration of each dye was determined by using the UV–Vis spectrophotometer at a wavelength of 617 nm for MG and 662 nm for MB [15,16]. This procedure was then continued for the mixed dyes solutions of MG and MB (20– 80 mg L1) by using the optimized PIM. The volume ratio of the mixed dyes solutions was fixed at 1:1. 2.5. Determination of per cent dyes removal The concentration of the removed dyes from the aqueous solution was determined based on the absorbance of the light quantified by using the UV–Vis spectrophotometer. The per cent extraction of the dye, E% is calculated using the following equation:
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
Simultaneous extraction of basic dyes by using PIM E% ¼ ð½dyei ½dyef Þ=½dyei 100;
3 ð1Þ
where [dye]i is the initial dye concentration in the aqueous solution (mg L1) and [dye]f is the final dye concentration after the extraction process in the aqueous solution (mg L1).
Table 1 The values of the wavenumbers (cm1) and the types of molecular vibrations in each materials and membrane. Materials
Wavenumbers (cm1)
Type of molecular vibrations
PVC
2912.20 1427.10 691.57 2959.11–2930.08 2861.03 1223.32 1011.23 2958.27–2929.07 2860.10 1723.82 1600.01–1461.29 1380.24 1267.26 900.0–675.0 2959.84–2930.22 2861.09 1724.95 1462.85 1380.55 1230.96 1021.30 692.72
CAH stretching CAH bending CACl stretching Csp3AH Csp2AH P‚O PAO Csp3AH Csp2AH C‚O CAC in ring CAO stretching OAC CAH Csp3AH Csp2AH C‚O CAC stretching in ring CAO P‚O PAO CACl
3. Results and discussion B2EHP
3.1. Characterization of membrane composition 3.1.1. Identification of spectral membrane
DOP
In this study, the FTIR is used to study the vibrations of molecular bonds that present in the membrane (PIM V). Fig. 1 represents the FTIR absorption spectra of PIM V with composition of PVC 35 wt% (m/m): B2EHP 60 wt% (m/m): DOP 5 wt% (m/m) in 650–4000 cm1 region. As stated in Table 1, the wavenumbers of the membrane surfaces matched with the raw materials of the membrane compositions. The obtained results showed that the two weak peaks at 2959.84–2930.08 cm1 attributed to CAH stretching in the PVC and Csp3AH in B2EHP and DOP. Whereas, the two weak bands at 2861.09 cm1 correspond to Csp2AH in B2EHP and DOP. Weak band at 1724.95 cm1 arises from the C‚O group of DOP while the sharp and weak band at 1462.85 cm1 indicating the CAC stretching in the ring of DOP structure. The very weak band at 1380.55 cm1 results from stretching of CAO group of DOP. The medium peak at 1230.96 cm1 assigned to P‚O group of B2EHP, whereas, the strong and intense peak at 1021.30 cm1 attributed to PAO group of B2EHP. Lastly, the weak band at 692.72 cm1 occurs due to CACl stretching of PVC. Thus, it shows that the intermolecular interactions correlated between the base polymer and extractant in the membrane. This implies that only weak interaction of Van der Waals forces is present between the compositions of PIM.
Fig. 1
Membrane
3.1.2. Morphological properties of PIM membrane SEM is a technique to provide information on extractant and plasticizer distributions within the base polymer. Fig. 2 showed the morphology of the polymeric composition of the membrane. It was observed that a smooth, less porous and high dense membrane was formed. This suggested that the membrane become more homogenous and the changes of the microstructure of PIM shall increase the rate of movement of ions across the membrane [17,18].
FTIR spectrum of PIM V (PVC: B2EHP: DOP).
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
4
N.H. Mohd Amin et al.
Fig. 2
SEM image of PIM V (PVC: B2EHP: DOP) surface morphology.
3.1.3. TGA analysis As shown in Fig. 3, thermogram of PIM indicates the occurrence of three major steps of weight loss. First weight loss occurred at around 170 °C which was due to weight loss of DOP with a weight loss of 39% of the original weight. Then, at a temperature of around 285 °C, weight loss of B2EHP occurred. Lastly, at a temperature of 388 °C, the decomposition of polymer chains happened (a loss of 17% of the original weight). 3.2. Optimization of the PIM Each MG and MB with a concentration of 100 mg L1 was extracted using a PIM with a different composition. Different
Fig. 3
compositions of PIM were studied to optimize the extraction capability as given in Table 2. In general, the purpose of optimizing the condition is to increase the absorption and uniformity of membrane surfaces towards the cationic dye from the aqueous solution. It is known that a transparent, selfsupporting and homogeneous membrane is crucial for yielding high extraction capability [15]. Here, B2EHP acts as a complexing agent that combines with the cationic dye and assists the transport of the dye across the membrane from the feeding phase to the receiving phase. DOP’s function is to promote a better extraction capability by improving the flexibility of the membrane and the solubility of the extractant species in the liquid phase. The positive charge existing on the cationic dyes, MG and MB atoms attracted to the negatively charged B2EHP of PIM to form dye-B2EHP neutral ion complex.
Thermogram of PIM V (PVC: B2EHP: DOP).
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
Simultaneous extraction of basic dyes by using PIM Table 2
5
The composition of PIM with the total mass of 500 mg.
Membrane
PVC (mg)
B2EHP (mg)
DOP (mg)
Composition (wt%)
I II III IV V
250 250 275 200 175
200 225 200 250 300
50 25 25 50 25
50:40:10 50:45:05 55:40:05 40:50:10 35:60:05
þ Dyeþ aq: þ ½RH2 org $ ½DyeðRHRÞorg þ Haq:
ð2Þ
where, RH2 is an extractant and [Dye (RHR)]org is a neutral ion pair complex. To choose the PIM for simultaneous extraction of MG and MB dyes from aqueous solution, an initial individual extraction experiment was carried out. The results in Table 3 show that the highest extraction of MG and MB dye by an individual extraction process was obtained by using PIM II and V with values for E% of 99.13% and 99.22%, respectively. The suitable ratio of B2EHP and DOP in the polymeric membrane has been found to allow the best extraction efficiency of each dye. Interestingly, these PIMs also produced a satisfactory calculated value at 95% confidence limit which are 98.11 ± 0.9% for MG and 96.35 ± 4.1% for MB. So, it shows there is no significantly error observed from these PIMs at 95% confidence level. Thus, those PIM compositions were considered for further study. The effect of initial concentration on the extraction efficiency of each individual dye at optimum condition was studied in the range of 20–100 mg L1 as illustrated in Figs. S1 and S2. The results revealed that the E% increase with increasing time for various initial dye concentration. However, after at certain stage of analysis, E% for each different initial concentration become constant. This phenomena is probably attributed to the membrane saturation and lower efficiency membrane area after prolonged exposure to the dyes solutions. The obtained results were comparable with the previously reported experiments [19–21].
the concentration of the dye extracted by the PIM. In this study, PIM is able to extract MG and MB dyes from the aqueous solution by complexing the positive ions of the dyes with negatively charged B2EHP. This indicated that there is an electrostatic attraction between the cationic dye and B2EHP during the extraction process. The comparison made in Figs. 4–8 shows that PIM V achieved a slightly better extraction efficiency than PIM II. The maximum E% was observed at 100 mg L1 of initial dyes where the extraction of the dyes mixture approaching 100%. This can be explained by the presence of an optimum amount of B2EHP in the PIM V compared with PIM II, providing microchannels in the membrane structure for speeding up the movement of ions. However, it cannot achieve exactly 100% 120 Av. percentage extraction (E%)
Then, the cationic dye is extracted across the hydrophobic PIM with high extraction efficiency. The reaction is as stated in Eq. (2) below:
100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 4 Simultaneous extraction of MG and MB dyes with initial concentration of 100 mg L1 for PIM II and PIM V.
3.3. Simultaneous extraction of MG and MB dyes
Table 3 The comparison of percent extraction of an individual dye (MG and MB) for each different PIM composition. PIM
I II III IV V
Percent extraction of dye (E%) MG
MB
97.95 99.13 98.46 97.99 97.03
93.11 97.98 92.32 99.11 99.22
120 Av. percentage extraction (E%)
The simultaneous extraction of the dyes was conducted based on the optimized PIM for each individual extraction. The per cent extraction efficiency of each dye was calculated based on
100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 5 Simultaneous extraction of MG and MB dyes with initial concentration of 80 mg L1 for PIM II and PIM V.
Please cite this article in press as: N.H. Mohd Amin et al., A novel approach in simultaneous extraction of basic dyes by using a batch reactor consisting a polymer inclusion membrane, Alexandria Eng. J. (2019), https://doi.org/10.1016/j.aej.2019.08.007
6
N.H. Mohd Amin et al.
Av. percentage extraction (E%)
120 100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 6 Simultaneous extraction of MG and MB dyes with initial concentration of 60 mg L1 for PIM II and PIM V.
The fast uptake of basic dyes at the beginning of extraction process as shown in Figs. 4–8 may be attributed to the rapid complexation of dye molecules with the extractant. The different uptake of dye also may be affected by their molecular weight of dye [22–26]. The dye with lower molecular weight (MB) will diffuse faster into the membrane and forming the complex of dye-B2EHP and followed by dye with higher molecular weight (MG). The average percentage extraction of PIM V is higher than PIM II at an optimum pH 5.0 due to the complexation of positively charged dyes with negatively charged B2EHP. From the result showed in Figs. 4–8, the time taken for the simultaneous extraction process for PIM V is faster than PIM II, which is achieving more than 92% starting from 90 min for concentrations of 20–40 mg L1 and 120 min for 60–100 mg L–1, even though there was competition between extraction of MG and MB dyes. In addition, the extraction process for PIM V is faster than for PIM II due to the optimum concentration of B2EHP to extract the dyes rapidly.
Av. percentage extraction (E%)
120
4. Conclusion 100 80 60
PIM II PIM V
40 20 0 0
50
100
150 200 Time (min)
250
300
Fig. 7 Simultaneous extraction of MG and MB dyes with initial concentration of 40 mg L1 for PIM II and PIM V.
A batch reactor consisting a PIM was successfully developed to extract MG and MB dyes simultaneously from an aqueous solution. The extraction of the dyes is influenced by three main parameters, the membrane composition, the initial dyes’ concentrations and the pH of the feeding solution. The PIM prepared is highly capable of performing simultaneous extraction of two dyes in an aqueous solution due to its extraction capability and membrane properties (mechanically and chemically stable). In order to explore the potential application of this dyes recovery system, additional studies are currently been carried such as optimizing the PIM in terms of stability and size, increasing the concentration of dyes and testing the system with real wastewater samples. Declaration of Competing Interest
Av. percentage extraction (E%)
120
None.
100
Acknowledgement
80 60
PIM II
Authors would like to acknowledge Universiti Sains Malaysia for providing financial assistance through Bridging grant scheme (304.PKIMIA.6316215).
PIM V
40
Appendix A. Supplementary material
20 0 0
50
100
150 200 Time (min)
250
300
Fig. 8 Simultaneous extraction of MG and MB dyes with initial concentration of 20 mg L1 for PIM II and PIM V.
due to the saturation of the membrane area, which does not allow any further extraction. Nevertheless, this limitation can be overcome by utilizing a PIM with a higher surface area or using a different cell arrangement (e.g. flow-through cell) for the extraction process.
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