Precision Engineered Graphene Oxide Membranes Optimizing Thin Film Composite Layers for Solvent and Dye Separation
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Keywords:
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Membrane, Organic Solvent Nanofiltration, Graphene Oxide, Thin-film Composite, Interfacial Polymerization
Abstract
Organic solvent nanofiltration (OSN) is a promising separation technology with low energy consumption and environmental benefits. However, membrane stability in harsh organic solvents remains a challenge. Graphene oxide (GO) is widely explored due to its exceptional mechanical strength and selective permeability; however, further modifications are necessary to optimize its performance. This study investigates the enhancement of GO membranes by incorporating a thin-film composite (TFC) layer through interfacial polymerization using polyethyleneimine (PEI) and trimethyl chloride (TMC). The fabricated membranes were characterized for their
morphology, chemical structure, and filtration performance using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), X-ray Photoelectron Spectroscopy (XPS), and contact angle measurements. Filtration tests were conducted with ethanol and Congo red dye solutions. The optimized membrane, composed of 0.1 wt% PEI 800 Mw and 0.05 wt% TMC, exhibited superior performance, demonstrating a permeance of 8.06 ± 2.31 L L m-2 h-1 bar-1 and a rejection rate of 95.20 ± 1.54% for Congo red dye. Additionally, the membrane exhibited a charge-dependent separation mechanism, achieving a 98.64 ± 0.38% rejection of methyl green due to both affinity and Donnan effects. These findings provide insights into developing advanced OSN membranes for efficient solvent purification and dye separation.
References
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Chang, C.-M., H.-T. Chen, S.-H. Chuang, H.-C. Tsai, W.-S. Hung, and J.-Y. Lai (2021). Mechanisms of One-Dimensional and Two-Dimensional Synergistic Thermal Responses on Graphene Oxide-Modified PNIPAm Framework Membranes for Control of Molecular Separation. Separation and Purification Technology, 266; 118568.
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Cheng, X., Y. Qin, Y. Ye, X. Chen, K. Wang, Y. Zhang, A. Figoli, and E. Drioli (2021). Finely Tailored Pore Structure of Polyamide Nanofiltration Membranes for Highly Efficient Application in Water Treatment. Chemical Engineering Journal, 417; 127976.
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Gontarek-Castro, E. and R. Castro-Muñoz (2024). How to Make Membrane Distillation Greener: A Review of Environmentally Friendly and Sustainable Aspects. Green Chemistry, 26(1); 164–185.
Grzebyk, K., M. D. Armstrong, and O. Coronell (2022). Accessing Greater Thickness and New Morphology Features in Polyamide Active Layers of Thin-Film Composite Membranes by Reducing Restrictions in Amine Monomer Supply. Journal of Membrane Science, 644; 120112.
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Marchetti, P., M. F. Jimenez Solomon, G. Szekely, and A. G. Livingston (2014). Molecular Separation With Organic Solvent Nanofiltration: A Critical Review. Chemical Reviews, 114(21); 10735–10806.
Naibaho, M., J. Widakdo, B. Kurniawan, P. Z. Z. Nehan, O. Vitayaya, W. A. Adi, and M. Ginting (2024). Analysis of Structure, Morphology, Magnetic Properties, and Microwave Absorption of Lanthanum Orthoferrite (LaFeO₃). Science and Technology Indonesia, 9(4); 851–856.
Nawi, N. S. M., W. J. Lau, P. S. Goh, J. W. Chew, S. Gray, N. Yusof, and A. F. Ismail (2024). The Impacts of 2D Graphene Oxide on Selective and Substrate Layer of TFC Membrane: A Critical Review on Fabrication Techniques and Performance in Water Treatment. Journal of Environmental Chemical Engineering, 12(2); 112298.
Nie, L., C. Y. Chuah, T. H. Bae, and J. M. Lee (2021). Graphene–Based Advanced Membrane Applications in Organic Solvent Nanofiltration. Advanced Functional Materials, 31(6); 2006949.
Oguzie, K., E. Oguzie, S. Nwanonenyi, J. Edoziem, and L. Vrsalović (2021). Electrochemical Decolorization of Disperse Blue-1 Dye in Aqueous Solution. Environmental Engineering & Management Journal (EEMJ), 20(9); 1467–1476.
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Qian, Y., C. Zhou, and A. Huang (2018). Cross-Linking Modification With Diamine Monomers to Enhance Desalination Performance of Graphene Oxide Membranes. Carbon, 136; 28–37.
Rianjanu, A., S. A. Muhtar, H. F. M. Austria, T. Taher, N. S. Gultom, W. H. Saputera, H. S. Wasisto, F. F. Abdi, W.-S. Hung, and J. Widakdo (2025). 3D Hierarchical Rare-Earth Metal Composite Nanofiber Membranes for Highly Durable and Efficient Photodegradations of Organic Pollutants. Materials Advances, 6(5); 1755–1768.
Saeedi, M., B. Malekmohammadi, and S. Tajalli (2024). Interaction of Benzene, Toluene, Ethylbenzene, and Xylene With Human’s Body: Insights Into Characteristics, Sources and Health Risks. Journal of Hazardous Materials Advances, 16; 100459.
Shen, L., J. Zuo, and Y. Wang (2017). Tris (2-aminoethyl) Amine In-Situ Modified Thin-Film Composite Membranes for Forward Osmosis Applications. Journal of Membrane Science, 537; 186–201.
Subrahmanya, T., J. Widakdo, S. Mani, H. F. M. Austria, W.-S. Hung, M. HK, J. K. Nagar, C.-C. Hu, and J.-Y. Lai (2022). An Eco-Friendly and Reusable Syringe Filter Membrane for the Efficient Removal of Dyes From Water Via Low Pressure Filtration Assisted Self-Assembling of Graphene Oxide and SBA-15/PDA. Journal of Cleaner Production, 349; 131425.
Swan, N. B. and M. A. A. Zaini (2019). Adsorption of Malachite Green and Congo Red Dyes From Water: Recent Progress and Future Outlook. Ecological Chemistry and Engineering S, 26(1); 119–132.
Thebo, K. H., X. Qian, Q. Zhang, L. Chen, H.-M. Cheng, and W. Ren (2018). Highly Stable Graphene-Oxide-Based Membranes With Superior Permeability. Nature Communications, 9(1); 1486.
Tian, L., N. Graham, T. Liu, K. Sun, and W. Yu (2022). Dual-Site Supported Graphene Oxide Membrane With Enhanced Permeability and Selectivity. Journal of Membrane Science, 646; 120223.
Volkov, A. V., V. V. Parashchuk, D. F. Stamatialis, V. S. Khotimsky, V. V. Volkov, and M. Wessling (2009). High Permeable PTMSP/PAN Composite Membranes for Solvent Nanofiltration. Journal of Membrane Science, 333(1–2); 88–93.
Wan, X., Y. Huang, and Y. Chen (2012). Focusing on Energy and Optoelectronic Applications: A Journey for Graphene and Graphene Oxide at Large Scale. Accounts of Chemical Research, 45(4); 598–607.
Wang, Y.-C., W.-J. Wang, Q. Wang, Z.-Y. Wang, X.-Y. Yan, L.-L. Zhao, X.-L. Cao, and S.-P. Sun (2022). Solvent Remelted Nylon Polyamide Nanofibrous Substrate That Enhances Thin-Film Composite Membranes for Organic Solvent Nanofiltration. Separation and Purification Technology, 285; 120322.
Wang, Z., X. Luo, J. Zhang, F. Zhang, W. Fang, and J. Jin (2023). Polymer Membranes for Organic Solvent Nanofiltration: Recent Progress, Challenges and Perspectives. Advanced Membranes, 3; 100063.
Wei, J., X. Liu, C. Qiu, R. Wang, and C. Y. Tang (2011). Influence of Monomer Concentrations on the Performance of Polyamide-Based Thin Film Composite Forward Osmosis Membranes. Journal of Membrane Science, 381(1–2); 110–117.
Wen, H. and C. Liu (2022). Effect of the Interlayer Construction on the Performances of the TFC-FO Membranes: A Review From Materials Perspective. Desalination, 541; 116033.
Widakdo, J., G. T. M. Kadja, A. Anawati, T. Subrahmanya, H. F. M. Austria, T.-H. Huang, E. Suharyadi, and W.-S. Hung (2023). Graphene Oxide–Melamine Nanofilm Composite Membrane for Efficient CO₂ Gas Separation. Separation and Purification Technology, 323; 124521.
Wu, L., X. Liu, G. Lv, R. Zhu, L. Tian, M. Liu, Y. Li, W. Rao, T. Liu, and L. Liao (2021). Study on the Adsorption Properties of Methyl Orange by Natural One-Dimensional Nano-Mineral Materials With Different Structures. Scientific Reports, 11(1); 10640.
Xiao, H., Y. Feng, W. R. Goundry, and S. Karlsson (2024). Organic Solvent Nanofiltration in Pharmaceutical Applications. Organic Process Research & Development, 28(4); 891–923.
Xie, X., Y. Wang, W. Zhou, C. Chen, and Z. Xiong (2021). Investigation of U(VI) Adsorption Properties of Poly (Trimesoyl Chloride-Co-Polyethyleneimine). Journal of Solid State Chemistry, 296; 121966.
Xu, Q., H. Xu, J. Chen, Y. Lv, C. Dong, and T. S. Sreeprasad (2015). Graphene and Graphene Oxide: Advanced Membranes for Gas Separation and Water Purification. Inorganic Chemistry Frontiers, 2(5); 417–424.
Xu, Y., F. You, H. Sun, and L. Shao (2017). Realizing Mussel-Inspired Polydopamine Selective Layer With Strong Solvent Resistance in Nanofiltration Toward Sustainable Reclamation. ACS Sustainable Chemistry & Engineering, 5(6); 5520–5528.
Yang, Y., G. Li, D. Ouyang, Z. Cai, and Z. Lin (2023). Dual-Activation Interfacial Polymerization Based Anionic Covalent Organic Framework Nanofiltration Membrane for High-Flux Dye Separation. Chemical Engineering Journal, 456; 141008.
Zhai, Z., X. Wang, Y. Huang, H. Yang, and Y. Zhao (2023). Fabrication of Advanced Positively Charged Polyamide Nanofiltration Membrane for Effective Removal of Heavy Metal Ions Via Surfactant-Plasticizer-Synergy Assisted Interfacial Polymerization. Separation and Purification Technology, 322(1); 124216.
Zhao, S., Z. Zha, C. Mao, Z. Wang, and J. Wang (2022). In-Situ Fabricated Covalent Organic Frameworks-Polyamide Hybrid Membrane for Highly Efficient Molecular Separation. Journal of Membrane Science, 653; 120544.
Abegunde, S. M., M. A. Adebayo, and E. F. Olasehinde (2024). Green Synthesis of ZnO Nanoparticles and Its Application for Methyl Green Dye Adsorption. Green Energy and Resources, 2(2); 100073.
Amri, A., A. Lesbani, and R. Mohadi (2023). Malachite Green Dye Adsorption From Aqueous Solution Using a Ni/Al Layered Double Hydroxide–Graphene Oxide Composite Material. Science and Technology Indonesia, 8(2); 280–287.
Austria, H. F. M., J. Widakdo, O. Setiawan, T. Subrahmanya, W.-S. Hung, C.-F. Wang, C.-C. Hu, K.-R. Lee, and J.-Y. Lai (2023). Tailoring the Specific Crosslinking Sites of Graphene Oxide Framework Nanosheets for Controlled Nanofiltration of Salts and Dyes. Journal of Cleaner Production, 395; 136280.
Barton, S. S. (1987). The Adsorption of Methylene Blue by Active Carbon. Carbon, 25(3); 343–350.
Chang, C.-M., H.-T. Chen, S.-H. Chuang, H.-C. Tsai, W.-S. Hung, and J.-Y. Lai (2021). Mechanisms of One-Dimensional and Two-Dimensional Synergistic Thermal Responses on Graphene Oxide-Modified PNIPAm Framework Membranes for Control of Molecular Separation. Separation and Purification Technology, 266; 118568.
Chen, D., H. Feng, and J. Li (2012). Graphene Oxide: Preparation, Functionalization, and Electrochemical Applications. Chemical Reviews, 112(11); 6027–6053.
Cheng, X., Y. Qin, Y. Ye, X. Chen, K. Wang, Y. Zhang, A. Figoli, and E. Drioli (2021). Finely Tailored Pore Structure of Polyamide Nanofiltration Membranes for Highly Efficient Application in Water Treatment. Chemical Engineering Journal, 417; 127976.
Cseri, L., M. Razali, P. Pogany, and G. Szekely (2018). Organic Solvents in Sustainable Synthesis and Engineering. In Green Chemistry. Elsevier, pp. 513–553.
Farahani, M. H. D. A. and T.-S. Chung (2018). Solvent Resistant Hollow Fiber Membranes Comprising P84 Polyimide and Amine-Functionalized Carbon Nanotubes with Potential Applications in Pharmaceutical, Food, and Petrochemical Industries. Chemical Engineering Journal, 345; 174–185.
Gontarek-Castro, E. and R. Castro-Muñoz (2024). How to Make Membrane Distillation Greener: A Review of Environmentally Friendly and Sustainable Aspects. Green Chemistry, 26(1); 164–185.
Grzebyk, K., M. D. Armstrong, and O. Coronell (2022). Accessing Greater Thickness and New Morphology Features in Polyamide Active Layers of Thin-Film Composite Membranes by Reducing Restrictions in Amine Monomer Supply. Journal of Membrane Science, 644; 120112.
Gu, S., S. Li, and Z. Xu (2024). Organic Solvent Nanofiltration Membranes for Separation in Non-Polar Solvent System. Green Energy & Environment, 10(2); 244–267.
Hermans, S., E. Dom, H. Mariën, G. Koeckelberghs, and I. F. Vankelecom (2015). Efficient Synthesis of Interfacially Polymerized Membranes for Solvent Resistant Nanofiltration. Journal of Membrane Science, 476; 356–363.
Huang, L., J. Chen, T. Gao, M. Zhang, Y. Li, L. Dai, L. Qu, and G. Shi (2016). Reduced Graphene Oxide Membranes for Ultrafast Organic Solvent Nanofiltration. Advanced Materials, 28(39); 8669–8674.
Ji, C., Z. Zhai, C. Jiang, P. Hu, S. Zhao, S. Xue, Z. Yang, T. He, and Q. J. Niu (2021). Recent Advances in High-Performance TFC Membranes: A Review of the Functional Interlayers. Desalination, 500; 114869.
Joshi, D. R. and N. Adhikari (2019). An Overview on Common Organic Solvents and Their Toxicity. Journal of Pharmaceutical Research International, 28(3); 1–18.
Joshi, R. K., S. Alwarappan, M. Yoshimura, V. Sahajwalla, and Y. Nishina (2015). Graphene Oxide: The New Membrane Material. Applied Materials Today, 1(1); 1–12.
Kang, Y., J. Jang, S. Kim, J. Lim, Y. Lee, and I. S. Kim (2020). PIP/TMC Interfacial Polymerization with Electrospray: Novel Loose Nanofiltration Membrane for Dye Wastewater Treatment. ACS Applied Materials & Interfaces, 12(32); 36148–36158.
Liu, L., J. Zhang, J. Zhao, and F. Liu (2012). Mechanical Properties of Graphene Oxides. Nanoscale, 4(19); 5910–5916.
Marchetti, P., M. F. Jimenez Solomon, G. Szekely, and A. G. Livingston (2014). Molecular Separation With Organic Solvent Nanofiltration: A Critical Review. Chemical Reviews, 114(21); 10735–10806.
Naibaho, M., J. Widakdo, B. Kurniawan, P. Z. Z. Nehan, O. Vitayaya, W. A. Adi, and M. Ginting (2024). Analysis of Structure, Morphology, Magnetic Properties, and Microwave Absorption of Lanthanum Orthoferrite (LaFeO₃). Science and Technology Indonesia, 9(4); 851–856.
Nawi, N. S. M., W. J. Lau, P. S. Goh, J. W. Chew, S. Gray, N. Yusof, and A. F. Ismail (2024). The Impacts of 2D Graphene Oxide on Selective and Substrate Layer of TFC Membrane: A Critical Review on Fabrication Techniques and Performance in Water Treatment. Journal of Environmental Chemical Engineering, 12(2); 112298.
Nie, L., C. Y. Chuah, T. H. Bae, and J. M. Lee (2021). Graphene–Based Advanced Membrane Applications in Organic Solvent Nanofiltration. Advanced Functional Materials, 31(6); 2006949.
Oguzie, K., E. Oguzie, S. Nwanonenyi, J. Edoziem, and L. Vrsalović (2021). Electrochemical Decolorization of Disperse Blue-1 Dye in Aqueous Solution. Environmental Engineering & Management Journal (EEMJ), 20(9); 1467–1476.
Pan, Z., L. He, L. Qiu, A. H. Korayem, G. Li, J. W. Zhu, F. Collins, D. Li, W. H. Duan, and M. C. Wang (2015). Mechanical Properties and Microstructure of a Graphene Oxide–Cement Composite. Cement and Concrete Composites, 58; 140–147.
Qian, Y., C. Zhou, and A. Huang (2018). Cross-Linking Modification With Diamine Monomers to Enhance Desalination Performance of Graphene Oxide Membranes. Carbon, 136; 28–37.
Rianjanu, A., S. A. Muhtar, H. F. M. Austria, T. Taher, N. S. Gultom, W. H. Saputera, H. S. Wasisto, F. F. Abdi, W.-S. Hung, and J. Widakdo (2025). 3D Hierarchical Rare-Earth Metal Composite Nanofiber Membranes for Highly Durable and Efficient Photodegradations of Organic Pollutants. Materials Advances, 6(5); 1755–1768.
Saeedi, M., B. Malekmohammadi, and S. Tajalli (2024). Interaction of Benzene, Toluene, Ethylbenzene, and Xylene With Human’s Body: Insights Into Characteristics, Sources and Health Risks. Journal of Hazardous Materials Advances, 16; 100459.
Shen, L., J. Zuo, and Y. Wang (2017). Tris (2-aminoethyl) Amine In-Situ Modified Thin-Film Composite Membranes for Forward Osmosis Applications. Journal of Membrane Science, 537; 186–201.
Subrahmanya, T., J. Widakdo, S. Mani, H. F. M. Austria, W.-S. Hung, M. HK, J. K. Nagar, C.-C. Hu, and J.-Y. Lai (2022). An Eco-Friendly and Reusable Syringe Filter Membrane for the Efficient Removal of Dyes From Water Via Low Pressure Filtration Assisted Self-Assembling of Graphene Oxide and SBA-15/PDA. Journal of Cleaner Production, 349; 131425.
Swan, N. B. and M. A. A. Zaini (2019). Adsorption of Malachite Green and Congo Red Dyes From Water: Recent Progress and Future Outlook. Ecological Chemistry and Engineering S, 26(1); 119–132.
Thebo, K. H., X. Qian, Q. Zhang, L. Chen, H.-M. Cheng, and W. Ren (2018). Highly Stable Graphene-Oxide-Based Membranes With Superior Permeability. Nature Communications, 9(1); 1486.
Tian, L., N. Graham, T. Liu, K. Sun, and W. Yu (2022). Dual-Site Supported Graphene Oxide Membrane With Enhanced Permeability and Selectivity. Journal of Membrane Science, 646; 120223.
Volkov, A. V., V. V. Parashchuk, D. F. Stamatialis, V. S. Khotimsky, V. V. Volkov, and M. Wessling (2009). High Permeable PTMSP/PAN Composite Membranes for Solvent Nanofiltration. Journal of Membrane Science, 333(1–2); 88–93.
Wan, X., Y. Huang, and Y. Chen (2012). Focusing on Energy and Optoelectronic Applications: A Journey for Graphene and Graphene Oxide at Large Scale. Accounts of Chemical Research, 45(4); 598–607.
Wang, Y.-C., W.-J. Wang, Q. Wang, Z.-Y. Wang, X.-Y. Yan, L.-L. Zhao, X.-L. Cao, and S.-P. Sun (2022). Solvent Remelted Nylon Polyamide Nanofibrous Substrate That Enhances Thin-Film Composite Membranes for Organic Solvent Nanofiltration. Separation and Purification Technology, 285; 120322.
Wang, Z., X. Luo, J. Zhang, F. Zhang, W. Fang, and J. Jin (2023). Polymer Membranes for Organic Solvent Nanofiltration: Recent Progress, Challenges and Perspectives. Advanced Membranes, 3; 100063.
Wei, J., X. Liu, C. Qiu, R. Wang, and C. Y. Tang (2011). Influence of Monomer Concentrations on the Performance of Polyamide-Based Thin Film Composite Forward Osmosis Membranes. Journal of Membrane Science, 381(1–2); 110–117.
Wen, H. and C. Liu (2022). Effect of the Interlayer Construction on the Performances of the TFC-FO Membranes: A Review From Materials Perspective. Desalination, 541; 116033.
Widakdo, J., G. T. M. Kadja, A. Anawati, T. Subrahmanya, H. F. M. Austria, T.-H. Huang, E. Suharyadi, and W.-S. Hung (2023). Graphene Oxide–Melamine Nanofilm Composite Membrane for Efficient CO₂ Gas Separation. Separation and Purification Technology, 323; 124521.
Wu, L., X. Liu, G. Lv, R. Zhu, L. Tian, M. Liu, Y. Li, W. Rao, T. Liu, and L. Liao (2021). Study on the Adsorption Properties of Methyl Orange by Natural One-Dimensional Nano-Mineral Materials With Different Structures. Scientific Reports, 11(1); 10640.
Xiao, H., Y. Feng, W. R. Goundry, and S. Karlsson (2024). Organic Solvent Nanofiltration in Pharmaceutical Applications. Organic Process Research & Development, 28(4); 891–923.
Xie, X., Y. Wang, W. Zhou, C. Chen, and Z. Xiong (2021). Investigation of U(VI) Adsorption Properties of Poly (Trimesoyl Chloride-Co-Polyethyleneimine). Journal of Solid State Chemistry, 296; 121966.
Xu, Q., H. Xu, J. Chen, Y. Lv, C. Dong, and T. S. Sreeprasad (2015). Graphene and Graphene Oxide: Advanced Membranes for Gas Separation and Water Purification. Inorganic Chemistry Frontiers, 2(5); 417–424.
Xu, Y., F. You, H. Sun, and L. Shao (2017). Realizing Mussel-Inspired Polydopamine Selective Layer With Strong Solvent Resistance in Nanofiltration Toward Sustainable Reclamation. ACS Sustainable Chemistry & Engineering, 5(6); 5520–5528.
Yang, Y., G. Li, D. Ouyang, Z. Cai, and Z. Lin (2023). Dual-Activation Interfacial Polymerization Based Anionic Covalent Organic Framework Nanofiltration Membrane for High-Flux Dye Separation. Chemical Engineering Journal, 456; 141008.
Zhai, Z., X. Wang, Y. Huang, H. Yang, and Y. Zhao (2023). Fabrication of Advanced Positively Charged Polyamide Nanofiltration Membrane for Effective Removal of Heavy Metal Ions Via Surfactant-Plasticizer-Synergy Assisted Interfacial Polymerization. Separation and Purification Technology, 322(1); 124216.
Zhao, S., Z. Zha, C. Mao, Z. Wang, and J. Wang (2022). In-Situ Fabricated Covalent Organic Frameworks-Polyamide Hybrid Membrane for Highly Efficient Molecular Separation. Journal of Membrane Science, 653; 120544.
Authors
Widakdo, J., Fadly Azril Priodani, Hannah Faye M. Austria, Tsung Han-Huang, Aditya Rianjanu, Canggih Setya Budi, Anawati Anawati, & Wei-Song Hung. (2025). Precision Engineered Graphene Oxide Membranes Optimizing Thin Film Composite Layers for Solvent and Dye Separation. Science and Technology Indonesia, 10(4), 1031–1048. https://doi.org/10.26554/sti.2025.10.4.1031-1048
This work is licensed under a Creative Commons Attribution 4.0 International License.