MXene/MIL-101 Nanocomposite with Octahedral and Rod-like Morphology: Synthesis and Application in Rhodamine B Removal

Document Type : Original Article

Authors

1 Department of Environment, Institute of Science and High Technology and Environmental Sciences, Graduate University of Advanced Technology, P.O. Box: 76315-117, Kerman, Iran

2 Department of Chemistry, Iran University of Science and Technology, P.O. Box: 16846-13114, Tehran, Iran

10.30509/jcst.2026.167811.1286

Abstract

In this study, MXene/MIL-101 nanocomposites with two different morphologies, octahedral (via solvothermal method) and rod-like (via reflux method), were synthesized. The synthesized products were characterized using XRD, FTIR, and SEM analyses. The results of the structural analyses showed that the synthesis method has a significant effect on the morphology of the nanocomposites, such that the solvothermal synthesis led to the formation of octahedral particles, while the reflux method produced rod-like particles. Rhodamine B adsorption experiments demonstrated that both nanocomposites exhibit high performance in dye removal. Furthermore, the nanocomposite with octahedral morphology showed a higher removal efficiency (about 93%) compared to the rod-like morphology (about 85%). The maximum adsorption capacity under optimal conditions (i.e., pH = 7, adsorbent dosage = 0.05 g, and contact time = 50 min) was found to be 61.73 mg g⁻¹ for the adsorbent synthesized via the solvothermal method. The kinetic data were analyzed using the Lagergren pseudo-first-order and pseudo-second-order equations, and the pseudo-second-order model showed the best fit for the kinetic studies (R² > 0.99). Moreover, the reusability study showed that the proposed adsorbent retains its favorable performance even after six adsorption-regeneration cycles. Finally, the findings of this study indicate that the MXene/MIL-101 nanocomposite synthesized via the solvothermal method is an efficient adsorbent for the removal of organic dyes and can play an effective role in the development of novel water treatment technologies.

Keywords

Main Subjects

References

  1. Dousti S, Mahmoodi B, Bijari M, Shahbazi A, Investigating the Effect of Various Precursors in the Synthesis and Improvement of the Photocatalytic Performance of Graphite Carbon Nitride in the Degradation of Rhodamine B Dye Under Visible Light. J Color Sci Tech. 2024;18(2):135-150. https://doi.org/10.30509/JCST.2024.167291.1224. [In Persian].
  2. Safa MB, Steffy J, Syed A, Subhiksha V, Elgorban AM, Verma M, et al. Unveiling the enhanced rhodamine B degradation in water by Sn3O4@ Au: Insight into degra-dation pathway and by-products toxicity evaluation. J Water Process Eng. 2025;72:107475. https://doi.org/10.1016/j. jwpe.2025.107475.
  3. Liu D, Chen D, Hao Z, Tang Y, Jiang L, Li T, et al. Efficient degradation of Rhodamine B in water by CoFe2O4/H2O2 and CoFe2O4/PMS systems: A comparative study. Chemosphere. 2022; 307:135935. https://doi.org/10.1016/j.chemosphere. 2022.135935.
  4. Fayazi M. Synthesis of ZnO nanostructures with different morphologies on biochar support for photocatalytic degradation of organic dye. J Water Environ Nanotechnol. 2024;9(2):137-148. https://doi.org/10.22090/jwent.2024.02. 02.
  5. Ahmad S, Mujtaba G, Zubair M, Shah MUH, Daud M, Mu'azu ND, et al. A review of performance, mechanism, and challenges of layered double hydroxide-based biocomposites for the adsorptive removal of dye contaminants from water and wastewater. J Water Process Eng. 2025;70:106837. cess to Document. https://doi.org/ 10.1016/j.jwpe.2024.106837.
  6. Farazmand S, Fayazi M. Single-step solvothermal synthesis of sepiolite-CoFe2O4 nanocomposite as a highly efficient heterogeneous catalyst for photo Fenton-like reaction. Mater Chem Phys. 2024;312:128627. https://doi.org/10.1016/j. matchemphys.2023.128627.
  7. Bhatia D, Sharma NR, Singh J, Kanwar RS. Biological methods for textile dye removal from wastewater: A review. Critical Reviews Environ Sci Technol. 2017;47(19):1836-1876 https://doi.org/10.1080/10643389.2017.1393263.
  8. Jafaryan P, Foroughirad S. Magnetic Molecularly Imprinted Polymers: Fundamentals, Synthesis, Characterization, and Adsorptive Applications in the Removal of Organic Contaminants from Water and Wastewater. J Color Sci Tech. 2026;20(1):17-36. https://doi.org/10.30509/jcst.2026. 167783.1284 [In Persian].
  9. Eslaminejad S, Rahimi R, Fayazi M. Sepiolite-metal organic framework-iron oxide catalyst for degradation of Rhodamine B using Fenton-like process. J Taiwan Inst Chem Eng. 2023; 152:105181. https://doi.org/10.1016/j.jtice.2023.105181.
  10. Gharanjig K, Kazemian H, Hosseinnezhad M, Ghasemi E, Etezad SM, Goudarzi S, Imani H, Gharanjig H. Removal of Reseda Luteola Dyes in Dyeing Wastewater by Metal-organic Framework Adsorbent. J Color Sci Tech. 2024; 18(2):79-92. https://doi.org/10.30509/JCST.2024.82014. [In Persian].
  11. Akiyama G, Matsuda R, Sato H, Hori A, Takata M, Kitagawa S. Effect of functional groups in MIL-101 on water sorption behavior. Microporous and Mesoporous Materials. 2012;157:89-93. https://doi.org/ 10.1016/j. micromeso.2012.01.015.
  12. Zorainy MY, Gar Alalm M, Kaliaguine S, Boffito DC. Revisiting the MIL-101 metal–organic framework: design, synthesis, modifications, advances, and recent applications. J Mater Chem A. 2021;9(39):22159-217. https://doi.org/ 10.1039/D1TA06238G.
  13. Far HS, Hasanzadeh M, Najafi M, Rabbani M. Magnetic metal-organic framework (Fe3O4@ MIL-101) functionalized with dendrimer: Highly efficient and selective adsorption removal of organic dyes. Journal of Inorganic and Organometallic Polymers and Materials. 2022;32(10):3848-63. https://doi.org/10.1007/s10904-022-02398-7.
  14. Hasanzadeh M, Simchi A, Far HS. Nanoporous composites of activated carbon-metal organic frameworks for organic dye adsorption: Synthesis, adsorption mechanism and kinetics studies. J Ind Eng Chem. 2020;81:405-14. https://doi.org/10.1016/j.jiec.2019.09.031.
  15. Song Y, Zheng S, Ji Y, He B, Wang M. Fabrication of novel mixed matrix composite membranes with polyethylen-eimine-modified MIL-101 for CO2/CH4 separation. Chem Eng J. 2025;518:164526. https://doi.org/10.1016/j.cej. 2025.164526.
  16. Lei J-C, Zhang X, Zhou Z. Recent advances in MXene: Preparation, properties, and applications. Front Phys. 2015; 10(3):276-86. https://doi.org/10.1007/s11467-015-0493-x.
  17. Qu L, Wu M, Zhao L, Li J, Pan H. A sandwich electrochemical immunosensor based on MXene@ dual MOFs for detection of tumor marker CA125. Microchim Acta. 2023;190(4):147. https://doi.org/10.1007/s00604-023-05719-w.
  18. Stock N, Biswas S. Synthesis of metal-organic frameworks (MOFs): routes to various MOF topologies, morphologies, and composites. Chemical reviews. 2012;112(2):933-69. https://doi.org/ org/10.1021/cr200304e.
  19. Huang L, Wang H, Chen J, Wang Z, Sun J, Zhao D, et al. Synthesis, morphology control, and properties of porous metal–organic coordination polymers. Microporous Mesoporous Mater. 2003;58(2):105-14. https://doi.org/10. 1016/S1387-1811(02)00609-1.
  20. Choi J, Choi J-S, Park D, Park CM, Jang M, Jun B-M, et al. Applications of MXene-based nanomaterials for the removal of inorganic contaminants from water: A review. Journal of Hazardous Materials. 2026;504:141312. https://doi.org/10. 1016/j.jhazmat.2026.141312. 
  21. Huo J-B, Qin T, Cheng R, Guo X, Yu G. MXene-based composites as emerging adsorbents for removal of environmental pollutants. Sep Purif Technol. 2025:134408. https://doi.org/10.1016/j.seppur.2025.134408.
  22. Chen Y, Shi Y, Song G, Yang B, Pang H. Compositing MXene with organic coordination frameworks (MOFs, COFs, and HOFs) for enhanced electrochemical performance. Next Mater. 2025;6:100323. https://doi.org/ 10.1016/j.nxmate.2024.100323.
  23. Kashif S, Akram S, Murtaza M, Amjad A, Shah SSA, Waseem A. Development of MOF-MXene composite for the removal of dyes and antibiotic. Diamond Relat Mater. 2023; 136:110023.https://doi.org/10.1016/j.diamond.2023.110023.
  24. Khurram A, Jabbar A, Khan MA, Liu W, Mutahir S, Munir A, et al. 7pH-responsive MIL-101 (Fe)/NiFe-LDH composite membranes for high-flux removal of cationic and anionic dyes in wastewater treatment. Desalin. 2025:119438. https://doi.org/10.1016/j.desal.2025.119438.
  25. Safarkhani M, Aldhaher A, Lima EC, Zargar M, Jung EE, Huh Y, et al. Engineering MXene@ MOF composites for a wide range of applications: a perspective. ACS Applied Engineering Materials. 2023;1(11):3080-98. https://doi.org/ 10.1021/acsaenm.3c00529.
  26. Khot AC, Dongale TD, Park JH, Kesavan AV, Kim TG. Ti3C2-based MXene oxide nanosheets for resistive memory and synaptic learning applications. ACS Appl Mater Interfaces. 2021;13(4):5216-27. https://doi.org/10.1021/ acsami.0c19028.
  27. Li Z, Wang L, Sun D, Zhang Y, Liu B, Hu Q, et al. Synthesis and thermal stability of two-dimensional carbide MXene Ti3C2. Mater Sci Eng B. 2015;191:33-40. https://doi. org/10.1016/j.mseb.2014.10.009.
  28. Liu X, Liu Z, Zhang Q, Wu H, Wang R. Hydrothermal Catalytic Conversion of Glucose into Lactic Acid with Acidic MIL‐101 (Fe). J Chem. 2020;2020(1):1341563. https://doi.org/10.1155/2020/1341563.
  29. Edebali S. Synthesis and characterization of MIL-101 (Fe) as efficient catalyst for tetracycline degradation by using NaBH4: Artificial neural network modeling. Appl Surf Sci Adv.2023;18:100496. https://doi.org/10.1016/j.apsadv.2023. 100496.
  30. Haq Y-U, Ullah R, Mazhar S, Khattak R, Qarni AA, Haq Z-U, et al. Synthesis and characterization of 2D MXene: Device fabrication for humidity sensing. J Sci: Adv Mater Devices. 2022;7(1):100390. https://doi.org/10.1016/j.jsamd. 2021.08.003.
  31. Lee E, VahidMohammadi A, Prorok BC, Yoon YS, Beidaghi M, Kim D-J. Room temperature gas sensing of two-dimensional titanium carbide (MXene). ACS Appl Mater Interfaces. 2017;9(42):37184-90. https://doi.org/10. 1021/acsami.7b11055.
  32. Xue Q, Zhang H, Zhu M, Pei Z, Li H, Wang Z, et al. Photoluminescent Ti3C2 MXene quantum dots for multicolor cellular imaging. Adv Mater. 2017;29(15). https://doi.org/ 10.1002/adma.201604847.
  33. Hamedi A, Trotta F, Borhani Zarandi M, Zanetti M, Caldera F, Anceschi A, et al. In situ synthesis of MIL-100 (Fe) at the surface of Fe3O4@ AC as highly efficient dye adsorbing nanocomposite. Int J Mol Sci. 2019;20(22):5612. https://doi. org/10.3390/ijms20225612.
  34. Li Z, Liu X, Jin W, Hu Q, Zhao Y. Adsorption behavior of arsenicals on MIL-101 (Fe): the role of arsenic chemical structures. J Colloid Interface Sci. 2019;554:692-704. https://doi.org/10.1016/j.jcis.2019.07.046
  35. Liu Z, He W, Zhang Q, Shapour H, Bakhtari MF. Preparation of a GO/MIL-101 (Fe) composite for the removal of methyl orange from aqueous solution. ACS omega. 2021;6(7):4597-608. https://doi.org/10.1021/acsomega.0c05091.
  36. Zheng S, Zhou K, Zhang X, Ren N. Metal-organic framework/MXene-based materials: preparations and applications. RSC Adv. 2025;15(37):30921-68. https://doi. org/10.1039/d5ra04436g.
  37. Liao X, Wang F, Wang F, Cai Y, Yao Y, Teng B-T, et al. Synthesis of (100) surface oriented MIL-88A-Fe with rod-like structure and its enhanced fenton-like performance for phenol removal. Appl Catal B. 2019;259:118064. https://doi. org/ 10.1016/j.apcatb.2019.118064.
  38. Chen M-S, Fan H-F, Lin K-C. Kinetic and thermodynamic investigation of Rhodamine B adsorption at solid/solvent interfaces by use of evanescent-wave cavity ring-down spectroscopy. Anal Chem. 2010;82(3):868-77. https://doi. org/ 10.1016/j.jscs.2011.01.002.
  39. Fayazi M, Taher MA, Afzali D, Mostafavi A. Preparation of molecularly imprinted polymer coated magnetic multi-walled carbon nanotubes for selective removal of dibenzothiophene. Mater Sci Semicond Process. 2015;40: 501-7. https://doi.org/10.1016/j.mssp.2015.07.018.
  40. Patel R, Mahabari K, Patel K, Patel M, Jadhav AH, Dharaskar S, et al. MoS2/MXene composite material for high-performance removal of Rhodamine B dye: synthesis and application. Sci Rep. 2025;15(1):42099. https://doi. org/10.1038/s41598-025-26240-5.
  41. Saad HE, Mahmoud A. Coumarin-modified cellulose as an efficient adsorbent for cationic dye removal from aqueous environments: synthesis, characterization, and adsorption performance. Sci Rep. 2025;15(1):32511. https://doi.org/ 10.1038/s41598-025-17789-2.
  42. Celik Caglar T, Kayranli B. Comparative evaluation of regeneration strategies for Rhodamine B removal using raw date seeds: Insights into adsorption mechanisms. ACS omega. 2026;11(25):37266-83. https://doi.org/10.1021/acsomega.6c 01845.
  43. Liu H, Ren X, Chen L. Synthesis and characterization of magnetic metal-organic framework for the adsorptive removal of Rhodamine B from aqueous solution. J Ind Eng Chem. 2016;34:278-85. https://doi.org/10.1016/j.jiec.2015. 11.020.
  44. Firoozi M, Rafiee Z, Dashtian K. New MOF/COF hybrid as a robust adsorbent for simultaneous removal of auramine O and rhodamine B dyes. ACS omega. 2020;5(16):9420. https://doi.org/10.1021/acsomega.0c00539.
  45. Shenvi SS, Isloor AM, Ismail AF, Shilton SJ, Al Ahmed A. Humic acid based biopolymeric membrane for effective removal of methylene blue and rhodamine B. Ind Eng Chem Res. 2015;54(18):4965-75. https://doi.org/10.1021/acs.iecr. 5b00761.

Files

Share

How to cite

Statistics