Metal-Organic Frameworks with Linear and Branched Polyol Backbones for Dye Removal

Metal-Organic Frameworks with Linear and Branched Polyol Backbones for Dye Removal | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article Metal-Organic Frameworks with Linear and Branched Polyol Backbones for Dye Removal Safoora Gazvineh, Mohsen Adeli, Mohammad Nemati This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-8050532/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 11 You are reading this latest preprint version Abstract In this study, novel metal-organic frameworks (MOFs) were synthesized using functionalized polyols as ligands. Polyvinyl alcohol (PVA) and hyperbranched polyglycerol (hPG) were first mesylated and subsequently modified with 5-aminoisophthalic acid. These functionalized polymers were then reacted with iron (III) chloride hexahydrate to form related MOFs including PVA-MOF and hPG-MOF. The resulting MOFs exhibited high adsorption capacities for both cationic dyes (Rhodamine B and Methylene Blue) and an anionic dye (Fluorescein) from aqueous solutions. Adsorption studies revealed that dye removal followed the Langmuir isotherm model, with maximum capacities reaching 128.17–135.34 mg.g − 1 depending on the type of dye and MOF. Thermodynamic analysis showed that adsorption was endothermic, with increased entropy, and spontaneous for the anionic dye, while non-spontaneous for the cationic dyes. The materials also demonstrated excellent structural stability and regeneration potential over three adsorption-desorption cycles. Furthermore, performance was confirmed using real water samples, indicating that PVA-MOF and hPG-MOF are promising, reusable adsorbents for efficient dye removal in wastewater treatment. Physical sciences/Chemistry Earth and environmental sciences/Environmental sciences Physical sciences/Materials science Metal-organic framework polyvinyl alcohol hyperbranched polymer poly(glycerol) MIL-101 (Fe) dye removal Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Introduction The rapid technological advancements of recent decades have raised significant environmental concerns, particularly regarding water pollution. As the most vital resource for life, protecting water bodies from contamination driven by population growth, urbanization, and industrialization is a global priority shared by governments and citizens alike. 1 In recent years, water quality has declined due to pollutants such as pharmaceuticals, personal care products, and especially organic dyes released by the textile, paper, food, cosmetics, and pharmaceutical industries. 2 These colored effluents pose severe health risks, including skin irritation, allergic reactions, organ dysfunction, and even cancer, particularly when absorbed through the skin or ingested. 3 As a result, significant efforts have been made to remove such dyes using techniques like ion exchange, coagulation, flocculation, and adsorption. 4 Adsorption, in particular, has garnered attention due to its efficiency and simplicity. It involves the adhesion of atoms, ions, or molecules (adsorbates) to the surface of a solid (adsorbent), particularly within its internal porous structure, which significantly enhances the surface area. 5 In this context, polymer-based metal-organic frameworks (MOFs) have emerged as promising adsorbents due to their tunable porosity and functional versatility. 6 MOFs are crystalline, porous materials composed of metal ions or clusters coordinated to organic ligands. Their applications span catalysis, gas separation, drug delivery, and adsorption 7 , 8 Among them, MIL-101 stands out for its mesoporous nature, large pore size, and chemical stability, particularly in organic solvents at room temperature. 9 Polymers are increasingly integrated with MOFs to create composite materials that are lightweight, cost-effective, and mechanically robust. 10 Research into MOF-polymer composites has evolved significantly since the early 2000s, with growing applications in sensing, separation, and environmental remediation. 11 PVA is a hydrophilic, semi-crystalline synthetic biopolymer known for its biodegradability, thermal stability, and strong film-forming and chemical resistance properties. 12 Its hydroxyl-rich structure facilitates strong hydrogen bonding, contributing to its semi-crystalline nature and compatibility with other materials. 13 Widely used in textiles, adhesives, medical products, and water treatment, 14,18 PVA does have limitations in mechanical strength and solvent resistance. These can be mitigated through cross-linking strategies, which enhance its network structure, reduce hydrophilicity, and improve its suitability for dye and heavy metal adsorption. 19 Hyperbranched polyglycerols (hPGs), on the other hand, offer another compelling polymer due to their biocompatibility, low toxicity, and simple one-step synthesis. 20 These highly branched, water-soluble polymers are under active investigation for pharmaceutical and biomedical applications, such as drug delivery and tissue engineering. 21 Their molecular weight and mechanical properties can be tuned via synthesis conditions, making them highly adaptable. 22 , 23 Combining MOFs with branched polyglycerol polymers results in porous hybrid materials that exhibit high surface area, tunable properties, and potential for use in environmental, energy, and biomedical fields. 24,25 In this study, stable PVA-MOF and hPG-MOF composites were synthesized and thoroughly characterized using techniques such as TGA, FTIR, SEM, EDX, XRD, CHNS analysis, BET, zeta potential measurements, UV-Vis DRS, and NMR spectroscopy. These MOFs were applied as efficient adsorbents for the removal of both cationic (Rhodamine B, Methylene Blue) and anionic (Fluorescein) dyes from aqueous solutions. Adsorption capacity was analyzed under varying pH, temperature, and dye concentrations. Isothermal models (Langmuir and Freundlich) and thermodynamic analyses were applied to understand adsorption behavior. The results show these MOFs to be promising agents for rapid and effective dye removal from contaminated water. Experimental Information regarding materials and methods and experiments can be found in ESI. Results Metal–organic frameworks (MOFs) with polymeric backbones were synthesized by first conjugating ligands to the functional groups of polyols, followed by a ligand exchange reaction with iron (III) chloride (Fig. 1 ). Using this approach, MOFs with polyvinyl alcohol (PVA) and hyperbranched polyglycerol (hPG) matrices were successfully synthesized and by various spectroscopy and microscopy methods along with thermal and elemental analyses characterized. In the IR spectrum of PVA-OMs, the intensity of the O–H absorbance band characteristic of PVA is notably reduced, indicating substitution by mesylate groups (Fig. 2 A). Additionally, sharp and intense absorbance bands observed in the range of 1100–1400 cm − 1 are attributed to the S = O stretching vibrations of the mesyl functional groups. In the spectrum of polyvinyl alcohol functionalized with 5-amino isophthalic acid (PVA-AIP), a broad O–H stretching band between 3238.26 and 3741.65 cm − 1 corresponding to the carboxyl groups of the conjugated ligands, confirmed the successful attachment of 5-amino isophthalic acid (AIP) to the PVA backbone. Further evidence of PVA-AIP formation was provided by absorbance bands at 1627.81 cm − 1 and 1552.59 cm − 1 , corresponding to aromatic C = C stretching of the benzene ring, and a band at 1398.30 cm − 1 , assigned to C = N imine stretching vibration. In the IR spectrum of PVA-MOF, the O–H absorbance band associated with acidic groups involved in coordinative bonding with Fe(III) became broadened and decreased in intensity, indicating coordination to the metal centers within the MOF structure. Furthermore, the absorbance band at 1728.10 cm − 1 , attributed to the C = O stretching of the carboxyl group in the ligand, was significantly reduced, supporting the occurrence of a ligand exchange reaction and coordination of carboxylate groups to iron(III). 26 Similar spectral changes confirmed the successful functionalization of hPG and the formation of the corresponding MOF. A decrease in the intensity of hydroxyl absorbance bands around 3357.84 cm − 1 , along with the appearance of a broad absorbance band in the range of 3100-3741.65 cm − 1 , indicated mesylation and subsequent attachment of the AIP ligand to the hPG backbone. Furthermore, a reduction in the intensity of carboxyl-related bands, as well as a decrease in the C = O absorbance bands at 1714.60 cm − 1 and 1575.73 cm − 1 , provided further evidence for the formation of hPG-MOF through coordination of the carboxylate groups to iron(III). 27 The crystallinity and long-range order of the synthesized MOFs were evaluated using X-ray diffraction (XRD). In the XRD pattern of pure PVA, a characteristic peak at 2θ = 19.5° corresponds to the (101) plane, while additional peaks at 2θ = 22.7° and 45.5° are assigned to the (200) and (111) planes, respectively. Following mesylation and subsequent conjugation of the ligand to PVA, the diffraction peaks became noticeably broader and weaker, indicating a significant increase in the amorphous character. This reduction in crystallinity suggests the formation of hydrogen bonding interactions between the PVA backbone and the amine and hydroxyl functional groups of the ligand ring. The XRD pattern of PVA-MOF exhibited peaks at 2θ = 9.66° and 18.88°, similar to those observed in MIL-101, albeit with lower intensity, indicating successful incorporation of iron into the framework (Fig. 2 C). As expected for amorphous materials, no distinct diffraction peaks were observed for hPG, hPG-OMs, or hPG-AIP. In contrast, the XRD pattern of hPG-MOF closely resembled that of PVA-MOF, also showing peaks at 2θ = 8.4° and 18.38° (Fig. 2 D). These shared features with MIL-101 confirm the presence of iron-based coordination but with predominantly amorphous structures. The lack of sharp, well-defined peaks in both PVA-MOF and hPG-MOF is consistent with their polymeric backbones, which limit the formation of long-range crystalline order. 28 , 29 The functionalization of the polymeric precursors and synthesis of multifunctional ligands with a polymeric backbone were confirmed by nuclear magnetic resonance (NMR) spectroscopy. Following mesylation, the ¹H NMR spectra of PVA-OMs and hPG-OMs showed characteristic signals at δ = (2.3) and (2.1), respectively. Corresponding ¹³C NMR spectra displayed new signals at δ = (48.6) and (45.8), providing further evidence of successful mesylation of PVA and hPG (Fig. 3 ). Substitution of mesyl groups with 2-aminoterephthalic acid (AIP) resulted in the appearance of aromatic proton signals in the range of δ = 7.9–8.4 ppm in the ¹H NMR spectra of PVA-AIP and hPG-AIP, confirming successful conjugation of AIP ligands to the polymeric backbones. Additionally, new signals observed in the ¹³C NMR spectra within the range of δ = 120–163 ppm further support the incorporation of AIP ligands via mesyl group substitution (Fig. 3 ). 30,31 The morphology of PVA-MOF and hPG-MOF in three different solvents including DMF, D 2 O, and CHCl 3 was examined using scanning electron microscopy (SEM). Both materials exhibited sheet-like structures with lateral dimensions of several micrometers and well-defined edges. The observed solvent-dependent morphological variations suggest a high degree of responsivity of the polymeric backbones to the surrounding medium. Specifically, PVA-MOF retained a flat, sheet-like morphology in DMF, while displaying partially crumpled structures in D 2 O and CHCl 3 . Conversely, hPG-MOF showed smooth, sheet-like surfaces in D 2 O and CHCl 3 but appeared crumpled in DMF. In all conditions, stacked sheets forming thick, layered frameworks were evident. These solvent-responsive morphological changes are attributed to the interplay between solvent polarity and the nature of the polymeric backbone, influencing the structural arrangement through specific solvent–polymer interactions (Figs. 4 a- 4 l). 32 , 33 The composition and elemental distribution of the materials were analyzed using energy-dispersive X-ray spectroscopy (EDX) (Figs. 4 m and 4 n). The spectra of PVA and hPG showed the presence of carbon and oxygen, consistent with their polymeric structures. In PVA-OMs and hPG-OMs, the appearance of sulfur peaks confirmed successful mesylation of the original polymers. Following functionalization with 5-amino isophthalic acid (AIP), nitrogen was detected in PVA-AIP and hPG-AIP, while sulfur content decreased, indicating successful conjugation of AIP to the polymer backbones. In PVA-MOF and hPG-MOF, the presence of iron, along with nitrogen, carbon, and oxygen, confirmed the formation of coordination bonds between the acidic functional groups of the ligands and Fe(III), consistent with MOF formation. Moreover, the composition of the synthesized materials was further confirmed by elemental analysis, and the results were consistent with the EDX data (Table S1 ). The optical properties of the MOFs were investigated using UV-Vis spectroscopy. Both PVA-MOF and hPG-MOF exhibited broad absorption in the range of 270–670 nm, indicating a high density of metal–ligand interactions and the presence of aromatic rings within their structures (Figs. 5 a and 5 b and S1). This broad absorption is advantageous, as it suggests potential for photocatalytic applications such as reactive oxygen species (ROS) generation, although such activity is beyond the scope of the present study. 34 , 35 The aim of this study was to evaluate the ability of the synthesized MOF frameworks to remove dye pollutants from aqueous solutions. To this end, the surface charge of the MOFs was investigated at various pH values, as it is a key factor influencing their adsorption performance. Due to the presence of carboxyl functional groups, the MOFs exhibited a highly negative surface charge under neutral and basic conditions, which shifted to a positive charge in acidic environments. This behavior is attributed to the pH-dependent protonation states of the functional groups: under basic and neutral conditions, carboxyl groups are deprotonated to carboxylates, conferring a negative charge, whereas in acidic conditions, carboxyl groups become protonated and amine groups are converted to their positively charged ammonium form (Figs. 5 c and 5 d). 36 , 37 The porous structures of the synthesized PVA-MOF and hPG-MOF were characterized by nitrogen adsorption–desorption isotherms measured at 77 K and 81 kPa, corresponding to the saturation pressure of nitrogen at this temperature. The resulting isotherms are presented in Fig. 6 and summarized in Table S2. Both materials exhibited type IV isotherms, according to the IUPAC classification based on Brunauer et al., indicative of mesoporous structures with uniform pore distributions. PVA-MOF and hPG-MOF showed total pore volumes of 0.048105 cm³.g − 1 and 0.051623 cm³.g − 1 , respectively. The specific surface areas, calculated using the Brunauer–Emmett–Teller (BET) method, were approximately 15.509 m².g − 1 for PVA-MOF and 18.609 m².g − 1 for hPG-MOF. The Barrett–Joyner–Halenda (BJH) analysis revealed average pore diameters of 11.8 nm for PVA-MOF and 11.2 nm for hPG-MOF, with pore size distributions ranging from 2 to 50 nm (Figs. 5 e- 5 h). The measured specific surface areas were lower than expected, likely due to the collapse of the polymeric backbone in the dry state during nitrogen physisorption analysis. In the solution state, the polymeric network is expected to swell, maintaining a more open structure that would result in significantly higher accessible surface areas. 38 The discharge of organic dyes such as Methylene Blue (MB), Rhodamine B (RhB), and Fluorescein (FL) into water bodies poses significant environmental and health hazards due to their toxic and non-biodegradable nature. Therefore, developing efficient adsorbents for dye removal is of great importance. 39 MOF–polymer composites combine the high surface area and porosity of MOFs with the chemical functionality and flexibility of polymers, resulting in materials with excellent adsorption capabilities for various dye molecules.In this study, 1 mg of the synthesized PVA-MOF or hPG-MOF was dispersed in 5 mL of dye solution (50 ppm) and subjected to sonication followed by stirring for 24 hours at 25°C. As shown in Fig. 4 , both adsorbents exhibited high adsorption capacities toward all three tested dyes. These results highlight the strong potential of PVA-MOF and hPG-MOF composites for efficient dye removal in aqueous environments. The maximum adsorption capacities of PVA-MOF for the cationic dyes rhodamine B (Rh B) and methylene blue (MB), as well as the anionic dye fluorescein (FL), were 128.17 mg.g − 1 , 128.24 mg.g − 1 , and 124.77 mg.g − 1 , respectively. Under the same conditions, hPG-MOF exhibited adsorption capacities of 131.46 mg.g − 1 for Rh B, 135.34 mg.g − 1 for MB, and 128.31 mg.g − 1 for FL (Table S3). While PVA-MOF showed superior performance in the removal of the anionic dye, hPG-MOF demonstrated significantly higher adsorption capacities for cationic dyes compared to its linear counterpart. Interestingly, both MOFs were able to adsorb the anionic FL dye effectively, despite their negatively charged surfaces under neutral and basic conditions. This observation suggests that electrostatic interactions are not the sole driving force governing dye adsorption; other mechanisms, such as π–π stacking, hydrogen bonding, and coordination interactions, may also play a significant role. Discussion Table S3 presents a comparison of the adsorption capacities of the synthesized MOFs with those of similar materials reported in the literature. Despite having fewer aromatic ligands and lower metal content-due to the nature of their polymeric backbones-both PVA-MOF and hPG-MOF exhibit excellent performance in dye pollutant removal. The use of PVA and hPG as the primary structural components not only contributes to high adsorption efficiency but also enhances the biocompatibility of the materials. Moreover, this design minimizes the risk of leaching toxic aromatic ligands into aqueous environments, making these MOFs promising candidates for environmentally friendly water purification applications. To elucidate the adsorption mechanisms of the dyes, the rate constants for both the pseudo-first-order and pseudo-second-order kinetic models were examined for each dye (see Tables S4). The adsorption behavior at various concentrations followed the pseudo-second-order kinetic model more closely, as evidenced by the better fit of the kinetic data with this model, as shown in Fig. 7 . The adsorption kinetics of Methylene Blue (MB), Rhodamine B (Rh B), and Fluorescein (FL) on the synthesized MOFs were best described by the pseudo-second-order kinetic model. The calculated parameters showed excellent agreement with the experimental data, indicating that the adsorption process is predominantly governed by chemisorption involving valence forces through electron sharing or exchange between the dye molecules and the adsorbent surface (Fig. 7 and Figure S6). To evaluate the adsorption isotherms, both Langmuir and Freundlich models were applied. The Langmuir model yielded higher correlation coefficients (R 2 ) for all three dyes, FL, MB, and Rh B, suggesting monolayer adsorption on a homogeneous surface (Figure S3). The maximum adsorption capacities predicted by the Langmuir model are presented in Table S6. The adsorption process is likely driven by a combination of electrostatic interactions, π–π stacking, and hydrogen bonding. The presence of carboxyl and amino functional groups within the polymeric framework enhances these interactions, facilitating strong binding between the dye molecules and the MOF surface. According to the Langmuir isotherm model, dye molecules are uniformly adsorbed within the cavities of the MOFs with polymeric matrices, indicating a homogeneous adsorption surface. This uniform adsorption behavior suggests that the PVA-MOF and hPG-MOF possess a structurally consistent and well-defined scaffold. The calculated maximum adsorption capacities for Fluorescein, Methylene Blue (MB), and Rhodamine B (Rh B), based on the Langmuir equation, are summarized in Table S7. Thermodynamic parameters provide deeper insights into the mechanisms of dye adsorption (see Figure S4 and Table S5). Thermodynamic analyses confirmed that the adsorption process is endothermic, becoming more favorable with increasing temperature and accompanied by an increase in disorder. For cationic dyes (such as Rhodamine B and Methylene Blue), the adsorption is non-spontaneous, whereas for the anionic dye (such as Fluorescein), the process is spontaneous (see Fig. 8 and Table S8). The interactions between the dyes and the adsorbents are primarily driven by electrostatic forces and hydrogen bonding, both of which are endothermic. The rise in entropy during the adsorption of the dyes may be attributed to the dispersion and aggregation of dye molecules post-interaction with the MOFs, leading to increased disorder within the system. The pH parameter is of critical importance in adsorption studies. The adsorption of MB, RhB, and FL was investigated over a pH range of 2 to 10 (Fig. 9 a and 9 b). The initial dye solution had a pH approximately equal to 7. Acidic and alkaline conditions were adjusted by adding volumes of 0.1 M HCl and 0.1 M NaOH, respectively. The findings indicated that both removal efficiency and adsorption capacity reach their maximum around pH 10 for Rh B and MB and decline at higher pH values. In basic mediums MB and Rh B are not positively charged, therefore electrostatic interaction with the negatively charged MOFs is not a driving force. On the other side FL was considerably adsorbed by hPG-MOF in basic medium while both dye and MOF are negatively charged. One possible explanation for the observed pH-dependent adsorption behavior is that, at higher pH values, the carboxyl groups of the AIP ligand become deprotonated, resulting in increased negative surface charge within the MOF pores. This electrostatic repulsion among negatively charged sites may lead to pore expansion or enhanced accessibility. As a result, the adsorption capacity increases, primarily through hydrogen bonding and π–π interactions rather than electrostatic attraction. Adsorption of FL by PVA-MOF was not significant in basic pH, indicating a major role for the electrostatic repulsion in the case. Given that, in real environmental matrices such as municipal water, other elements coexist simultaneously, it is essential to evaluate the adsorption performance of the selected adsorbents under actual conditions. To this end, removal efficiency and adsorption capacity were assessed using samples of municipal water, Khoramrood River water, and Stone Stormwater, each containing dye concentrations of 50 ppm. Samples of each water source were analyzed prior to treatment to determine their initial dye concentrations. Subsequently, 1mg of the adsorbent was added to each solution, and the mixtures were stirred for a predetermined period. The residual dye concentrations were measured at specific time intervals to evaluate the adsorption kinetics. The removal efficiency and adsorption capacity were then calculated based on the initial and final dye concentrations. The results are summarized in tables S9. The results of the experiment with D 2 O showed that both MOF adsorbents performed well in the adsorption of dyes. The adsorption capacity data showed distinct patterns for each dye: methylene blue showed the highest adsorption efficiency (128.24–135.34), followed by rhodamine B (128.17–131.46), while fluorescein showed the lowest adsorption capacity (124.77–128.31). The results showed that hPG-MOF consistently outperformed PVA-MOF in all types of dyes, with the most pronounced difference observed in the adsorption of methylene blue. These results were also confirmed in subsequent experiments with real waters (rock storm water, river water, and drinking water), indicating that both adsorbents also perform well in real environmental conditions. The stability and reusability of the adsorbents are essential for their practical application in dye removal from aqueous media. To assess these properties, 1 mg of each MOF was employed to adsorb dyes (10 mg.L⁻¹) from aqueous solutions. In the first cycle, both PVA-MOF and hPG-MOF demonstrated near-complete dye removal. After each cycle, the adsorbents were regenerated by washing with acetone to desorb the dye molecules, followed by drying at 70°C before reuse. As shown in Fig. 9 c, the removal efficiency of both MOFs remained nearly constant over three consecutive adsorption–desorption cycles, confirming their excellent stability and reusability. The combination of high adsorption capacity, favorable kinetic behavior, and straightforward regeneration underscores the strong potential of these MOF–polymer composites for industrial-scale dye removal and wastewater treatment applications. Conclusions In this study, metal-organic frameworks (MOFs) incorporating polymeric backbones were successfully synthesized through ligand conjugation to linear and hyperbranched polyols, followed by ligand exchange with iron (III) chloride. The resulting materials exhibited efficient removal of both cationic and anionic dyes from aqueous solutions, with adsorption performance showing strong pH dependency. Maximum dye uptake occurred under alkaline conditions, where the frameworks' pores were in an open state, enhancing adsorption capacity. These results underscore the potential of polymer-integrated MOFs as effective and responsive materials for environmental remediation. Furthermore, this work paves the way for the development of a new class of functional MOFs with polymeric matrices, offering promising applications in catalysis, water treatment, and advanced separation processes. Methods Synthesis of mesylated polyvinyl alcohol (PVA-OMs) Initially, polyvinyl alcohol (PVA) (0.2 gr,0.0028 mmol) was added to a round-bottom flask along with the solvent dimethylformamide (DMF) (10 mL) and heated to 110°C until fully dissolved. The solution was then cooled to room temperature, and trimethylamine (Et 3 N) (1 mL) was added at room temperature and stirred for 2 hours. The resulting solution was placed in an ice bath, and methanesulfonyl chloride (MsCl) (1.78 mL,23mmol) was gradually added over the course of one hour. The mixture was then stirred at room temperature for 3 days. Product was crystalized in acetonitrile and used for further experiments The overall reaction yield was approximately 69.70%. Conjugation of 5-amino isophthalic acid (AIP) to polyvinyl alcohol (PVA-AIP) Mesylated polyvinyl alcohol (PVA-Oms) (0.1 gr, 0.000736 mmol) was dissolved in acetonitrile (25 ml), after which potassium carbonate (k 2 CO 3 ) (0.1 gr ,0.724 mmol) and 5-amino isophthalic acid (AIP) (0.11 gr ,0.6 mmol) were added. The mixture was refluxed at 80°C for 24 hours. The final product was purified using a dialysis bag in dimethylformamide (DMF), distilled water (D 2 O), and ethanol (EtOH), and it was dried in a vacuum oven at 50°C.The overall reaction yield was approximately 84.04%. Synthesis of PVA-MOF PVA-AIP and hexahydrate iron (III) chloride were mixed in a 2:1 ratio in a beaker, and the solvent dimethylformamide (DMF) (25 mL) was added. The resulting mixture was stirred for 2 hours and then placed in an autoclave, where it was heated to 110°C for 20 hours. The final product was purified by washing with dimethylformamide (DMF) and ethanol and was then dried in a vacuum oven at 50°C.The overall reaction yield was approximately 70.39%. Synthesis of mesylated hyperbranched polyglycerol (hPG-OMs) Hyperbranched polyglycerol (hPG) (Mn = 5000), (0.258 gr, 0.0516 mmol) was dissolved in a polymerization ampoule under an inert gas atmosphere (nitrogen) in dimethylformamide (DMF) (10 mL), and subsequently, triethylamine (Et 3 N) (1 mL) was added while maintaining the temperature at 0°C. Msyl chloride (MsCl) (1.74 mL, 22.47 mmol), was gradually added over the course of 1 hour. After the addition of mesyl chloride, the mixture was refluxed in a nitrogen atmosphere at room temperature for 24 hours. The crude product was purified using a dialysis bag in acetonitrile.The overall reaction yield was approximately 78.66%. Conjugation of 5-Amino isophthalic acid (AIP) to mesylated hyperbranched Polyglycerol (hPG-AIP) Mesylated hyperbranched polyglycerol (hPG-Oms) (0.1 gr, 0.0156 mmol) was dissolved in acetonitrile (25 mL), after which potassium carbonate (k 2 CO 3 ) (0.1 gr, 0.724 mmol) and 5-amino isophthalic acid (AIP) (0.234 gr, 1.29 mmol) were added. The mixture was stirred at 80°C for 24 hours. The final product was purified using a dialysis bag in dimethylformamide (DMF), distilled water (D 2 O), and ethanol (EtOH), and it was dried in a vacuum oven at 50°C.The overall reaction yield was approximately 83.66%. Synthesis of hPG-MOF The synthesis method for this compound is similar to that of PVA-MOF. Dye removal A stock solution of methylene blue, rhodamine B, and fluorescein was prepared by dissolving 100 mg.L − 1 of these dyes in water. Subsequently, standard solutions were prepared by diluting the stock solution for testing. For adsorption experiments, 3 mg of PVA-MOF and hPG-MOF was added to 5 mL of color solutions at concentrations of 20 ppm, 10 ppm, and 5 ppm (Rhodamine B, Methylene Blue, and Fluorescein) and incubated for 24 hours under ambient conditions (25°C) without agitation. After 24 hours, it was observed that the adsorbent could significantly absorb cationic dyes (Rhodamine B, Methylene Blue) and, to a lesser extent, the anionic dye (Fluorescein). Using a spectrophotometer, the absorbance of all samples at the corresponding λmax for each dye was obtained and compared with the standard curve. The dye adsorption capacity qt (mg. g − 1 ) and the percentage removal of dye (%R) by the adsorbent at each time point were calculated. Our aim was to investigate the adsorption of cationic and anionic dyes, which are among the most significant water pollutants. Data availability The datasets used and/or analysed during the current study available from the corresponding author on reasonable request. Declarations Acknowledgements We would like to thank Core Facility of Lorestan University for the analysis of the synthesized materials. Author contributions S.G performed the relevant synthesis and analyses, also wrote the first manuscript. M.A conceptualized the projects and edited the manuscript. M. N helped with the formal analysis. Competing interests The authors declare that they have no competing interests. Funding Declaration The research described in this manuscript didn’t support by funding. References Kordbacheh, F. & Heidari, G. Water pollutants and approaches for their removal. Mater. Chem. Horizons . 2 (2), 139–153 (2023). Rahman, N. A. A. A., Khasri, A., Ahmad, A. A., Jamir, M. R. M. & Yasin, N. H. M. Preparation of AC/TiO2 doped N-Ce Synthesized via Microwave Irradiation for Amoxicillin Photodegradation. Int. J. Integr. Eng. 16 (2), 237–244 (2024). Essifi, K. et al. 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14:12:37","extension":"html","order_by":31,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":111667,"visible":true,"origin":"","legend":"","description":"","filename":"earlyproof.html","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/fa71ede569f07701610d2389.html"},{"id":96852333,"identity":"c7f4a407-c97c-4902-9bd0-aa9789f92f41","added_by":"auto","created_at":"2025-11-26 17:57:40","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":371654,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic illustration of the synthesis of PVA-MOF and hPG-MOF. Following mesylation of PVA and hPG, the polymers were functionalized with 5-amino isophthalic acid (AIP), and subsequently subjected to a ligand exchange reaction with iron(III) chloride to yield the corresponding MOFs.\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/4f0614ac446574c2edd4330f.png"},{"id":96852332,"identity":"fd117ad7-6d13-42d9-9a20-7dc88bfa2a0d","added_by":"auto","created_at":"2025-11-26 17:57:40","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":204348,"visible":true,"origin":"","legend":"\u003cp\u003eIR spectra of PVA-MOF (A) and hPG-MOF (B) and their precursors. XRD diffractograms of PVA-MOF (C) and hPG-MOF (D) and their precursors.\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/9068ba7896ce982e1bc341c6.png"},{"id":96852334,"identity":"f913885a-9be9-40e1-86f3-35dbd4d78eab","added_by":"auto","created_at":"2025-11-26 17:57:40","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":273208,"visible":true,"origin":"","legend":"\u003cp\u003eThe successful functionalization of PVA and hPG was confirmed by ¹H and ¹³C NMR spectroscopy. The NMR spectra provided clear evidence for the conjugation of AIP ligands to the polymeric backbones, enabling the formation of multifunctional platforms suitable for MOF construction.\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/dd1b32eaa7c80e0bf8cb61d3.png"},{"id":96918978,"identity":"db31fcf7-424f-4cad-a14d-6dc42ea4a218","added_by":"auto","created_at":"2025-11-27 14:12:56","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":496091,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of PVA-MOF in DMF (a,b), distilled water (c,d) and chloroform (e,f). SEM images of hPG-MOF in DMF (g,h), distilled water (i,j), and chloroform (k,l). EDX elemental mapping and distribution for PVA-MOF (m) and hPG-MOF (n).\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/2b00ee3393dc8068f1729ad0.png"},{"id":96852338,"identity":"5392c1e6-1b9b-4954-84fa-9137028e31c6","added_by":"auto","created_at":"2025-11-26 17:57:40","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":184595,"visible":true,"origin":"","legend":"\u003cp\u003eUV-Vis absorption spectra of PVA-MOF (a) and hPG (b) and the related precursors ligand. Zeta potential values of PVA-MOF (c) and hPG-MOF (d) under acidic, neutral and basic conditions. N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherm (V vs. P/P\u003csub\u003e0\u003c/sub\u003e) of PVA-MOF(e) and hPG-MOF(g). Pore size distribution curve (dV/dRp vs. Rp) of PVA-MOF(f) \u0026nbsp;and hPG-MOF(h).\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/d15336c23a1e0b58b466c89c.png"},{"id":96852336,"identity":"98247e5c-0a36-4aee-b75c-dd5dff84a33c","added_by":"auto","created_at":"2025-11-26 17:57:40","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":151047,"visible":true,"origin":"","legend":"\u003cp\u003eDigital photographs of PVA-MOF (a) and hPG-MOF (b) before and after incubation with different dye solutions (50 ppm, 5 mL). The MOFs were incubated with the dyes for 24 hours at room temperature.\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/f3903a030e78bf2049cc0740.png"},{"id":96852341,"identity":"a34c16dd-d8e3-4810-a4dd-99f3f2804596","added_by":"auto","created_at":"2025-11-26 17:57:40","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":116752,"visible":true,"origin":"","legend":"\u003cp\u003ePseudo-second-order kinetic model describing the adsorption of Methylene Blue (MB), Rhodamine B (Rh B), and Fluorescein (FL) onto PVA-MOF and hPG-MOF. The strong correlation between experimental data and the model suggests that chemisorption is the dominant mechanism governing dye uptake. All experiments were performed under constant shaking conditions to assess the adsorption kinetics and capacities of the composites for the selected dyes.\u003c/p\u003e","description":"","filename":"7.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/7a66111015f48ac720bcf7fa.png"},{"id":96919313,"identity":"d241ed10-a952-4cac-954d-f70b16f4cb37","added_by":"auto","created_at":"2025-11-27 14:13:34","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":87322,"visible":true,"origin":"","legend":"\u003cp\u003ePercentage dye removal efficiency (%R) and adsorption capacity (q\u003csub\u003et\u003c/sub\u003e) of PVA-MOF and hPG-MOF for Methylene Blue (MB), Rhodamine B (Rh B), and Fluorescein (FL) at various temperatures. Dye solutions (10 mg.L⁻¹) were treated with each composite under shaking conditions, and dye removal was quantified using UV-Vis spectroscopy. Both composites demonstrated improved adsorption performance with increasing temperature, highlighting their potential for thermally responsive dye removal applications.\u003c/p\u003e","description":"","filename":"8.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/3145dc7d7bee306a9ed4708c.png"},{"id":96918032,"identity":"3fb6ec0d-80fd-4558-8038-ab872b5dd901","added_by":"auto","created_at":"2025-11-27 14:11:02","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":54886,"visible":true,"origin":"","legend":"\u003cp\u003e(a) The adsorption capacities of PVA-MOF at various pH levels, demonstrating a strong correlation between pH and adsorption efficiency.(b) The adsorption capacities of hPG-MOF across different pH values, highlighting the influence of pH on the adsorption performance.(c) Recyclability assessment of the synthesized MOFs for dye removal, including three consecutive adsorption-desorption cycles. The results indicate the stability and reusability of the materials over multiple cycles.\u003c/p\u003e","description":"","filename":"9.png","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/dc6d1447af5f56a652688036.png"},{"id":96923294,"identity":"79b5f790-309b-4793-afda-6e4115309c4b","added_by":"auto","created_at":"2025-11-27 14:21:24","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2399911,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/1aa40601-e63f-416a-bede-b9e475a9eedc.pdf"},{"id":96919753,"identity":"c5ec294c-08c0-4c5e-bc4a-565e88f19177","added_by":"auto","created_at":"2025-11-27 14:14:25","extension":"docx","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":963748,"visible":true,"origin":"","legend":"","description":"","filename":"ESI.docx","url":"https://assets-eu.researchsquare.com/files/rs-8050532/v1/f79ec4c7b0d6c940f6a17082.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Metal-Organic Frameworks with Linear and Branched Polyol Backbones for Dye Removal","fulltext":[{"header":"Introduction","content":"\u003cp\u003eThe rapid technological advancements of recent decades have raised significant environmental concerns, particularly regarding water pollution. As the most vital resource for life, protecting water bodies from contamination driven by population growth, urbanization, and industrialization is a global priority shared by governments and citizens alike.\u003csup\u003e\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u003c/sup\u003e In recent years, water quality has declined due to pollutants such as pharmaceuticals, personal care products, and especially organic dyes released by the textile, paper, food, cosmetics, and pharmaceutical industries.\u003csup\u003e\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e\u003c/sup\u003e These colored effluents pose severe health risks, including skin irritation, allergic reactions, organ dysfunction, and even cancer, particularly when absorbed through the skin or ingested.\u003csup\u003e\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eAs a result, significant efforts have been made to remove such dyes using techniques like ion exchange, coagulation, flocculation, and adsorption.\u003csup\u003e\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e\u003c/sup\u003e Adsorption, in particular, has garnered attention due to its efficiency and simplicity. It involves the adhesion of atoms, ions, or molecules (adsorbates) to the surface of a solid (adsorbent), particularly within its internal porous structure, which significantly enhances the surface area.\u003csup\u003e\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e\u003c/sup\u003e In this context, polymer-based metal-organic frameworks (MOFs) have emerged as promising adsorbents due to their tunable porosity and functional versatility.\u003csup\u003e\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eMOFs are crystalline, porous materials composed of metal ions or clusters coordinated to organic ligands. Their applications span catalysis, gas separation, drug delivery, and adsorption\u003csup\u003e\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e,\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e\u003c/sup\u003e Among them, MIL-101 stands out for its mesoporous nature, large pore size, and chemical stability, particularly in organic solvents at room temperature.\u003csup\u003e\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003ePolymers are increasingly integrated with MOFs to create composite materials that are lightweight, cost-effective, and mechanically robust.\u003csup\u003e\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e\u003c/sup\u003e Research into MOF-polymer composites has evolved significantly since the early 2000s, with growing applications in sensing, separation, and environmental remediation.\u003csup\u003e\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003ePVA is a hydrophilic, semi-crystalline synthetic biopolymer known for its biodegradability, thermal stability, and strong film-forming and chemical resistance properties.\u003csup\u003e\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e\u003c/sup\u003e Its hydroxyl-rich structure facilitates strong hydrogen bonding, contributing to its semi-crystalline nature and compatibility with other materials.\u003csup\u003e\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e\u003c/sup\u003e Widely used in textiles, adhesives, medical products, and water treatment,\u003csup\u003e14,18\u003c/sup\u003e PVA does have limitations in mechanical strength and solvent resistance. These can be mitigated through cross-linking strategies, which enhance its network structure, reduce hydrophilicity, and improve its suitability for dye and heavy metal adsorption.\u003csup\u003e\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eHyperbranched polyglycerols (hPGs), on the other hand, offer another compelling polymer due to their biocompatibility, low toxicity, and simple one-step synthesis.\u003csup\u003e\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e\u003c/sup\u003e These highly branched, water-soluble polymers are under active investigation for pharmaceutical and biomedical applications, such as drug delivery and tissue engineering.\u003csup\u003e\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e\u003c/sup\u003e Their molecular weight and mechanical properties can be tuned via synthesis conditions, making them highly adaptable.\u003csup\u003e\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e,\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eCombining MOFs with branched polyglycerol polymers results in porous hybrid materials that exhibit high surface area, tunable properties, and potential for use in environmental, energy, and biomedical fields. \u003csup\u003e24,25\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eIn this study, stable PVA-MOF and hPG-MOF composites were synthesized and thoroughly characterized using techniques such as TGA, FTIR, SEM, EDX, XRD, CHNS analysis, BET, zeta potential measurements, UV-Vis DRS, and NMR spectroscopy. These MOFs were applied as efficient adsorbents for the removal of both cationic (Rhodamine B, Methylene Blue) and anionic (Fluorescein) dyes from aqueous solutions. Adsorption capacity was analyzed under varying pH, temperature, and dye concentrations. Isothermal models (Langmuir and Freundlich) and thermodynamic analyses were applied to understand adsorption behavior. The results show these MOFs to be promising agents for rapid and effective dye removal from contaminated water.\u003c/p\u003e\n\u003ch3\u003eExperimental\u003c/h3\u003e\n\u003cp\u003eInformation regarding materials and methods and experiments can be found in ESI.\u003c/p\u003e"},{"header":"Results","content":"\u003cp\u003eMetal\u0026ndash;organic frameworks (MOFs) with polymeric backbones were synthesized by first conjugating ligands to the functional groups of polyols, followed by a ligand exchange reaction with iron (III) chloride (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). Using this approach, MOFs with polyvinyl alcohol (PVA) and hyperbranched polyglycerol (hPG) matrices were successfully synthesized and by various spectroscopy and microscopy methods along with thermal and elemental analyses characterized.\u003c/p\u003e\u003cp\u003eIn the IR spectrum of PVA-OMs, the intensity of the O\u0026ndash;H absorbance band characteristic of PVA is notably reduced, indicating substitution by mesylate groups (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eA). Additionally, sharp and intense absorbance bands observed in the range of 1100\u0026ndash;1400 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e are attributed to the S\u0026thinsp;=\u0026thinsp;O stretching vibrations of the mesyl functional groups.\u003c/p\u003e\u003cp\u003eIn the spectrum of polyvinyl alcohol functionalized with 5-amino isophthalic acid (PVA-AIP), a broad O\u0026ndash;H stretching band between 3238.26 and 3741.65 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e corresponding to the carboxyl groups of the conjugated ligands, confirmed the successful attachment of 5-amino isophthalic acid (AIP) to the PVA backbone. Further evidence of PVA-AIP formation was provided by absorbance bands at 1627.81 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 1552.59 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, corresponding to aromatic C\u0026thinsp;=\u0026thinsp;C stretching of the benzene ring, and a band at 1398.30 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, assigned to C\u0026thinsp;=\u0026thinsp;N imine stretching vibration.\u003c/p\u003e\u003cp\u003eIn the IR spectrum of PVA-MOF, the O\u0026ndash;H absorbance band associated with acidic groups involved in coordinative bonding with Fe(III) became broadened and decreased in intensity, indicating coordination to the metal centers within the MOF structure. Furthermore, the absorbance band at 1728.10 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, attributed to the C\u0026thinsp;=\u0026thinsp;O stretching of the carboxyl group in the ligand, was significantly reduced, supporting the occurrence of a ligand exchange reaction and coordination of carboxylate groups to iron(III).\u003csup\u003e\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eSimilar spectral changes confirmed the successful functionalization of hPG and the formation of the corresponding MOF. A decrease in the intensity of hydroxyl absorbance bands around 3357.84 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, along with the appearance of a broad absorbance band in the range of 3100-3741.65 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, indicated mesylation and subsequent attachment of the AIP ligand to the hPG backbone. Furthermore, a reduction in the intensity of carboxyl-related bands, as well as a decrease in the C\u0026thinsp;=\u0026thinsp;O absorbance bands at 1714.60 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 1575.73 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, provided further evidence for the formation of hPG-MOF through coordination of the carboxylate groups to iron(III).\u003csup\u003e\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eThe crystallinity and long-range order of the synthesized MOFs were evaluated using X-ray diffraction (XRD). In the XRD pattern of pure PVA, a characteristic peak at 2θ\u0026thinsp;=\u0026thinsp;19.5\u0026deg; corresponds to the (101) plane, while additional peaks at 2θ\u0026thinsp;=\u0026thinsp;22.7\u0026deg; and 45.5\u0026deg; are assigned to the (200) and (111) planes, respectively. Following mesylation and subsequent conjugation of the ligand to PVA, the diffraction peaks became noticeably broader and weaker, indicating a significant increase in the amorphous character. This reduction in crystallinity suggests the formation of hydrogen bonding interactions between the PVA backbone and the amine and hydroxyl functional groups of the ligand ring.\u003c/p\u003e\u003cp\u003eThe XRD pattern of PVA-MOF exhibited peaks at 2θ\u0026thinsp;=\u0026thinsp;9.66\u0026deg; and 18.88\u0026deg;, similar to those observed in MIL-101, albeit with lower intensity, indicating successful incorporation of iron into the framework (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eC). As expected for amorphous materials, no distinct diffraction peaks were observed for hPG, hPG-OMs, or hPG-AIP. In contrast, the XRD pattern of hPG-MOF closely resembled that of PVA-MOF, also showing peaks at 2θ\u0026thinsp;=\u0026thinsp;8.4\u0026deg; and 18.38\u0026deg; (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eD). These shared features with MIL-101 confirm the presence of iron-based coordination but with predominantly amorphous structures. The lack of sharp, well-defined peaks in both PVA-MOF and hPG-MOF is consistent with their polymeric backbones, which limit the formation of long-range crystalline order.\u003csup\u003e\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e,\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe functionalization of the polymeric precursors and synthesis of multifunctional ligands with a polymeric backbone were confirmed by nuclear magnetic resonance (NMR) spectroscopy.\u003c/p\u003e\u003cp\u003eFollowing mesylation, the \u0026sup1;H NMR spectra of PVA-OMs and hPG-OMs showed characteristic signals at δ = (2.3) and (2.1), respectively. Corresponding \u0026sup1;\u0026sup3;C NMR spectra displayed new signals at δ = (48.6) and (45.8), providing further evidence of successful mesylation of PVA and hPG (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e). Substitution of mesyl groups with 2-aminoterephthalic acid (AIP) resulted in the appearance of aromatic proton signals in the range of δ\u0026thinsp;=\u0026thinsp;7.9\u0026ndash;8.4 ppm in the \u0026sup1;H NMR spectra of PVA-AIP and hPG-AIP, confirming successful conjugation of AIP ligands to the polymeric backbones. Additionally, new signals observed in the \u0026sup1;\u0026sup3;C NMR spectra within the range of δ\u0026thinsp;=\u0026thinsp;120\u0026ndash;163 ppm further support the incorporation of AIP ligands via mesyl group substitution (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e). \u003csup\u003e30,31\u003c/sup\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe morphology of PVA-MOF and hPG-MOF in three different solvents including DMF, D\u003csub\u003e2\u003c/sub\u003eO, and CHCl\u003csub\u003e3\u003c/sub\u003e was examined using scanning electron microscopy (SEM). Both materials exhibited sheet-like structures with lateral dimensions of several micrometers and well-defined edges. The observed solvent-dependent morphological variations suggest a high degree of responsivity of the polymeric backbones to the surrounding medium. Specifically, PVA-MOF retained a flat, sheet-like morphology in DMF, while displaying partially crumpled structures in D\u003csub\u003e2\u003c/sub\u003eO and CHCl\u003csub\u003e3\u003c/sub\u003e. Conversely, hPG-MOF showed smooth, sheet-like surfaces in D\u003csub\u003e2\u003c/sub\u003eO and CHCl\u003csub\u003e3\u003c/sub\u003e but appeared crumpled in DMF. In all conditions, stacked sheets forming thick, layered frameworks were evident. These solvent-responsive morphological changes are attributed to the interplay between solvent polarity and the nature of the polymeric backbone, influencing the structural arrangement through specific solvent\u0026ndash;polymer interactions (Figs.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea-\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003el).\u003csup\u003e\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e,\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eThe composition and elemental distribution of the materials were analyzed using energy-dispersive X-ray spectroscopy (EDX) (Figs.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003em and \u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003en). The spectra of PVA and hPG showed the presence of carbon and oxygen, consistent with their polymeric structures. In PVA-OMs and hPG-OMs, the appearance of sulfur peaks confirmed successful mesylation of the original polymers. Following functionalization with 5-amino isophthalic acid (AIP), nitrogen was detected in PVA-AIP and hPG-AIP, while sulfur content decreased, indicating successful conjugation of AIP to the polymer backbones. In PVA-MOF and hPG-MOF, the presence of iron, along with nitrogen, carbon, and oxygen, confirmed the formation of coordination bonds between the acidic functional groups of the ligands and Fe(III), consistent with MOF formation. Moreover, the composition of the synthesized materials was further confirmed by elemental analysis, and the results were consistent with the EDX data (Table \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e).\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe optical properties of the MOFs were investigated using UV-Vis spectroscopy. Both PVA-MOF and hPG-MOF exhibited broad absorption in the range of 270\u0026ndash;670 nm, indicating a high density of metal\u0026ndash;ligand interactions and the presence of aromatic rings within their structures (Figs.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea and \u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb and S1). This broad absorption is advantageous, as it suggests potential for photocatalytic applications such as reactive oxygen species (ROS) generation, although such activity is beyond the scope of the present study.\u003csup\u003e\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e,\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eThe aim of this study was to evaluate the ability of the synthesized MOF frameworks to remove dye pollutants from aqueous solutions. To this end, the surface charge of the MOFs was investigated at various pH values, as it is a key factor influencing their adsorption performance. Due to the presence of carboxyl functional groups, the MOFs exhibited a highly negative surface charge under neutral and basic conditions, which shifted to a positive charge in acidic environments. This behavior is attributed to the pH-dependent protonation states of the functional groups: under basic and neutral conditions, carboxyl groups are deprotonated to carboxylates, conferring a negative charge, whereas in acidic conditions, carboxyl groups become protonated and amine groups are converted to their positively charged ammonium form (Figs.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ec and \u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ed).\u003csup\u003e\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e,\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eThe porous structures of the synthesized PVA-MOF and hPG-MOF were characterized by nitrogen adsorption\u0026ndash;desorption isotherms measured at 77 K and 81 kPa, corresponding to the saturation pressure of nitrogen at this temperature. The resulting isotherms are presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e and summarized in Table S2. Both materials exhibited type IV isotherms, according to the IUPAC classification based on Brunauer et al., indicative of mesoporous structures with uniform pore distributions.\u003c/p\u003e\u003cp\u003ePVA-MOF and hPG-MOF showed total pore volumes of 0.048105 cm\u0026sup3;.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 0.051623 cm\u0026sup3;.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, respectively. The specific surface areas, calculated using the Brunauer\u0026ndash;Emmett\u0026ndash;Teller (BET) method, were approximately 15.509 m\u0026sup2;.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for PVA-MOF and 18.609 m\u0026sup2;.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for hPG-MOF. The Barrett\u0026ndash;Joyner\u0026ndash;Halenda (BJH) analysis revealed average pore diameters of 11.8 nm for PVA-MOF and 11.2 nm for hPG-MOF, with pore size distributions ranging from 2 to 50 nm (Figs.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ee-\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eh). The measured specific surface areas were lower than expected, likely due to the collapse of the polymeric backbone in the dry state during nitrogen physisorption analysis. In the solution state, the polymeric network is expected to swell, maintaining a more open structure that would result in significantly higher accessible surface areas.\u003csup\u003e\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe discharge of organic dyes such as Methylene Blue (MB), Rhodamine B (RhB), and Fluorescein (FL) into water bodies poses significant environmental and health hazards due to their toxic and non-biodegradable nature. Therefore, developing efficient adsorbents for dye removal is of great importance.\u003csup\u003e\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\u003cp\u003eMOF\u0026ndash;polymer composites combine the high surface area and porosity of MOFs with the chemical functionality and flexibility of polymers, resulting in materials with excellent adsorption capabilities for various dye molecules.In this study, 1 mg of the synthesized PVA-MOF or hPG-MOF was dispersed in 5 mL of dye solution (50 ppm) and subjected to sonication followed by stirring for 24 hours at 25\u0026deg;C. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e, both adsorbents exhibited high adsorption capacities toward all three tested dyes. These results highlight the strong potential of PVA-MOF and hPG-MOF composites for efficient dye removal in aqueous environments.\u003c/p\u003e\u003cp\u003eThe maximum adsorption capacities of PVA-MOF for the cationic dyes rhodamine B (Rh B) and methylene blue (MB), as well as the anionic dye fluorescein (FL), were 128.17 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, 128.24 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, and 124.77 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, respectively. Under the same conditions, hPG-MOF exhibited adsorption capacities of 131.46 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for Rh B, 135.34 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for MB, and 128.31 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for FL (Table S3). While PVA-MOF showed superior performance in the removal of the anionic dye, hPG-MOF demonstrated significantly higher adsorption capacities for cationic dyes compared to its linear counterpart.\u003c/p\u003e\u003cp\u003eInterestingly, both MOFs were able to adsorb the anionic FL dye effectively, despite their negatively charged surfaces under neutral and basic conditions. This observation suggests that electrostatic interactions are not the sole driving force governing dye adsorption; other mechanisms, such as π\u0026ndash;π stacking, hydrogen bonding, and coordination interactions, may also play a significant role.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e"},{"header":"Discussion","content":"\u003cp\u003eTable S3 presents a comparison of the adsorption capacities of the synthesized MOFs with those of similar materials reported in the literature. Despite having fewer aromatic ligands and lower metal content-due to the nature of their polymeric backbones-both PVA-MOF and hPG-MOF exhibit excellent performance in dye pollutant removal. The use of PVA and hPG as the primary structural components not only contributes to high adsorption efficiency but also enhances the biocompatibility of the materials. Moreover, this design minimizes the risk of leaching toxic aromatic ligands into aqueous environments, making these MOFs promising candidates for environmentally friendly water purification applications.\u003c/p\u003e\u003cp\u003eTo elucidate the adsorption mechanisms of the dyes, the rate constants for both the pseudo-first-order and pseudo-second-order kinetic models were examined for each dye (see Tables S4). The adsorption behavior at various concentrations followed the pseudo-second-order kinetic model more closely, as evidenced by the better fit of the kinetic data with this model, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e.\u003c/p\u003e\u003cp\u003eThe adsorption kinetics of Methylene Blue (MB), Rhodamine B (Rh B), and Fluorescein (FL) on the synthesized MOFs were best described by the pseudo-second-order kinetic model. The calculated parameters showed excellent agreement with the experimental data, indicating that the adsorption process is predominantly governed by chemisorption involving valence forces through electron sharing or exchange between the dye molecules and the adsorbent surface (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e and Figure S6).\u003c/p\u003e\u003cp\u003eTo evaluate the adsorption isotherms, both Langmuir and Freundlich models were applied. The Langmuir model yielded higher correlation coefficients (R\u003csup\u003e2\u003c/sup\u003e) for all three dyes, FL, MB, and Rh B, suggesting monolayer adsorption on a homogeneous surface (Figure S3). The maximum adsorption capacities predicted by the Langmuir model are presented in Table S6.\u003c/p\u003e\u003cp\u003eThe adsorption process is likely driven by a combination of electrostatic interactions, π\u0026ndash;π stacking, and hydrogen bonding. The presence of carboxyl and amino functional groups within the polymeric framework enhances these interactions, facilitating strong binding between the dye molecules and the MOF surface.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eAccording to the Langmuir isotherm model, dye molecules are uniformly adsorbed within the cavities of the MOFs with polymeric matrices, indicating a homogeneous adsorption surface. This uniform adsorption behavior suggests that the PVA-MOF and hPG-MOF possess a structurally consistent and well-defined scaffold. The calculated maximum adsorption capacities for Fluorescein, Methylene Blue (MB), and Rhodamine B (Rh B), based on the Langmuir equation, are summarized in Table S7.\u003c/p\u003e\u003cp\u003eThermodynamic parameters provide deeper insights into the mechanisms of dye adsorption (see Figure S4 and Table S5). Thermodynamic analyses confirmed that the adsorption process is endothermic, becoming more favorable with increasing temperature and accompanied by an increase in disorder. For cationic dyes (such as Rhodamine B and Methylene Blue), the adsorption is non-spontaneous, whereas for the anionic dye (such as Fluorescein), the process is spontaneous (see Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e and Table S8).\u003c/p\u003e\u003cp\u003eThe interactions between the dyes and the adsorbents are primarily driven by electrostatic forces and hydrogen bonding, both of which are endothermic. The rise in entropy during the adsorption of the dyes may be attributed to the dispersion and aggregation of dye molecules post-interaction with the MOFs, leading to increased disorder within the system.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe pH parameter is of critical importance in adsorption studies. The adsorption of MB, RhB, and FL was investigated over a pH range of 2 to 10 (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003ea and \u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003eb). The initial dye solution had a pH approximately equal to 7. Acidic and alkaline conditions were adjusted by adding volumes of 0.1 M HCl and 0.1 M NaOH, respectively.\u003c/p\u003e\u003cp\u003eThe findings indicated that both removal efficiency and adsorption capacity reach their maximum around pH 10 for Rh B and MB and decline at higher pH values. In basic mediums MB and Rh B are not positively charged, therefore electrostatic interaction with the negatively charged MOFs is not a driving force. On the other side FL was considerably adsorbed by hPG-MOF in basic medium while both dye and MOF are negatively charged. One possible explanation for the observed pH-dependent adsorption behavior is that, at higher pH values, the carboxyl groups of the AIP ligand become deprotonated, resulting in increased negative surface charge within the MOF pores. This electrostatic repulsion among negatively charged sites may lead to pore expansion or enhanced accessibility. As a result, the adsorption capacity increases, primarily through hydrogen bonding and π\u0026ndash;π interactions rather than electrostatic attraction. Adsorption of FL by PVA-MOF was not significant in basic pH, indicating a major role for the electrostatic repulsion in the case.\u003c/p\u003e\u003cp\u003eGiven that, in real environmental matrices such as municipal water, other elements coexist simultaneously, it is essential to evaluate the adsorption performance of the selected adsorbents under actual conditions. To this end, removal efficiency and adsorption capacity were assessed using samples of municipal water, Khoramrood River water, and Stone Stormwater, each containing dye concentrations of 50 ppm.\u003c/p\u003e\u003cp\u003eSamples of each water source were analyzed prior to treatment to determine their initial dye concentrations. Subsequently, 1mg of the adsorbent was added to each solution, and the mixtures were stirred for a predetermined period. The residual dye concentrations were measured at specific time intervals to evaluate the adsorption kinetics. The removal efficiency and adsorption capacity were then calculated based on the initial and final dye concentrations. The results are summarized in tables S9. The results of the experiment with D\u003csub\u003e2\u003c/sub\u003eO showed that both MOF adsorbents performed well in the adsorption of dyes. The adsorption capacity data showed distinct patterns for each dye: methylene blue showed the highest adsorption efficiency (128.24\u0026ndash;135.34), followed by rhodamine B (128.17\u0026ndash;131.46), while fluorescein showed the lowest adsorption capacity (124.77\u0026ndash;128.31). The results showed that hPG-MOF consistently outperformed PVA-MOF in all types of dyes, with the most pronounced difference observed in the adsorption of methylene blue. These results were also confirmed in subsequent experiments with real waters (rock storm water, river water, and drinking water), indicating that both adsorbents also perform well in real environmental conditions.\u003c/p\u003e\u003cp\u003eThe stability and reusability of the adsorbents are essential for their practical application in dye removal from aqueous media. To assess these properties, 1 mg of each MOF was employed to adsorb dyes (10 mg.L⁻\u0026sup1;) from aqueous solutions. In the first cycle, both PVA-MOF and hPG-MOF demonstrated near-complete dye removal. After each cycle, the adsorbents were regenerated by washing with acetone to desorb the dye molecules, followed by drying at 70\u0026deg;C before reuse.\u003c/p\u003e\u003cp\u003eAs shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003ec, the removal efficiency of both MOFs remained nearly constant over three consecutive adsorption\u0026ndash;desorption cycles, confirming their excellent stability and reusability. The combination of high adsorption capacity, favorable kinetic behavior, and straightforward regeneration underscores the strong potential of these MOF\u0026ndash;polymer composites for industrial-scale dye removal and wastewater treatment applications.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e"},{"header":"Conclusions","content":"\u003cp\u003eIn this study, metal-organic frameworks (MOFs) incorporating polymeric backbones were successfully synthesized through ligand conjugation to linear and hyperbranched polyols, followed by ligand exchange with iron (III) chloride. The resulting materials exhibited efficient removal of both cationic and anionic dyes from aqueous solutions, with adsorption performance showing strong pH dependency. Maximum dye uptake occurred under alkaline conditions, where the frameworks' pores were in an open state, enhancing adsorption capacity. These results underscore the potential of polymer-integrated MOFs as effective and responsive materials for environmental remediation. Furthermore, this work paves the way for the development of a new class of functional MOFs with polymeric matrices, offering promising applications in catalysis, water treatment, and advanced separation processes.\u003c/p\u003e"},{"header":"Methods","content":"\u003cp\u003eSynthesis of mesylated polyvinyl alcohol (PVA-OMs)\u003c/p\u003e\u003cp\u003eInitially, polyvinyl alcohol (PVA) (0.2 gr,0.0028 mmol) was added to a round-bottom flask along with the solvent dimethylformamide (DMF) (10 mL) and heated to 110\u0026deg;C until fully dissolved. The solution was then cooled to room temperature, and trimethylamine (Et\u003csub\u003e3\u003c/sub\u003eN) (1 mL) was added at room temperature and stirred for 2 hours. The resulting solution was placed in an ice bath, and methanesulfonyl chloride (MsCl) (1.78 mL,23mmol) was gradually added over the course of one hour. The mixture was then stirred at room temperature for 3 days. Product was crystalized in acetonitrile and used for further experiments The overall reaction yield was approximately 69.70%.\u003c/p\u003e\n\u003ch3\u003eConjugation of 5-amino isophthalic acid (AIP) to polyvinyl alcohol (PVA-AIP)\u003c/h3\u003e\n\u003cp\u003eMesylated polyvinyl alcohol (PVA-Oms) (0.1 gr, 0.000736 mmol) was dissolved in acetonitrile (25 ml), after which potassium carbonate (k\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e) (0.1 gr ,0.724 mmol) and 5-amino isophthalic acid (AIP) (0.11 gr ,0.6 mmol) were added. The mixture was refluxed at 80\u0026deg;C for 24 hours. The final product was purified using a dialysis bag in dimethylformamide (DMF), distilled water (D\u003csub\u003e2\u003c/sub\u003eO), and ethanol (EtOH), and it was dried in a vacuum oven at 50\u0026deg;C.The overall reaction yield was approximately 84.04%.\u003c/p\u003e\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\u003ch2\u003eSynthesis of PVA-MOF\u003c/h2\u003e\u003cp\u003ePVA-AIP and hexahydrate iron (III) chloride were mixed in a 2:1 ratio in a beaker, and the solvent dimethylformamide (DMF) (25 mL) was added. The resulting mixture was stirred for 2 hours and then placed in an autoclave, where it was heated to 110\u0026deg;C for 20 hours. The final product was purified by washing with dimethylformamide (DMF) and ethanol and was then dried in a vacuum oven at 50\u0026deg;C.The overall reaction yield was approximately 70.39%.\u003c/p\u003e\u003c/div\u003e\n\u003ch3\u003eSynthesis of mesylated hyperbranched polyglycerol (hPG-OMs)\u003c/h3\u003e\n\u003cp\u003eHyperbranched polyglycerol (hPG) (Mn\u0026thinsp;=\u0026thinsp;5000), (0.258 gr, 0.0516 mmol) was dissolved in a polymerization ampoule under an inert gas atmosphere (nitrogen) in dimethylformamide (DMF) (10 mL), and subsequently, triethylamine (Et\u003csub\u003e3\u003c/sub\u003eN) (1 mL) was added while maintaining the temperature at 0\u0026deg;C. Msyl chloride (MsCl) (1.74 mL, 22.47 mmol), was gradually added over the course of 1 hour. After the addition of mesyl chloride, the mixture was refluxed in a nitrogen atmosphere at room temperature for 24 hours. The crude product was purified using a dialysis bag in acetonitrile.The overall reaction yield was approximately 78.66%.\u003c/p\u003e\n\u003ch3\u003eConjugation of 5-Amino isophthalic acid (AIP) to mesylated hyperbranched Polyglycerol (hPG-AIP)\u003c/h3\u003e\n\u003cp\u003eMesylated hyperbranched polyglycerol (hPG-Oms) (0.1 gr, 0.0156 mmol) was dissolved in acetonitrile (25 mL), after which potassium carbonate (k\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e) (0.1 gr, 0.724 mmol) and 5-amino isophthalic acid (AIP) (0.234 gr, 1.29 mmol) were added. The mixture was stirred at 80\u0026deg;C for 24 hours. The final product was purified using a dialysis bag in dimethylformamide (DMF), distilled water (D\u003csub\u003e2\u003c/sub\u003eO), and ethanol (EtOH), and it was dried in a vacuum oven at 50\u0026deg;C.The overall reaction yield was approximately 83.66%.\u003c/p\u003e\u003cdiv id=\"Sec11\" class=\"Section2\"\u003e\u003ch2\u003eSynthesis of hPG-MOF\u003c/h2\u003e\u003cp\u003eThe synthesis method for this compound is similar to that of PVA-MOF.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec12\" class=\"Section2\"\u003e\u003ch2\u003eDye removal\u003c/h2\u003e\u003cp\u003eA stock solution of methylene blue, rhodamine B, and fluorescein was prepared by dissolving 100 mg.L\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e of these dyes in water. Subsequently, standard solutions were prepared by diluting the stock solution for testing. For adsorption experiments, 3 mg of PVA-MOF and hPG-MOF was added to 5 mL of color solutions at concentrations of 20 ppm, 10 ppm, and 5 ppm (Rhodamine B, Methylene Blue, and Fluorescein) and incubated for 24 hours under ambient conditions (25\u0026deg;C) without agitation.\u003c/p\u003e\u003cp\u003eAfter 24 hours, it was observed that the adsorbent could significantly absorb cationic dyes (Rhodamine B, Methylene Blue) and, to a lesser extent, the anionic dye (Fluorescein). Using a spectrophotometer, the absorbance of all samples at the corresponding λmax for each dye was obtained and compared with the standard curve. The dye adsorption capacity qt (mg. g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) and the percentage removal of dye (%R) by the adsorbent at each time point were calculated. Our aim was to investigate the adsorption of cationic and anionic dyes, which are among the most significant water pollutants.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec13\" class=\"Section2\"\u003e\u003ch2\u003eData availability\u003c/h2\u003e\u003cp\u003eThe datasets used and/or analysed during the current study available from the corresponding author on reasonable request.\u003c/p\u003e\u003c/div\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgements\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eWe would like to thank Core Facility of Lorestan University for the analysis of the synthesized materials.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eS.G performed the relevant synthesis and analyses, also wrote the first manuscript. M.A conceptualized the projects and edited the manuscript. M. N helped with the formal analysis.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCompeting interests\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare that they have no competing interests.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding Declaration\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe research described in this manuscript didn’t support by funding.\u0026nbsp;\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eKordbacheh, F. \u0026amp; Heidari, G. Water pollutants and approaches for their removal. \u003cem\u003eMater. Chem. Horizons\u003c/em\u003e. \u003cb\u003e2\u003c/b\u003e (2), 139\u0026ndash;153 (2023).\u003c/span\u003e\u003c/li\u003e\u003cli\u003e\u003cspan\u003eRahman, N. A. A. A., Khasri, A., Ahmad, A. A., Jamir, M. R. M. \u0026amp; Yasin, N. H. M. Preparation of AC/TiO2 doped N-Ce Synthesized via Microwave Irradiation for Amoxicillin Photodegradation. \u003cem\u003eInt. J. Integr. 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Control\u003c/em\u003e. \u003cb\u003e97\u003c/b\u003e (11), 2539\u0026ndash;2551 (2024).\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true},"keywords":"Metal-organic framework, polyvinyl alcohol, hyperbranched polymer poly(glycerol), MIL-101 (Fe), dye removal","lastPublishedDoi":"10.21203/rs.3.rs-8050532/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-8050532/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eIn this study, novel metal-organic frameworks (MOFs) were synthesized using functionalized polyols as ligands. Polyvinyl alcohol (PVA) and hyperbranched polyglycerol (hPG) were first mesylated and subsequently modified with 5-aminoisophthalic acid. These functionalized polymers were then reacted with iron (III) chloride hexahydrate to form related MOFs including PVA-MOF and hPG-MOF. The resulting MOFs exhibited high adsorption capacities for both cationic dyes (Rhodamine B and Methylene Blue) and an anionic dye (Fluorescein) from aqueous solutions. Adsorption studies revealed that dye removal followed the Langmuir isotherm model, with maximum capacities reaching 128.17\u0026ndash;135.34 mg.g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e depending on the type of dye and MOF. Thermodynamic analysis showed that adsorption was endothermic, with increased entropy, and spontaneous for the anionic dye, while non-spontaneous for the cationic dyes. The materials also demonstrated excellent structural stability and regeneration potential over three adsorption-desorption cycles. Furthermore, performance was confirmed using real water samples, indicating that PVA-MOF and hPG-MOF are promising, reusable adsorbents for efficient dye removal in wastewater treatment.\u003c/p\u003e","manuscriptTitle":"Metal-Organic Frameworks with Linear and Branched Polyol Backbones for Dye Removal","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-11-26 17:57:36","doi":"10.21203/rs.3.rs-8050532/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-12-15T11:28:45+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-11-27T07:01:24+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-11-21T07:38:17+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"101759797738476114874643222589099490111","date":"2025-11-19T06:28:27+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"69323586448890196380345874119072719566","date":"2025-11-17T08:10:46+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"302533567501747566304193684886017087935","date":"2025-11-17T06:24:27+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-11-17T05:06:34+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-11-11T15:41:32+00:00","index":"","fulltext":""},{"type":"editorInvited","content":"","date":"2025-11-11T12:56:11+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-11-10T12:43:54+00:00","index":"","fulltext":""},{"type":"submitted","content":"Scientific Reports","date":"2025-11-10T12:39:55+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"11d65841-0efa-4e12-9eb5-be8301519d73","owner":[],"postedDate":"November 26th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[{"id":58368075,"name":"Physical sciences/Chemistry"},{"id":58368076,"name":"Earth and environmental sciences/Environmental sciences"},{"id":58368077,"name":"Physical sciences/Materials science"}],"tags":[],"updatedAt":"2026-01-21T09:43:40+00:00","versionOfRecord":[],"versionCreatedAt":"2025-11-26 17:57:36","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-8050532","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-8050532","identity":"rs-8050532","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}