Development of sustainable flame-retardant bio-based hydrogel composites from hemp/wool nonwovens with chitosan-banana sap hydrogel | Scientific Reports

Scientific Reports volume 14, Article number: 22116 (2024) Cite this article

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Flame retardant (FR) finishing is crucial for developing protective textiles, traditionally relying on halogen, phosphorus, and phosphorus-nitrogen chemistries, which have limitations like toxicity and fabric stiffening. Innovative approaches such as nanotechnology, plasma treatments, and natural resource-based finishes are being explored to achieve sustainable FR textiles. This study presents the development and comprehensive characterization of hydrogel composites made from nonwoven fabrics composed of various hemp/wool blends (70/30, 80/20, and 90/10). The nonwoven fabrics were treated with a chitosan hydrogel incorporating banana sap to enhance their properties. Scanning electron microscope (SEM) examined the surface morphology and structural integrity of the composites, while Fourier transform infrared spectroscopy (FTIR) identified chemical interactions and functional groups. Differential scanning calorimeter (DSC) revealed thermal properties, water absorbency tests demonstrated hydrophilicity, mechanical testing assessed tensile strength, and vertical flammability tests evaluated fire resistance. SEM and FTIR revealed a successful coating of chitosan hydrogel with banana sap inclusions onto the hemp/wool nonwoven fabric, forming a composite structure. DSC analysis suggests higher chitosan content and hemp fiber ratio (like 70/30) lead to increased thermal stability of hydrogel composites. Higher chitosan concentrations in the hydrogel significantly improve the flame-retardant properties of hemp/wool nonwoven fabrics by reducing char length and enhancing protective char layer formation, with banana sap further promoting charring. These results indicate that the developed composite can be effectively used in flame-retardant textiles.

The growing concern over environmental sustainability and fire safety in textiles has led to increased interest in the development of bio-based, flame-retardant materials1,2,3,4. Traditional flame retardants often rely on halogenated compounds, which, despite their effectiveness, pose significant environmental and health risks due to their toxicity and potential to release harmful byproducts during combustion. As a result, there is a pressing need to develop alternative materials that are both environmentally friendly and effective in enhancing the fire resistance of textiles.

Natural fibers are highly combustible, and fabric construction and density influence the flammability of fabrics made from these fibers5,6. while natural fibers have reactive groups, the challenge lies in achieving durable and effective FR treatments that are both environmentally friendly and capable of withstanding repeated use and laundering. Wool’s reactive groups can facilitate the attachment of FR agents; however, ensuring that these treatments are both sustainable and resistant to washing remains a significant challenge, especially when compared to synthetic fibers that may offer more straightforward options for durable FR finishes7.

Natural fibers, such as hemp and wool, have garnered attention for their inherent sustainability and biodegradability. Hemp, with its high strength, durability, and low environmental impact, is an attractive candidate for developing sustainable textile composites8. Wool, on the other hand, possesses natural flame-retardant properties due to its high nitrogen and sulfur content, making it a valuable component in flame-retardant materials. However, the challenge lies in further enhancing the flame resistance of these fibers to meet the stringent safety standards required in various applications9.

Flame-retardant fabrics can be produced through chemical grafting and finishing processes10,11. Methods such as blending flame retardants in spinning solutions12, chemical grafting, and finishing are efficient and cost-effective10,13. Organic flame retardants are often used in these methods. However, traditional flame retardants, including halogenated agents like bromine and chlorine, as well as certain phosphorus-based agents such as phosphonates and phosphoramides, pose significant risks. These risks stem from the production of toxic gases during combustion and the release of formaldehyde during use, making these compounds hazardous to human health and harmful to the environment14. Therefore, it is crucial to develop efficient, innovative, eco-friendly, and non-toxic flame-retardant systems that are halogen-free, formaldehyde-free, and produce less smoke. In this context, hydrogels derived from natural polymers like chitosan, a biopolymer obtained from chitin, offer a promising solution. Over the past decades, numerous eco-friendly materials have been explored to enhance the flame retardancy of flammable polymeric materials, including proteins, chitosan, starch, and phytic acid15,16,17,18.

Chitosan is not only biodegradable and non-toxic but also exhibits excellent film-forming capabilities, making it suitable for use as a matrix in composite materials. Furthermore, the incorporation of natural additives like banana sap, rich in phenolic compounds and antioxidants, can enhance the thermal stability and flame-retardant properties of the hydrogel composites19. A previous study examined the effectiveness of chitosan hydrogels in preventing spontaneous coal combustion, reporting that chitosan increased water retention and thermal stability. These materials typically impart flame resistance to polymeric materials through surface treatment and blending technologies for fabrics. However, the resulting treated fibers and fabrics often lack durability, leading to a relatively short service life20. Banana plant pseudostem sap (B. sap), is a stable liquid suitable for fabric applications across various pH ranges, showing khaki coloration in alkaline conditions without staining. Previous research highlighted its fire retardant properties and elemental composition on cotton fabric, revealing significant constituents like sodium, magnesium, silicate, and phosphates21.

This research focuses on the development of sustainable flame-retardant hydrogel composites by reinforcing hemp/wool nonwovens with a chitosan-banana sap hydrogel. The study aims to investigate the synergistic effects of combining these natural fibers with a bio-based hydrogel to create a composite material that not only meets environmental and sustainability criteria but also provides effective flame retardancy. The characterization of these composites will be conducted to assess their mechanical properties, thermal stability, water absorption, and flame resistance, thereby demonstrating their potential for application in fire-safe, eco-friendly textiles.

Chitosan as hydrogel’s precursor and acetic acid as a solvent were purchased from Sigma Aldrich. Wool and hemp fibers were taken from the National Textile University.

Table 1 presents the two factors considered in the experiment: the concentration of chitosan and the blend ratio of wool/hemp nonwoven fabric. Each factor has three levels, indicating the different concentrations and fabric types studied.

The experiment was structured using a full factorial design, generating nine samples in total. Table 2 provides detailed information about each sample.

Developing nonwoven fabric involved manually preparing and feeding wool and hemp fibers into (Dongwong-roll Co. Ltd., nonwoven) machines manufactured in Incheon, South Korea. This fabrication process comprised two main stages: web formation and web bonding. Initially, The web was formed by opening the fibres manually and passing them through a series of machines, such as a coarse fibre opening machine, a fine opener, a reserve hopper feeder, a mini carding machine, and a cross lapper. Subsequently, The formed web went through bonding processes by first being fed into a pre-needle punching machine, then into a 10 mm-deep needle punching machine. Three distinct nonwoven materials were manufactured, each varying in blend ratio according to the DOE in Table 2.

A series of solutions with varying concentrations of chitosan (0.5%, 1%, and 1.5% w/w) were prepared. In a beaker with a magnetic stirrer, chitosan was added to 1% v/v acetic acid for each concentration. The combination was mixed at 750 rpm for 4 h to guarantee total disintegration. The nonwoven fabrics previously prepared were then impregnated with these chitosan solutions at room temperature. Each nonwoven specimen was squeezed physically utilizing a glass bar to help in the absorption of the chitosan. When completely impregnated, the specimen was eliminated from the arrangement and hung to permit the extra chitosan to drain. Subsequently, the samples were air-dried at room temperature to enable proper crosslinking of the chitosan molecules. Following drying, the samples were immersed in B. sap solution, ensuring thorough absorption, after which they were removed and dried again.

To study the surface morphology of the non-conductive fibers, scanning electron microscope (Nova SEM) after coating the samples with gold for better analysis.

Fourier transform infrared spectroscopy (FTIR) was used to investigate the chemical composition of the samples before and after hydrogel coating. The spectra were collected from 4000 cm− 1 to 600 cm− 1 using a PerkinElmer FTIR spectrometer.

A differential scanning calorimeter (DSC) with a heating range of 25 to 400 °C and a heating rate of 5 °C per minute was used to conduct thermal analysis of the nonwovens before and following the application of the hydrogel.

ISO 13934-2 evaluated the hydrogel composite’s tensile strength. The “grab method” was used, where a 20 cm x 10 cm sample was gripped and steadily stretched until rupture at room temperature. The force at break was then recorded.

The water absorbency of the specimens was determined by ASTM D570.

ASTM D-6413 was used to conduct vertical flame tests on fabric strips measuring 30 cm by 7.6 cm.

Figure 1a is the SEM image of hemp/wool nonwoven fabric displaying a fibrous network with visible inter-fiber spaces, characteristic of nonwoven structures. The image reveals the entanglement and bonding of fibers, contributing to the material’s mechanical stability. The rough surface texture of the hemp fibers contrasts with the smoother wool fibers, enhancing the fabric’s overall surface area and potential adsorption properties. The scale bar indicates the magnification level. Figure 1b exhibits the SEM image of hemp/wool nonwoven fabric coated with banana sap incorporated chitosan hydrogel, showcasing the composite structure. The hydrogel layer is a continuous coating over the fibers, with visible adhesion points where the hydrogel firmly bonds to the fibrous network. Integrating the hydrogel into the fabric’s structure is evident, enhancing the composite’s mechanical and adsorption properties. The incorporation of banana sap is indicated by small inclusions within the hydrogel, contributing to its unique surface morphology and functionality.

SEM micrographs of (a) pure nonwoven fabric and (b) chitosan hydrogel composite.

Figure 2 shows the FTIR spectra of all the hydrogel composite samples of varying concentrations of chitosan hydrogel onto the hemp/wool nonwoven fabric. FTIR revealed the characteristic peaks of the hemp/wool nonwoven fabric and the chitosan hydrogel. The peak near 1550 cm−1 is due to the N-H bending vibrations in the protein backbone of wool. Additionally, a broad peak around 2800–3000 cm−1 will be present due to C-H stretching vibrations in both cellulose (hemp) and keratin (wool). A broad peak around 3000–3600 cm−1 signifies the presence of hydroxyl (OH) groups, while another peak in the 2800–3000 cm−1 region represents C-H stretching within the chitosan molecule. The presence of the carbonyl group in chitosan’s acetamide (COCH3) structure is evident by a peak around 1640 cm−1. Finally, peaks around 1000–1150 cm−1 are expected due to C-O-C stretching in the glycosidic linkages between sugar units of chitosan. The peak intensities are lowest for samples 1–3, higher for samples 4–6, and highest for samples 7–9. This is because 0.5% chitosan was applied to samples 1–3, 1% to samples 4–6, and 1.5% to samples 7–9. Increasing the concentration of hydrogel, more molecules will be present, increasing the intensity of the peaks. All these peaks confirm the presence of chitosan hydrogel on the surface of the wool/hemp nonwoven fabric.

FTIR analysis of hydrogel composite samples.

Differential Scanning Calorimetry (DSC) was performed on various nonwoven hydrogel composite samples to investigate their thermal properties and their results are shown in Fig. 3. The hemp/wool 70/30 sample exhibited an endothermic peak at 130 °C with a depth of −0.8 W/g and an exothermic peak above 350 °C with a peak height of 0.3 W/g, indicating moisture loss or phase transition and thermal degradation of the fibers, respectively. For the hemp/wool 70/30 composite with 1% chitosan hydrogel incorporated with banana sap, the endothermic peak at 130 °C had a depth of −1.5 W/g, and the exothermic peak shifted to 320 °C with the same peak height of 0.3 W/g. This suggests that the addition of chitosan and banana sap increased energy absorption due to enhanced moisture content or stronger interactions within the composite while slightly lowering thermal stability. Increasing the chitosan concentration to 1.5% in the same blend raised the endothermic peak to 135 °C with a depth of −1.5 W/g, and the exothermic peak occurred at 330 °C with a peak height of 0.2 W/g, indicating robust interactions and slightly improved thermal stability with reduced energy release during degradation. The hemp/wool 80/20 blend with 1.5% chitosan hydrogel showed an endothermic peak at 130 °C with a depth of −1.3 W/g and an exothermic peak at 330 °C with a peak height of 0.1 W/g, reflecting good thermal stability with less energy release upon degradation. The hemp/wool 90/10 blend with 1.5% chitosan hydrogel exhibited an endothermic peak at 125 °C with a depth of -0.9 W/g and an exothermic peak at 330 °C with a peak height of 0.1 W/g, indicating lower moisture absorption or weaker internal interactions but high thermal stability and minimal energy release upon degradation. The endothermic peaks around 125–135 °C are likely due to the loss of absorbed moisture or phase transitions. Higher chitosan content and specific blends (like 70/30 with chitosan) show higher depths, indicating more energy absorbed due to moisture loss or stronger internal interactions.

DSC thermograms of (A: Hemp/wool 70/30, B: Hemp/wool 70/30 1% chitosan, C: Hemp/wool 70/30 1.5% chitosan D: Hemp/wool 80/20 1.5% chitosan E: Hemp/wool 90/10 1.5% chitosan) hydrogel composites.

Figure 4 represents the tensile strength and elongation properties of hemp/wool nonwoven fabrics reinforced with chitosan hydrogel at varying concentrations. The nonwoven fabrics were prepared in three blend ratios: 70/30, 80/20, and 90/10. The tensile strength results reveal that the application of 0.5% chitosan hydrogel yields the lowest tensile strength across all fabric types, with the 70/30 blend exhibiting the highest strength (7.15 N), followed by the 80/20 blend (4.95 N), and the 90/10 blend (3.77 N). As the chitosan concentration increases to 1%, there is a significant improvement in tensile strength. The 70/30 blend shows the greatest enhancement (18.98 N), while the 80/20 and 90/10 blends also demonstrate notable increases (15.31 N and 14.11 N, respectively). At a chitosan concentration of 1.5%, the tensile strength reaches its peak, with the 70/30 blend exhibiting the highest strength (42.61 N), followed by the 90/10 blend (30.75 N) and the 80/20 blend (30.55 N). Overall, increasing the wool content generally leads to a reduction in tensile strength at each chitosan concentration, as hemp fibers provide higher tensile strength compared to wool fibers.

In terms of elongation, the 0.5% chitosan hydrogel concentration results in the highest elongation for all fabric types, with the 70/30 blend showing the highest elongation (48.39%), followed by the 80/20 blend (43.45%) and the 90/10 blend (42.51%). As the chitosan concentration increases to 1%, elongation slightly decreases, with the 70/30 blend showing the highest elongation (45.32%), followed by the 80/20 blend (40.11%) and the 90/10 blend (40.1%). At a 1.5% chitosan concentration, elongation decreases further, with the 70/30 blend exhibiting the highest elongation (45.76%), followed by the 80/20 blend (38.33%) and the 90/10 blend (36.45%). Increasing the wool content generally increases elongation, particularly at lower chitosan concentrations, due to wool fibers’ greater elasticity than hemp fibers. However, increasing the chitosan concentration slightly reduces elongation, likely due to forming a more rigid hydrogel matrix.

Mechanical properties of hydrogel composite samples.

The water absorption properties of the chitosan hydrogel composites, reinforced with hemp/wool nonwoven fabrics and incorporating banana sap, were systematically investigated and results are shown in Fig. 5. The study varied the concentration of the chitosan hydrogel solution (0.5, 1, and 1.5) and the composition of the nonwoven fabrics (hemp/wool ratios of 70/30, 80/20, and 90/10). Results indicated a clear trend where increased chitosan concentration led to higher water absorption values across all fabric types. Specifically, at a chitosan concentration of 0.5, the water absorption values were 483.838 for the 70/30 blend, 539.141 for the 80/20 blend, and 583.056 for the 90/10 blend. As the concentration increased to 1, the absorption values correspondingly increased to 538.23, 645.15, and 606.24 for the 70/30, 80/20, and 90/10 blends, respectively. The highest chitosan concentration of 1.5 yielded absorption values of 615.64 for the 70/30 blend, 638.813 for the 80/20 blend, and 678.929 for the 90/10 blend. Notably, the nonwoven fabric with a higher hemp content consistently exhibited greater water absorption capacity. This was particularly evident in the 90/10 hemp/wool blend, which achieved the maximum absorption of 678.929 at the highest chitosan concentration of 1.5. These findings suggest that both the chitosan concentration and the hemp content in the nonwoven fabric significantly enhance the water absorption capabilities of the composite. This study highlights the importance of optimizing both the polymer matrix concentration and the fabric composition to achieve desirable water absorption properties in hydrogel composites, which is crucial for their application in areas requiring high moisture retention.

Water absorbency of hydrogel composite samples.

Table 3 shows the results of the vertical flame-retardant test on all the composite samples and a control sample. The results show that increasing the chitosan concentration generally reduces the duration of flaming, especially at 1.5% concentration, where the shortest flaming times are observed (10 s or less). Higher chitosan concentratifons significantly reduce the char length, indicating better flame retardancy through more effective charring. At lower chitosan concentrations (0.5% and 1%), the composition of the nonwoven fabric does not significantly impact the char length, with all samples exhibiting a char length of 30 cm. However, at a 1.5% concentration, the char length is markedly reduced across all fabric compositions, suggesting enhanced flame-retardant properties with higher chitosan content. Interestingly, the after-glow time increases with the chitosan concentration of 1% chitosan, particularly for the 80/20 and 90/10 fabric compositions. This could be due to a more pronounced smoldering effect as the hydrogel potentially releases more water vapor and other non-combustible gases during burning. Conversely, at 1.5% chitosan, the after-glow times decrease significantly for all fabric types compared to 1%, indicating that the hydrogel effectively extinguishes the flame and prevents prolonged smoldering.

From Fig. 6, the control sample (0% chitosan) exhibits a very short duration of flaming (3 s) but a relatively long after-glow time and char length (30 cm). This indicates that while the initial flaming is brief, the material continues to burn slowly during the after-glow phase and does not effectively form a protective char layer. Chitosan, being a polysaccharide, can form a char layer upon heating, which acts as a barrier to heat and mass transfer. This char layer helps reduce flame spread and protect the underlying material. Incorporating banana sap could potentially enhance the flame-retardant properties by promoting charring and forming a protective layer. The ratio of hemp to wool in the nonwoven fabric affects the material’s inherent flammability, with wool being naturally flame retardant and hemp being less so. The observed results demonstrate that the overall flame-retardant properties are improved more significantly at higher chitosan concentrations, regardless of the fabric composition. In conclusion, the chitosan hydrogel concentration significantly influences the flame-retardant properties, with higher concentrations generally improving flame retardancy and reducing char length. The combination of chitosan hydrogel, banana sap, and the hemp/wool nonwoven fabric provides effective flame-retardant properties, particularly at higher chitosan concentrations.

Vertical flammability test results after burning of samples.

This study successfully developed and characterized flame-retardant hydrogel composites from nonwoven hemp/wool blends treated with chitosan hydrogel incorporating banana sap. Nonwoven fabrics with hemp/wool blends (70/30, 80/20, and 90/10) and varying chitosan concentrations (0.5%, 1%, and 1.5%) have been developed. SEM and FTIR analysis confirmed the application of chitosan hydrogel onto the nonwoven fabric samples. The results suggested that the chitosan coating improved the thermal stability and water absorbency of the composites, while higher chitosan content and hemp fiber ratio further enhanced these properties. Significantly, the composites exhibited improved flame retardancy compared to the untreated fabrics, with chitosan concentration and banana sap playing a key role in char formation. These findings suggest the potential of these bio-based composites for sustainable flame-retardant textiles.

All data generated/ analysed during this study are included within the manuscript.

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This work was supported by Ajman University UAE.

School of Engineering and Technology, National Textile University, Faisalabad, 37610, Pakistan

Zaid Ali, Farooq Azam, Bushra Mushtaq, Sheraz Ahmad, Faheem Ahmad, Abher Rasheed & Muhammad Qamar Khan

Department of Clinical Sciences, College of Dentistry, Ajman University, Ajman, United Arab Emirates

Muhammad Sohail Zafar

School of Dentistry, University of Jordan, Amman, Jordan

Muhammad Sohail Zafar

Department of Dental Materials, Islamic International Dental College, Riphah International University, Islamabad, Pakistan

Muhammad Sohail Zafar

Centre of Medical and Bio-allied Health Sciences Research, Ajman University, Ajman, United Arab Emirates

Muhammad Sohail Zafar

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Mr. Zaid Ali, Ms. Bushra and Dr. Farooq Azam conducted the research. Dr. Faheem Ahmad, Dr. Muhammad Sohail Zafar & Dr. Qamar Khan helped in the Characterization. Dr. Abher and Dr. Sheraz reviewed the manuscript and guided in the overall project.

Correspondence to Faheem Ahmad or Muhammad Sohail Zafar.

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Ali, Z., Azam, F., Mushtaq, B. et al. Development of sustainable flame-retardant bio-based hydrogel composites from hemp/wool nonwovens with chitosan-banana sap hydrogel. Sci Rep 14, 22116 (2024). https://doi.org/10.1038/s41598-024-73052-0

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Received: 06 August 2024

Accepted: 12 September 2024

Published: 27 September 2024

DOI: https://doi.org/10.1038/s41598-024-73052-0

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