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Article

Injection-Molded Poly(butylene succinate)/Wheat Flour By-Product Biocomposites: Mechanical, Thermal, and Structural Characterization

by
Bianca Peron-Schlosser
1,*,
Rúbia Martins Bernardes Ramos
1,
Luana Cristina Paludo
1,
Pablo Inocêncio Monteiro
1,
Fabíola Azanha de Carvalho
2,
Samuel Camilo da Silva
2,
Bruno Alexandro Bewzenko Cordova
3,
Benjamim de Melo Carvalho
3,
Fabio Yamashita
2 and
Michele Rigon Spier
1,*
1
Post-Graduation Program in Food Engineering, Technology Sector, Chemical Engineering Department, Federal University of Paraná (UFPR), Street Coronel Francisco Heráclito dos Santos, 210–Jardim das Américas, Curitiba 82590-300, Paraná, Brazil
2
Post-Graduation Program in Food Science, Food Science and Technology Department, State University of Londrina (UEL), Highway Celso Garcia Cid|PR 445 Km 380, Londrina 86057-970, Paraná, Brazil
3
Post-Graduation Program in Engineering and Material Science, State University of Ponta Grossa (UEPG), Av. Carlos Cavalcanti, 4748, Ponta Grossa 84030-900, Paraná, Brazil
*
Authors to whom correspondence should be addressed.
Processes 2025, 13(4), 1044; https://doi.org/10.3390/pr13041044
Submission received: 10 March 2025 / Revised: 26 March 2025 / Accepted: 29 March 2025 / Published: 31 March 2025
(This article belongs to the Section Materials Processes)
Browse Figures
Versions Notes

Abstract

:
The increasing concern regarding the environmental impact of conventional plastics has intensified the search for sustainable alternatives. This study investigated the development and characterization of biocomposites produced from glue flour (GF), a wheat milling by-product, and poly(butylene succinate) (PBS) using injection molding. GF/PBS ratios of 100/0 (PBS0), 80/20 (PBS20), 70/30 (PBS30), and 60/40 (PBS40) (w/w) were evaluated in terms of physical, mechanical, and thermal properties. The results showed that increasing the PBS content significantly enhanced tensile strength from 1.36 MPa (PBS0) to 12.23 MPa (PBS40) and Young’s modulus from 0.12 MPa to 1.54 MPa. Water solubility decreased from 37.03% (PBS0) to 16.08% (PBS40), and linear shrinkage was reduced from 5.5% (PBS0) to around 2.0% (PBS40). Scanning electron microscopy (SEM) analysis revealed improved homogeneity and reduced granule visibility with higher PBS concentration. Fourier transform infrared spectroscopy (FTIR) spectra indicated intensified interactions between starch, proteins, and PBS as its content in the formulation increased. Thermal analysis revealed that biocomposites containing PBS exhibited well-defined melting (Tm ~115 °C) and crystallization (Tc ~80 °C) temperatures, indicating more consistent thermal behavior than the PBS-free sample. These findings suggest that GF/PBS biocomposites have strong potential as sustainable alternatives to conventional plastics, offering viable applications across various industrial sectors.

Graphical Abstract

1. Introduction

The global production of plastics in 2023 reached 413.8 million tons, with the majority derived from fossil sources (90.4%). Only 8.7% of this production was classified as circular, highlighting the challenges in transitioning to a more sustainable economy [1]. Moreover, producing and incinerating fossil-based plastics generate significant CO2 emissions, contributing to global warming and causing direct environmental impacts [2]. Growing concerns about these effects have motivated significant advancements in scientific research, culminating in the development of more suitable alternatives such as biopolymers, biodegradable plastics, and biocomposites [3].
Biopolymers, derived from natural sources, emerge as a promising alternative to non-degradable plastics, potentially contributing to sustainable strategies for plastic waste management [4]. According to Drummond et al. [5], the reuse of waste from the food industry in packaging applications has increased in recent decades, mainly driven by the environmental implications associated with the extensive use of single-use polymer-based packaging. This practice has significantly contributed to the accumulation of plastic waste in landfills and surface and marine water bodies. Food waste and by-products contain various compounds, such as proteins, cellulose, starch, lipids, and waxes, which can be used as raw materials for developing biodegradable materials. Despite mechanical properties, permeability, and moisture absorption limitations, these biomolecules can be optimized to transform biological raw materials into viable biopolymers. Such solutions could replace petrochemical-derived plastics widely used in domestic and commercial packaging [6].
Starch is among the most extensively studied biopolymers for producing blends with both biodegradable and conventional polymers, partly due to its lower cost [7]. However, its application in this context competes directly with the food supply chain. Alternatively, by-products from wheat flour milling—rich in starch—present a promising source. Wheat, one of the world’s top five crops, is expected to reach a global production of approximately 791.2 million metric tons in the 2023/24 harvest [8]. Around 75% of this production is destined for flour production, while the remaining 25% results in industrial waste or agro-industrial by-products [low-grade flour, “clean-out” flour, wheat flour, and glue flour (GF)] [9,10].
According to Frantz et al. [10], GF is wheat flour that falls outside quality specifications and is commonly repurposed by the adhesive manufacturing industry. In addition to being a low-cost input, GF contains approximately 65% starch, 11% protein, 8% fiber, 2% lipids, and 0.5% ash; these components interact naturally and intrinsically, forming an effective bioplastic matrix, reinforcing its potential as a viable alternative for sustainable packaging applications [11,12]. In addition to starch content, the proteins present in flour can also serve as a polymer matrix in bioplastic production. However, other authors have reported that the effect of the content of proteins was not observed in the thermal or mechanical analyses of wheat-flour-based materials [13]. Lipids contribute to barrier properties, fibers act as reinforcing agents enhancing structural and mechanical characteristics, and ash plays a role in improving thermal properties [14,15]. Nevertheless, as these compounds are present in small amounts in GF, they likely had no significant influence on the material properties in this study. As the starch, GF is also biodegradable. These factors suggest that GF may be a promising material for blend studies in biocomposite production.
The incorporation of starch into biodegradable polyesters—such as poly(caprolactone) (PCL), poly(butylene adipate-co-terephthalate) (PBAT), poly(lactic acid) (PLA), and poly(butylene succinate) (PBS)—improves the intrinsic properties of starch without compromising its biodegradability [2,16,17]. PBS is an innovative, sustainable, and environmentally friendly material with excellent mechanical properties, good thermal and chemical resistance, and complete biodegradability [18]. It also has proven to be a promising polymer for use in combination with starch, contributing to the development of sustainable packaging [19]. Although PBS remains an expensive raw material compared to conventional plastics, its use in blends significantly reduces overall production costs [2,20].
Biocomposites produced from PBS-based blends through injection molding have been widely studied [21,22,23,24]. However, to the best of our knowledge, this is the first time that blends of PBS and wheat flour have been systematically studied for the development of biocomposites. Although previous studies have explored wheat flour with other biodegradable polymers, such as PLA [13,25] and PBAT [26,27], combining GF with PBS can result in biocomposites with satisfactory properties and reduced production costs. This approach enables the development of new material with potential for various applications, such as disposable trays, food packaging, and other products, while simultaneously adding value to an agro-industrial by-product and promoting more sustainable alternatives to conventional polymers. To achieve this, it is essential to investigate different proportions of GF and PBS. Therefore, this study aimed to develop and characterize biocomposites produced from GF and PBS blends.

2. Materials and Methods

2.1. Raw Materials

To produce the biocomposites, glue flour (GF) containing 19% amylose was sourced from a wheat mill in Curitiba, Paraná, Brazil. Glycerol, with a purity of 99.5%, was provided by Alphatec Ltda., São Paulo, Brazil. The PBS (TH803-S) was also obtained from Xinjiang Blueridge Tunhe Chemical Industry Co., Ltd., Changji, Xinjiang, China.

2.2. Biocomposites Production

Figure 1 illustrates the overall methodology followed for the preparation of the biocomposites.
Biocomposites with four different proportions of GF/PBS [100/0 (PBS0), 80/20 (PBS20), 70/30(PBS30), 60/40 (PBS40), w/w] were produced, and the ratio of glycerol to GF was (30/70 w/w). The components were weighted, mixed, and extruded in a pilot single-screw (model EL-25, BGM, São Paulo, Brazil) with a screw diameter of 25 mm (L/D = 30) and a screw speed of 35 rpm. The temperature profile was 90/150/150/130, using a two-hole cylindrical die (2 mm) for production. The materials were pelletized, and they were processed in a lab-scale injection molding machine AX16II (AX Plásticos Máquinas Técnicas Ltda., Diadema, São Paulo, Brazil) with a screw seed of 100 rpm and repression pressure of 0.35 to 0.69 MPa. The temperature profile was 130/120/130. The mold was maintained at room temperature. Biocomposites were molded in specimens according to ASTM D638-10 [28].

2.3. Biocomposite Characterization

2.3.1. Instrumental Color Measurement

The color parameters of the biocomposites were assessed using a colorimeter Chroma Meter CR-400 (Konica Minolta Sensing, Inc., Tokyo, Japan) based on the International Commission on Illumination (CIE Lab) color system. The results were reported in terms of L*, a*, and b*, where L* represents luminosity or brightness, ranging from black (0) to white (100); a* indicates the green (−60) to red (+60) spectrum; and b* corresponds to the blue (−60) to yellow (+60) axis.

2.3.2. Linear Contraction Index (LCI)

Ten specimens from each formulation were measured after seven days; they were conditioned in desiccators at 53% relative humidity at 25 °C, using a digital caliper (0.01 mm resolution, Starrett Indústria e Comércio Ltda., Itu, São Paulo, Brazil). The linear contraction of the specimens was determined according to Equation (1) [29].
L C I % = L c m − L c p L c m × 100
where Lcm is the length of the mold cavity (theoretical), and Lcp is the length of the specimen (after conditioning).

2.3.3. Solubility in Water

Biocomposites were cut, dried in an oven at 105 °C for 24 h, and weighed (m1, g). The dried pieces were then immersed in Erlenmeyer flasks containing 150 mL of distilled water and agitated on a shaker at 25 °C for 24 h. Subsequently, the samples were dried in an oven at 105 °C for 24 h and reweighed (m2, g). The solubility percentage for each formulation was calculated according to Equation (2).
S o l u b i l i t y   ( % ) = m 1 − m 2 m 1 × 100

2.3.4. Mechanical Properties

The mechanical properties of the biocomposites were performed on the AG-I equipment (Shimadzu, Kyoto, Japan) with a 10 kN load cell, following the standard method ASTM D638-10 [28] with modifications. The initial separation of the grips and the speed were 65 mm and 50 mm/min, respectively. Ten repetitions were performed for each biocomposite. The specimens from each formulation were conditioned in desiccators under 53% RH for 7 d at 25 °C before being analyzed.

2.3.5. Scanning Electron Microscopy (SEM)

The surface and cross-sectional morphology of the biocomposites were analyzed using a scanning electron microscope (SEM) model JSM 6360-LV (JEOL Ltd., Tokyo, Japan). Before analysis, the films were stored in a silica desiccator for seven days. Samples were fractured using liquid nitrogen, then fixed onto supports with copper tape and metalized with a thin layer of gold (model FL 9496, Balzers Union, Balzers, Liechtenstein). An acceleration voltage of 10 kV was utilized for image analysis, with magnifications of 250×.

2.3.6. Fourier Transform Infrared Spectroscopy (FTIR)

The biocomposites underwent FTIR analysis to investigate chemical interactions between matrix components. The analysis was conducted using an Alpha FTIR spectrometer (Bruker, MA, USA) equipped with an attenuated total reflectance (ATR) accessory, fitted with a zinc selenide crystal in the spectral range of 500–4000 cm−1 and a resolution of 4 cm−1.

2.3.7. Differential Scanning Calorimetry (DSC)

A differential scanning calorimeter (model DSC 60, Shimadzu Co., Ltd., Japan) was used to assess the melting (Tm) and crystallization (Tc) temperatures of the biocomposites. The samples (8–10 mg) were accurately weighed and sealed in aluminum pans. Subsequently, they were heated under a nitrogen atmosphere from 25 to 200 °C at a rate of 10 °C/min and cooled from 200 to 40 °C at a rate of 5 °C/min. Two heating and two cooling cycles were performed for each sample.

2.4. Statistical Analysis

All analyses were performed in triplicate, and the results were processed using the Statistica 7.0® software (Statsoft Inc., Tulsa, OK, USA). The Tukey test was used to compare means.

3. Results and Discussion

3.1. Visual Appearance and Color Parameters of Biocomposites

Figure 2 presents the physical appearance of injection-molded biocomposites with different PBS contents (0%, 20%, 30%, and 40%).
PBS0 biocomposites appear darker and rougher, indicating a more heterogeneous structure, possibly due to poor polymer dispersion or phase separation in the absence of PBS. This surface may suggest lower mechanical integrity, correlating with the lowest tensile strength and Young’s modulus in the mechanical data.
The biocomposites PBS20, PBS30, and PBS40 appear smoother, lighter, and more uniform with increasing PBS content. This suggests that PBS improves the homogeneity of the composite, leading to better dispersion of GF and polymer matrix. The increasing smoothness aligns with the improved mechanical properties (higher strength and Young’s modulus) and lower shrinkage observed in Table 3 and Figure 3, respectively.
The color parameters (L*, a*, and b*) of the biocomposites with and without PBS prepared by injection molding are shown in Table 1. The L* values, which indicate lightness, increased as the PBS content increased. The PBS0 sample exhibited the lowest L* value (38.98 ± 2.04), whereas the highest L* value was observed for PBS40 (53.65 ± 3.33), suggesting that the incorporation of PBS contributed to a lighter appearance of the biocomposites.
The a* parameter, representing the green–red spectrum, decreased with the addition of PBS, indicating a shift towards a greener hue. PBS0 had the highest a* value (8.94 ± 1.11), while PBS40 showed the lowest (3.56 ± 0.20), reinforcing the tendency toward reducing the red component as PBS content increased.
Similarly, the b* parameter, representing the blue–yellow spectrum, showed variations with PBS incorporation. The highest b* values were recorded for PBS20 (31.00 ± 3.17) and PBS30 (31.15 ± 1.05), while PBS40 exhibited a slight reduction (29.03 ± 2.66), suggesting that at higher PBS concentrations, the yellowish hue of the biocomposites was slightly diminished.
Statistical analysis (Tukey Test, p < 0.05) confirmed that significant differences existed among the samples in each color parameter (indicated by different lowercase letters in the same column). These variations highlight the impact of PBS content on the optical properties of the biocomposites, which may influence their aesthetic and functional applications in various industries.
In the study by Carvalho [30], biocomposites produced with PLA and cassava bagasse exhibited a similar effect. Formulations with higher PLA concentrations appeared lighter, as the increase in PLA content contributed to greater brightness and reduced opacity. As the fiber concentration increased, the samples became darker.

3.2. Shrinkage

Materials produced through injection molding can undergo contraction as they transition from a molten to a solid state under atmospheric pressure [31]. The linear contraction indexes (LCIs) of the GF/PBS biocomposites are shown in Figure 3. The highest shrinkage (~5.5%) was observed for PBS0, which indicates significant contraction after molding, probably due to the high starch concentration and the absence of PBS. For PBS20, PBS30, and PBS40, shrinkage decreases significantly (~2% for all), showing that adding PBS helps stabilize the biocomposite structure. The reduction in shrinkage with increased PBS content aligns with the increase in Young’s modulus (Table 3), reinforcing that PBS enhances rigidity.
The shrinkage exhibited no statistically significant differences among the PBS20, PBS30, and PBS40 samples, with values of 1.99% ± 0.20, 2.00% ± 0.17, and 1.73% ± 0.11, respectively. Suggesting that even small amounts of PBS (~20%) are enough to improve dimensional stability.
Studies indicate that an increase in fiber concentration reduces the contraction of the injected material. This occurs because fibers can act as fillers, occupying spaces in the blend’s structure and decreasing its ability to expand or shrink [21,32]. Wheat tailings flour contains a negligible amount of fibers, around 8.28% [11], which may have influenced the higher contraction observed in the sample with 100% GF.
The contraction percentage of the injected piece is also directly related to the mold temperature, with higher mold temperatures resulting in greater shrinkage [33]. Additionally, it can be influenced by other factors such as material composition, pressure, injection flow rate, and equipment design [21,34].

3.3. Biocomposites Solubility in Water

The solubility results of the PBS0, PBS20, PBS30, and PBS40 samples are presented in Table 2. The solubility ranged from 37.03% to 16.08% and showed significant differences (p < 0.05). The sample without PBS addition (PBS0) exhibited the highest mean water solubility of 37.03% due to the higher presence of starch molecules in the cola flour. The PBS40 sample showed the lowest mean solubility of 16.08%, with a statistically significant difference. Starch molecules form hydrogen bonds with water molecules, facilitating water absorption. Furthermore, the glucose in starch is hydrophilic [35,36].
It was observed that the addition of PBS resulted in a 56.6% reduction in the solubility of the samples. Similar results were described by Zeng et al. [16], who synthesized a mixture of thermoplastic starch (TPS) with reactive PBS (RPBS). The authors observed that TPS had more than 30% soluble fraction, while TPS/RPBS50 had only 10.5%. The decrease in solubility can be attributed to the hydrophobic nature of PBS, thus contributing to greater hydrophobicity of the material.

3.4. Tensile Strength, Elongation, and Young’s Modulus

Table 3 presents the mechanical properties (tensile strength, elongation, and Young’s modulus) of biocomposites made from GF with varying percentages of PBS. The PBS content ranges from 0% (PBS0) to 40% (PBS40), allowing for an analysis of how PBS affects the material’s mechanical properties.
The tensile strength is the lowest for PBS0 (1.36 ± 0.03 MPa). This indicates that the glue flour-based composite alone has weak resistance to tension. As PBS content increases, the tensile strength significantly improves. PBS20 exhibited a tensile strength about 4.5 times higher than PBS0, and the highest value (12.23 ± 0.16) was achieved for PBS40. This suggests that the PBS reinforces the GF matrix, significantly enhancing the tensile strength of the biocomposite. This behavior is consistent with previous findings on PBS/starch systems; according to Ayu et al. [22], the tensile strength of PBS blends decreased as the starch content increased, which is attributed to the transition of the main phase from flexible PBS to rigid starch. Furthermore, poor dispersion of starch in the PBS may lead to stress concentration zones, reducing tensile strength. Additionally, as the starch content increased, a higher number of voids may have been introduced into the structure, weakening the blends due to reduced interfacial interaction between PBS and the starch-based GF matrix, as can be observed in the SEM micrographs of this study (Figure 4).
The tensile strength values are consistent with those reported by Chabrat et al. [13] for PLA/wheat flour blends. A formulation containing 75% wheat flour, and 25% glycerol exhibited a tensile strength of 1.8 MPa, and the addition of 20 parts of PLA to the plasticized wheat flour increased this mechanical property to 9.6 MPa.
Sasimowski et al. [23] produced biocomposites from PBS and wheat bran, observing a mechanical behavior like that reported in this study. Samples with a higher PBS concentration and lower wheat bran content exhibited greater tensile strength. Since tensile strength strongly depends on the interactions between the matrix and the reinforcement, the authors attributed its reduction to weak interactions between the wheat bran and PBS and the absence of a compatibilizing agent. Consequently, due to their hydrophilic nature, samples with a higher wheat bran content exhibited more structural defects, which can act as failure initiation points during tensile testing. These observations are relevant and applicable to the present study.
Muthuraj et al. [37] demonstrated that this effect also occurred in biocomposites produced with PBS and perennial grasses. However, the authors reported that adding 5% of a compatibilizing agent based on maleic-anhydride-grafted PBS significantly improved the mechanical properties of the biocomposites. The same behavior was reported by Gowman et al. [38] for biocomposites from PBS and grape pomace.
The biocomposite without PBS has a relatively high elongation of 21.03 ± 0.50%, which is quite flexible. With increasing PBS, elongation decreases slightly to 18.09 ± 0.61% (PBS20) and further reduces to 16.06 ± 1.00% (PBS30). Interestingly, elongation increases to 24.77 ± 2.08% for PBS40. Initially, adding PBS reduces the elongation, possibly due to phase incompatibility or embrittlement at lower PBS contents. However, at 40% PBS, the material becomes more ductile again, likely due to better dispersion and polymer interaction. Although a linear increase in elongation with higher PBS content was expected, the behavior observed in this study may be related to the reduced glycerol content in the formulations. Since the primary function of a plasticizer is to enhance flexibility [39], the decrease in glycerol from 30% (PBS0) to 24% (PBS20) and 21% (PBS30) may have negatively influenced the elongation of the materials. On the other hand, the higher elongation observed for PBS40 could be attributed to the higher PBS content in the formulation, as PBS is inherently more flexible.
Chabrat et al. [13], in developing PLA and wheat flour blends, formulated a mixture containing only wheat flour and glycerol, 75% and 25%, respectively, like the PBS0 formulation used in the present study. In this work, the flour-to-glycerol ratio was 70:30. The plasticized wheat flour obtained by the authors resulted in ductile material, with Young’s modulus of 15 MPa and an elongation at break of 58%, values higher than that obtained in this study (Table 3). When 20 parts of PLA were incorporated into the plasticized flour (83.3% of wheat flour and 16.7% of glycerol), an increase in Young’s modulus (709 MPa) and a reduction in elongation (7%) were observed. The authors attributed the low elongation values to the reduced glycerol content in the blend.
Sasimowski et al. [23] observed a linear relationship between elongation and wheat bran content, where an increase in wheat bran content leads to a decrease in elongation. Similarly, Silva et al. [21] noted a linear reduction in elongation at break with the increase in oat hull content in PBS/starch/oat hull biodegradable materials.
In contrast to the results of the study of Chabrat et al. [13], GF/PBS biocomposites exhibited the lowest Young’s modulus for PBS0 (0.12 ± 0.01 MPa), indicating a very soft material. A significant increase was observed in this property with increasing PBS content. The Young’s modulus follows a clear increasing trend, showing that the addition of PBS enhances the rigidity of the composite. However, Sasimowski et al. [23] related a different trend from this study: Young’s modulus increases while increasing wheat bran content in biocomposites.

3.5. SEM Analysis

Figure 4 presents the morphological analysis of the surfaces and cross-sections of the samples PBS0, PBS20, PBS30, and PBS40. The PBS0 sample displays fractures and cracks throughout its surface and cross-section, which can be attributed to the absence of PBS in the formulation. As PBS is added (PBS20, PBS30, and PBS40), fractures decrease, and the material’s morphology becomes more homogeneous and continuous. In all samples, the presence of GF granules distributed throughout the material’s extent is noticeable (red circles). However, as the PBS content increases (PBS20, PBS30, and PBS40), the visibility of these granules decreases.
In a previous study, Silva et al. [40] synthesized materials with poly(lactic acid) (PLA) and starch and attributed the low visibility of the granules to their fusion and dispersion within the polymer matrix, resulting in materials with continuous phases, which can be observed in the surface analyses of the PBS30 and PBS40 samples. Ayu et al. [22] highlighted that the dispersion of the granules in PBS results in strong bonds between these components, positively influencing the mechanical properties of the materials. This can be proven with the PBS30 and PBS40 samples, which exhibit smoother surface morphology and higher tensile strength (Table 3). These results suggest a direct relationship between the improvement in morphology and increased tensile strength, emphasizing the crucial role of the interaction between wheat flour granules and PBS in the mechanical quality of the composites.
PBS40 exhibits a fibrillar morphology with a more homogeneous surface, while its cross-section displays visible fissures and folds in the fibers (indicated by blue arrows). These characteristics may result from the fracture process the sample underwent during the cross-section preparation, causing morphological changes in the material.
It is important to note that morphological variations are influenced by a series of factors, such as the composition of the mixtures, the interfacial energy, and the viscosity of the components in the samples [41]. These aspects may have influenced the morphological differences observed on the surface and in the cross-section of the samples with different contents of PBS and wheat flour.

3.6. FTIR (Fourier Transform Infrared) Analysis

Figure 5 shows the FTIR spectra of the PBS0, PBS20, PBS30, and PBS40 samples. The FTIR spectra of the PBS20, PBS30, and PBS40 samples exhibited a prominent band around 3300 cm−1, along with peaks at 2942, 1716, 1313, 1160, and 1036 cm−1.
According to previous studies, the band at 3300 cm−1 and the peaks at 2942 and 1160 cm−1 are consistent with characteristic starch groups, attributed to OH stretching, aliphatic CH groups, and CO stretching [12,42]. Peron-Schlosser et al. [11] highlighted that bands near 3280 cm−1 may be related to interactions between starch, glue flour, and protein in the sample composition and between hydroxyls and hydrogen bonds.
Regions between 1000 and 1350 cm−1 can be associated with C-N amine bonds, as studied by Peron-Schlosser et al. [12]. The authors related peaks in this range with amines present in the protein of glue flour. Beluci et al. [43] describe that regions between 1711 and 1720 cm−1 are attributed to the C=O stretching of ester groups in the sample components.
The peak at 1160 cm−1 is attributed to hydrogen bonds of starch present in the composition of wheat flour. A similar study was reported by Peron-Schlosser et al. [12], who synthesized films from wheat flour by-product enriched with rosemary extract and found a similar peak at 1150 cm−1.
The peaks observed in the regions between 1015 to 1017 cm−1 are present due to C-O-C bonds, specifically by C-O stretching vibrations in glycosidic bonds, as described by Zhai et al. [44]. In this work, these bonds can be identified by peaks in the region of 1036 to 1007 cm−1.
Finally, the band intensity at 3300 cm−1 was observed in all samples and the emergence of peaks at 1716, 1313, and 1160 cm−1 in the PBS20, PBS30, and PBS40 samples occurred as the PBS content in the formulation increased. This suggests that interactions between glue flour components and the polymeric matrix intensified as the PBS content increased, forming new functional groups.

3.7. Thermal Analysis

The thermal analysis of the biocomposites, with and without the addition of PBS, is presented in Figure 6. All samples demonstrated similar thermal behavior, except for the one without PBS (PBS0). The samples exhibited both endothermic and exothermic peaks, with a melting temperature (Tm) of approximately 115 °C and a crystallization temperature (Tc) of around 80 °C, respectively. These results indicate that the presence of PBS significantly influenced the thermal behavior of the materials containing PBS compared to those without it. A previous study by Schlosser [27] reported a Tm of 122.06 °C and a Tc of 82.25 °C for films of PBAT/GF blend containing 60%PBAT, 24% GF, and 16% glycerol.
Sasimowski et al. [24] observed a Tm of 118.5 °C for pure PBS. With the addition of 15% wheat bran or onion peels, these values were slightly decreased to 116.7 °C. At a 30% filler content, Tm values were slightly higher, suggesting that more homogeneous crystallites were formed during crystallization processes. The Tc value for pure PBS was 86.4 C, and the incorporation of the fillers led to a reduction in this temperature.
In the present study, the Tm and Tc for GF/PBS are close to those Sasimowski et al. [24] reported for pure PBS, indicating that the presence of GF may have slightly shifted the thermal transitions without significantly altering the crystallization behavior of the PBS.
Aziman et al. [45] did not observe a significant change in Tm for films with different contents of PBS, TPS, and silver particles. The authors attributed the minimal change in temperature to the large proportion of PBS used in the formulation.
Thermal analysis of materials and the identification of melting and crystallization temperatures are critical because the behavior of materials containing polymers in their composition is influenced by temperature during all phases, from production to storage, application, and distribution [46].

4. Conclusions

This study demonstrated the feasibility of producing GF/PBS biocomposites using injection molding. Although the most cost-effective and environmentally sustainable formulation is PBS0 (100% GF), this sample presented processing difficulties, and its properties were not satisfactory, highlighting the importance of developing blends. The results showed that increasing PBS content significantly enhanced the mechanical performance of the GF/PBS biocomposites, with tensile strength increasing from 1.36 MPa (PBS0) to 12.23 MPa (PBS40) and Young’s modulus rising from 0.12 MPa (PBS0) to 1.54 MPa (PBS40). Moreover, PBS incorporation reduced water solubility from 37.03% (PBS0) to 16.08% (PBS40) (a reduction of 56.6%) and linear shrinkage from 5.5% (PBS0) to approximately 2% (PBS40), indicating improved dimensional stability.
Morphological analysis via SEM confirmed a more homogeneous structure with higher PBS concentration, suggesting better interaction between PBS and GF. The FTIR analysis revealed intensified interactions between starch, wheat flour proteins, and PBS, supporting improved mechanical and structural properties. Furthermore, the thermal analysis indicated that formulations with PBS (PBS20, PBS30, and PBS40) exhibited well-defined melting (Tm ~115 °C) and crystallization (Tc ~80 °C), reinforcing their potential for industrial applications.
Regarding sustainability and biodegradability of the GF/PBS biocomposites, although no biodegradation tests were conducted in this study, the raw materials used in the formulations—GF, PBS, and glycerol—are recognized as biodegradable, as stood out in the introduction. Therefore, it can be inferred that the resulting biocomposites also exhibit biodegradability. However, for future studies, it is recommended to perform specific biodegradation assessments to quantify degradation rates under different environmental conditions and confirm their potential for sustainable applications.
Additionally, further improvements in GF/PBS biocomposite performance may be achieved by incorporating compatibilizers (e.g., maleic anhydride), applying physical and/or chemical treatment to GF to improve compatibility with PBS, using additional plasticizers (e.g., sorbitol or citric acid), and exploring nanomaterial reinforcement. Furthermore, it is recommended that future formulation and processing optimizations be guided by statistical experimental designs, such as mixture design or central composite rotational design (CCRD).

Author Contributions

Conceptualization, B.P.-S., F.Y. and M.R.S.; methodology, F.Y., F.A.d.C., S.C.d.S. and B.A.B.C.; formal analysis, B.P.-S., F.A.d.C., S.C.d.S. and B.A.B.C.; data curation, B.P.-S., R.M.B.R., L.C.P. and P.I.M.; writing—original draft preparation, B.P.-S., R.M.B.R., L.C.P. and P.I.M.; writing—review and editing, B.P.-S., R.M.B.R., L.C.P. and P.I.M.; supervision, M.R.S., B.d.M.C. and F.Y.; project administration, M.R.S. All authors have read and agreed to the published version of the manuscript.

Funding

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior–CAPES (nº 88882.381648/2019-1) and Conselho Nacional de Desenvolvimento Científico e Tecnológico-CNPq (nº 306591/2021-9).

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Acknowledgments

The authors would like to thank the Center for Studies in Biopharmacy and the Center for Electronic Microscopy (CEM) from UFPR.

Conflicts of Interest

The authors declare no conflicts of interest.

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Processes 13 01044 g001
Figure 1. Methodological steps for GF/PBS biocomposite development.
Figure 1. Methodological steps for GF/PBS biocomposite development.
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Figure 2. Physical appearance of injection-molded biocomposites.
Figure 2. Physical appearance of injection-molded biocomposites.
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Figure 3. Linear contraction index (LCI) of the GF/PBS biocomposites.
Figure 3. Linear contraction index (LCI) of the GF/PBS biocomposites.
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Figure 4. SEM micrographs of PBS0, PBS20, PBS30, and PBS40 surface (S) and cross-section (T). Red circles: GF granules; Blue arrows: fiber folds.
Figure 4. SEM micrographs of PBS0, PBS20, PBS30, and PBS40 surface (S) and cross-section (T). Red circles: GF granules; Blue arrows: fiber folds.
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Figure 5. ATR-FTI R spectra of PBS0, PBS20, PBS30, and PBS40 biocomposites.
Figure 5. ATR-FTI R spectra of PBS0, PBS20, PBS30, and PBS40 biocomposites.
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Figure 6. DSC heating (a) and cooling (b) thermograms of PBS0, PBS20, PBS30, and PBS40 biocomposites.
Figure 6. DSC heating (a) and cooling (b) thermograms of PBS0, PBS20, PBS30, and PBS40 biocomposites.
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Table 1. Color parameters of the GF/PBS biocomposites prepared by injection molding.
Table 1. Color parameters of the GF/PBS biocomposites prepared by injection molding.
BiocompositesL*a*b*
PBS038.98 ± 2.04 d8.94 ± 1.11 a19.15 ± 1.41 b
PBS2048.37 ± 1.13 c4.97 ± 0.30 b31.00 ± 3.17 a
PBS3050.86 ± 2.48 b4.75 ± 0.35 b31.15 ± 1.05 a
PBS4053.65 ± 3.33 a3.56 ± 0.20 c29.03 ± 2.66 a
Lowercase letters in the same column indicate significant differences (Tukey Test, p < 0.05).
Table 2. Solubility in water of the GF/PBS biocomposites prepared by injection molding.
Table 2. Solubility in water of the GF/PBS biocomposites prepared by injection molding.
BiocompositesSolubility (%)
PBS037.03 ± 0.91 a
PBS2026.98 ± 1.81 ab
PBS3021.99 ± 1.80 bc
PBS4016.08 ± 1.19 c
Lowercase letters in the same column indicate significant differences (Tukey Test, p < 0.05).
Table 3. Mechanical properties of the GF/PBS biocomposites prepared by injection molding.
Table 3. Mechanical properties of the GF/PBS biocomposites prepared by injection molding.
BiocompositesTensile Strength
(MPa)		Elongation
(%)		Young’s Modulus
(MPa)
PBS01.36 ± 0.03 d21.03 ± 0.50 b0.12 ± 0.01 d
PBS206.24 ± 0.22 c18.09 ± 0.61 c0.94 ± 0.03 c
PBS309.00 ± 0.48 b16.06 ± 1.00 d1.18 ± 0.04 b
PBS4012.23 ± 0.16 a24.77 ± 2.08 a1.54 ± 0.09 a
Lowercase letters in the same column indicate significant differences (Tukey Test, p < 0.05).
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MDPI and ACS Style

Peron-Schlosser, B.; Ramos, R.M.B.; Paludo, L.C.; Monteiro, P.I.; de Carvalho, F.A.; da Silva, S.C.; Cordova, B.A.B.; Carvalho, B.d.M.; Yamashita, F.; Spier, M.R. Injection-Molded Poly(butylene succinate)/Wheat Flour By-Product Biocomposites: Mechanical, Thermal, and Structural Characterization. Processes 2025, 13, 1044. https://doi.org/10.3390/pr13041044

AMA Style

Peron-Schlosser B, Ramos RMB, Paludo LC, Monteiro PI, de Carvalho FA, da Silva SC, Cordova BAB, Carvalho BdM, Yamashita F, Spier MR. Injection-Molded Poly(butylene succinate)/Wheat Flour By-Product Biocomposites: Mechanical, Thermal, and Structural Characterization. Processes. 2025; 13(4):1044. https://doi.org/10.3390/pr13041044

Chicago/Turabian Style

Peron-Schlosser, Bianca, Rúbia Martins Bernardes Ramos, Luana Cristina Paludo, Pablo Inocêncio Monteiro, Fabíola Azanha de Carvalho, Samuel Camilo da Silva, Bruno Alexandro Bewzenko Cordova, Benjamim de Melo Carvalho, Fabio Yamashita, and Michele Rigon Spier. 2025. "Injection-Molded Poly(butylene succinate)/Wheat Flour By-Product Biocomposites: Mechanical, Thermal, and Structural Characterization" Processes 13, no. 4: 1044. https://doi.org/10.3390/pr13041044

APA Style

Peron-Schlosser, B., Ramos, R. M. B., Paludo, L. C., Monteiro, P. I., de Carvalho, F. A., da Silva, S. C., Cordova, B. A. B., Carvalho, B. d. M., Yamashita, F., & Spier, M. R. (2025). Injection-Molded Poly(butylene succinate)/Wheat Flour By-Product Biocomposites: Mechanical, Thermal, and Structural Characterization. Processes, 13(4), 1044. https://doi.org/10.3390/pr13041044

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