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Article

Preparation of Antistatic Polyester Fiber via Layer-by-Layer Self-Assembly

by
Wei Wang
1,2,
Jialong Zhang
3,
Yifan Liu
1,2,
Mengyun Weng
1,2 and
Yanchun Fu
1,2,*
1
College of Furnishings and Industrial Design, Nanjing Forestry University, Nanjing 210037, China
2
Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources, Nanjing Forestry University, Nanjing 210037, China
3
College of Art and Design, Nanjing Forestry University, Nanjing 210037, China
*
Author to whom correspondence should be addressed.
Coatings 2024, 14(10), 1236; https://doi.org/10.3390/coatings14101236
Submission received: 29 August 2024 / Revised: 20 September 2024 / Accepted: 23 September 2024 / Published: 25 September 2024
(This article belongs to the Special Issue Polymer Thin Films: From Fundamentals to Applications (Second Edition))
Browse Figures
Versions Notes

Abstract

:
Polyester fibers tend to generate static electricity during the weaving and application processes, posing a threat to their production. Enhancing the water absorbency and electrical conductivity of polyester fibers themselves is an effective approach to improving their antistatic properties. In this study, multifunctional chitosan (CS), sodium phytate (SP), and Cu2+ were loaded on polyester fibers through layer-by-layer (LBL) self-assembly. The antistatic and water absorption capability of the modified polyester fibers was investigated by designing different process parameters combined with a surface resistance test and water contact angle tests. The antistatic property test results confirmed the positive effect of CS and Cu2+ on discharging electrostatic charge. Within a definite scope, with the increase in the number of assembly layers, assembly duration, and the concentration of the assembly substances, the wettability of the modified polyester fibers became more favorable and the antistatic effect became more remarkable.

1. Introduction

In the present era of organic synthesis and the development of macromolecule polymers, an increasing number of highly practical polyester fibers with different specialties are being developed and put into production and use [1,2]. Polyester fibers are widely used in the textile industry for their superior mechanical properties, comfort, and breathing abilities, such as high tensile strength and modulus, moderate resilience, excellent thermal setting effects, good heat, light resistance, etc. [3,4]. Polyester fiber has become the fiber with the fastest development and the largest output among synthetic fibers due to the good controllability of the preparation process and excellent product performance [5,6]. However, the significant problem of static electricity generation has limited its production and application to a certain extent. Effective antistatic modification is urgently needed to expand the application range of polyester fiber [7,8,9]. Various polymeric modifiers are utilized for the permanent antistatic modification of synthetic fibers. Sano et al. designed copoly(amide-ethers)-containing ionic units as antistatic modifiers to form hygroscopic paths, which greatly reduce resistivity. Even after dyeing, the antistatic properties persisted. This is due to the fact that both hydrophilic and ionic groups had been effectively immobilized on the surface of polyester fibers [10,11].
Metal ion coordination modification is an effective method utilized to create functional fabrics [12,13,14,15]. This process forms a crosslinked structure via coordination between metal ions and the ligand functional groups present on the fabric’s surface. In this way, the antistatic, antimicrobial, and other physicochemical properties of fabrics can be effectively improved for a wide range of demanding applications. Xu et al. employed phytic acid, seafoam, polyaspartic acid, and Fe3+ as raw materials and successfully prepared dense protective film coatings on the surface of cotton fabrics by using a layer-by-layer self-assembly method and spraying technique. This protective layer endowed cotton fabric with long-lasting flame-retardant properties [16]. Nabipour et al. deposited guanazole complexes containing silver and zinc ions on the surface of cotton fabrics by layer-by-layer self-assembly. The treated cotton fabrics showed excellent flame retardancy with a UL-94 V-0 rating in a vertical combustion test. At the same time, they also had excellent antimicrobial properties, and the silver guanazole-treated cotton fabrics also had good antifungal activity [17]. In recent years, there has been a growing interest in employing layer-by-layer (LBL) self-assembly technology for the antistatic modification of polyester fibers [18,19,20]. LBL self-assembly is a highly versatile and used technique for surface modification that involves the sequential adsorption of a polyanion and a polycation to form thin polymer films [21,22]. This technique offers a broad range of materials for constructing layer-by-layer assemblies, from basic polyelectrolytes and organic small molecules to advanced functional nanoparticles and even polyvalent metal ions [23,24,25]. While most research efforts have traditionally focused on synthetic polyelectrolytes, natural macromolecules such as chitosan, pectin, sodium alginate, and xanthan gum are also promising materials for constructing polyelectrolyte layers. These natural polyelectrolytes exhibit excellent water solubility and are more amenable to cross-linking with other substances, which enhances their adsorption properties and interface stability [26,27,28].
In this study, we developed a method for constructing an antistatic coating on the surface of polyester fibers via LBL self-assembled technology. The LBL self-assembly process involved the sequential deposition of chitosan, a cationic polyelectrolyte, sodium phytate, an anionic polyelectrolyte, and Cu2+ to form a composite coating on the polyester fiber surface. In search of a more feasible and efficient process for the preparation of antistatic polyester fibers, a series of multiple experiments were conducted with different numbers of assembled layers, assembly durations, and concentrations of assembled substances as variables.

2. Materials and Methods

2.1. Materials

Dust-free polyester fiber cloth specimen: 100% low-elastic polyester fiber (75D/36F, straight grain, weave, 110 g/m2) was purchased from Bufan Industrial Co., Ltd. (Dongguan, China), with a smooth surface, firm sealing edge, and no obvious defects. Chitosan (degree of deacetylation ≥ 95%, viscosity 100–200 mPa·s), sodium phytate (99.0%), and copric chloride dihydrate (CuCl2·2H2O, purity 99.9% on a metal basis) were supplied by Shanghai Machlin Biochemical Co., Ltd., Shanghai, China. Hydrochloric acid (36.5–38.0%) was purchased from Nanjing Chemical Reagent Co., Ltd., Nanjing, China. The distilled water utilized in the experiments was produced by a laboratory-grade ultrapure water system (model PLUS-E3-10TH, provided by Nanjing Yipu Yida Technology Development Co., Ltd., Nanjing, China).

2.2. Pre-Treatment of Polyester Fiber Substrate

The polyester fibers were made into samples with sizes of 100 mm × 100 mm × 10 mm, 40 mm × 40 mm × 1 mm, and 15 mm × 15 mm × 1 mm, respectively, which were used for antistatic and surface wettability experiments and characterization. The substrates of the polyester fibers were cleaned twice with deionized water until they were free of dust impurities. Then, they were placed in an oven at 60 °C for drying for 0.5 h, removed, and stored in a desiccator for standby.

2.3. Preparation of the Self-Assembly Solution

The positively charged CS solution was prepared by dissolving CS powder in distilled water. Subsequently, dilute hydrochloric acid was added dropwise into to CS solution and stirred at a constant rate until the pH of the solution was 3. The anionic SP solution was prepared by dissolving SP powder in distilled water, stirring at a constant speed, and gradually adding dilute hydrochloric acid until the pH of the solution was 3. For the Cu2+ solution, CuCl2·2H2O powder was dissolved in distilled water while being continuously stirred.

2.4. Formation of Antistatic Coatings on Polyester Fibers via Layer-by-Layer Self-Assembly

In this experiment, the LBL self-assembly technique was employed, with the mutual adsorption of CS, SP, and Cu2+ resulting in the formation of antistatic coatings on polyester fibers. First, the polyester fiber specimens were impregnated in the CS solution and immersed for a period of time at room temperature and atmospheric pressure. As the surface of the polyester fibers had a negative charge after the surface activation treatment in the early stage, the positive and negative charges [29] were attracted to each other, and the surface of the polyester fibers was successfully loaded with CS polycation layers. After the impregnation, the specimens were removed, cleaned with distilled water, and dried in a drying oven at 50 °C for 0.5 h. At this time, the polyester fibers possessed a positive surface charge. Then, they were impregnated in the SP solution and immersed for a period of time. After the impregnation, the specimen was removed, cleaned with distilled water, and dried in a drying oven at 50℃ for 0.5 h. At this time, the surface of the polyester fibers had a negative charge. Subsequently, the specimens continued to be impregnated in the solution of CuCl2 for some time. Then, the samples were rinsed with distilled water and dried in the oven at 50 °C for another 30 min. One layer of SP and one layer of Cu2+ were considered to comprise a single deposition cycle. After that, the SP and the Cu2+ layers were loaded several times using cyclic loading to ensure the performance effect. The preparation process is schematically shown in Figure 1.
The concentrations of polyelectrolyte and Cu2+ solutions, the soaking time, and the number of layers assembled were taken as variables in the growth control experiments. The original polyester fiber was taken as the control group. Multiple experiments were set up to explore the optimal process conditions or process range for the surface performance improvement in polyester fiber. The concentration of all the assembly substances was set as 1, 5, and 10 g/L. The soaking time was set as 30, 60, and 90 min. Moreover, the number of SP/Cu2+ loading layers were set as 1, 3, and 6. When exploring the effect of a particular variable, all other conditions were kept identical.

2.5. Characterization and Measurements

The surface morphology and elemental composition of the polyester fiber coatings were characterized using scanning electron microscopy (SEM, Quanta 400 FEG, FEI Inc., Eindhoven, The Netherlands) equipped with an energy-dispersive X-ray spectroscopy (EDX) system. Each sample was coated with a 5–10 nm Au layer prior to SEM imaging. A Fourier transform infrared spectroscopy (FT-IR) analysis of the samples was performed using an ALPHA II infrared spectrometer (ALPHA II, Bruker, Fällanden, Switzerland) in the scanning region of 4000~600 cm−1.

2.6. Surface Resistance Test

The surface resistance (R) of the samples (size: 100 × 100 × 10 mm3) was measured at a temperature of 22 °C and 51% humidity using a handheld surface resistivity meter (VC385, Victorlong Instruments, Shenzhen, China). The average value was calculated after every three point measurements. The antistatic effect of the samples was evaluated and analyzed according to the standard AATCC 76-2018 [30] and GB/T 12703.4-2010 [31].

2.7. Water Absorption Performance Test

The water contact angle was measured using a contact angle system (CA, CAST2.0 CA, Solon Information Technology Co., Ltd., Shanghai, China) at room temperature. Distilled water droplets of 5 µL each were employed for the contact angle analysis. To evaluate the change in the contact angle over time, the test solution was continuously dispensed onto the polyester fiber for one minute. Three distinct locations on the sample were measured, and an average was determined. Additionally, the contact angle of the unmodified fiber was measured to serve as a comparative reference.

3. Results and Discussion

3.1. Surface Morphology and Structure Analysis

The surface morphology of the polyester fibers before and after modification was investigated by SEM, as shown in Figure 2a–e. As observed, the surface of the untreated polyester fibers was smooth but with some granular impurities. After a 90 min deposition of CS (1 g/L) and SP (1 g/L), the fibers displayed a more rugged appearance, indicating the formation of a coating wrapping around the surface of the polyester fibers (Figure 2b,c). When a layer of CuCl2 (1 g/L) was deposited on the polyester fiber surface for 90 min, merely a small quantity of particle-like impurities were present (Figure 2d). As it was further deposited up to three layers, the number of particles seemed to pile up and agglomerate. However, the distribution remained uneven (Figure 2e). Following the assembly of six layers, a thick and compact coating appeared on the entire surface of the polyester fiber (Figure 2f,g). As shown in Figure 2h, there are N, P, and Cu elements from CS, SP, and CuCl2 on the coated polyester fiber. The results demonstrate that the CS/SP/Cu2+ coating was successfully formed.
The FT-IR spectra of the above specimen are also shown in Figure 3. The peaks present across the wavelength of 1720 cm−1 to 720 cm−1 were related to the cyclic group in the polyester fiber structure. The characteristic peaks of the polyester fiber became weaker after the application of the CS/SP/Cu2+ coating, indicating that the polyester fiber surface was covered by the self-assembled layer. The diminished peaks in the infrared spectrum provide less information because the typical absorption peaks of the polyester fiber were very strong in this wavenumber range. Additionally, the absorption peaks in the range of 1600–1700 cm−1, corresponding to -OH groups, showed a shift, which may be due to the formation of hydrogen bonds [32,33].

3.2. Analysis of Surface Resistance

The data concerning the effects of varying numbers of assembly layers, assembly durations, and concentrations of the assembly substances influencing the surface resistance of the polyester fibers are summarized in Table 1. The surface resistance of the original polyester fiber exceeded the measurement range of the resistance tester, surpassing 1012 Ω, and thus classifying it as an insulating material. The polyester fibers with a single layer of CS loading exhibited a reduction in surface resistance, which further decreased as the CS concentration increased, ultimately reaching as low as 1010 Ω. This indicated that the loading of CS improved the antistatic property of the polyester fiber. A higher CS concentration means more positively charged ions, creating more conductive channels on the fiber surface that facilitate charge migration and dissipation [34]. However, the addition of SP seemed to have no significant impact on the antistatic property of the polyester fiber. The incorporation of conductive Cu2+ led to a marked decrease in surface resistance, with the reduction continuing as the concentration increased. Under the identical concentration (10 g/L) and number of assembly layers (six layers), the surface resistance of the polyester fiber treated for a 30 min immersion was 108 Ω, which met the basic antistatic requirement for polyester fibers. Extending the immersion time to 90 min further reduced the surface resistance to as low as 106 Ω. It can be observed that a longer immersion duration of the polyelectrolyte and Cu2+ on the polyester fiber leads to a greater reduction in surface resistance and a more pronounced antistatic effect. A similar tendency was also observed with variations in the number of loading layers. An increase in the number of loading layers corresponded to a decrease in surface resistance and an improvement in its antistatic property. The antistatic durability of the modified polyester fiber was further evaluated by washing experiments. According to GB/T 12490-2014 [35], the washing solution was added to a water bath containing stainless steel beads. A sample (10 g/L, 90 min soaking, and six layers) was taken and stirred in the water bath at 40 °C for 30 min. This process was recorded as one washing time. The test sample still maintained an antistatic surface resistivity of about 108 Ω after being washed 10 times.

3.3. Analysis of Surface Wettability

The water absorption data of the modified polyester fibers are revealed through the water contact angle test (Figure 4). An analysis of the experimental data (Figure 4a) shows that the water contact angle of the original polyester fiber was 136°, with no obvious change observed within 60 s. This lack of change is attributed to the synthetic nature of polyester fibers, which feature a dense molecular structure that inhibits water molecule infiltration and absorption. In contrast, the initial water contact angle of the sample loaded with one layer of CS was 133°, but decreased to 52° after 60 s, indicating a notable improvement in its water absorption property. This enhancement is due to the presence of a large number of hydrophilic groups, such as hydroxyl and amino groups, in the CS structure [36]. After loading SP, there was no significant change in the water absorption properties. This result aligns with the surface resistance test findings, indicating that SP did not improve the antistatic effect and mainly served as a bridge to connect CS and Cu2+. However, the introduction of Cu2+ led to a dramatic reduction in the water contact angle from 130° to 0° within 20 s, demonstrating a remarkable improvement in water absorption compared to the previous samples. The CS/SP/Cu2+ coating altered the surface morphology and microstructure of the polyester fiber, facilitating water molecule penetration and absorption [34]. Water absorption performance under different assembly conditions was analyzed, revealing a trend similar to that observed in the surface resistance test. Specifically, a greater number of loading layers within a certain range improved the water absorption effect (Figure 4b). In this experiment, the most effective water absorption was achieved when both the nanoparticle and polyelectrolyte concentrations were 10 g/L (Figure 4c). At this concentration, water was absorbed almost instantly upon contact. Additionally, the water absorption of polyester fibers increased with prolonged treatment time (Figure 4d). It is evident that all polyester fibers treated with CS/SP/Cu2+ exhibited water droplet absorption within 5 s. This finding indicates that the treatment method significantly enhances the water absorption capacity of the polyester fibers, which, in turn, facilitates charge conduction and dissipation, thereby improving the antistatic performance.

4. Conclusions

This study successfully achieved efficient antistatic CS/SP/Cu2+ coatings on polyester fiber surfaces via the LBL self-assembly method. Under various self-assembly conditions, the surface resistance values of the modified polyester fiber samples ranged from 1012 to 106 Ω, meeting the requirements of antistatic materials and demonstrating a good antistatic effect. Generally, both Cu2+ and CS were effective in enhancing the antistatic property. As the number of assembly layers, assembly durations, and the concentration of assembly substances increased, the antistatic performance improved correspondingly. Based on a comprehensive analysis of the test results, the optimal conditions for achieving a superior antistatic property in this experiment are an assembly time of 90 min, an assembly cycle of six layers, and a concentration of 10 g/L. Further washing experiments showed that the modified samples still maintained an antistatic surface resistivity of about 108 Ω after washing 10 times and good antistatic durability.

Author Contributions

Conceptualization, W.W. and J.Z.; methodology, W.W., M.W. and Y.F.; software, Y.L.; validation, W.W., J.Z. and Y.L.; formal analysis, W.W., J.Z. and M.W.; investigation, Y.L.; resources, W.W.; data curation, W.W.; writing—original draft preparation, Y.F., Y.L. and J.Z.; writing—review and editing, W.W. and Y.F.; visualization, J.Z.; supervision, W.W.; project administration, W.W. and Y.F. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Natural Science Foundation of Jiangsu Province (grant number BK20220426) and Natural Science Research of Jiangsu Higher Education Institutions of China (grant number 22KJB220004).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The original contributions presented in the study are included in the article, further inquiries can be directed to the corresponding author.

Acknowledgments

The authors thank the Institute of Chemical Industry of Forest Products for providing invaluable technical assistance in the chemistry laboratory.

Conflicts of Interest

The authors declare no conflicts of interest.

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Coatings 14 01236 g001
Figure 1. Scheme of fabricating CS/SP/Cu2+ coatings on polyester fiber surface by LBL self-assembly.
Figure 1. Scheme of fabricating CS/SP/Cu2+ coatings on polyester fiber surface by LBL self-assembly.
Coatings 14 01236 g001
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Figure 2. SEM images of (a) original polyester fiber, (b) CS-coated polyester fiber, (c) CS/SP-coated polyester fiber, (d) 1 layer of CS/SP/Cu2+-coated polyester fiber, (e) 3 layers of CS/SP/Cu2+-coated polyester fiber, 6 layers of CS/SP/Cu2+-coated polyester fiber at (f) 5000× and (g) 20,000× magnification, and (h) EDS analysis of CS/SP/Cu2+-coated polyester fiber.
Figure 2. SEM images of (a) original polyester fiber, (b) CS-coated polyester fiber, (c) CS/SP-coated polyester fiber, (d) 1 layer of CS/SP/Cu2+-coated polyester fiber, (e) 3 layers of CS/SP/Cu2+-coated polyester fiber, 6 layers of CS/SP/Cu2+-coated polyester fiber at (f) 5000× and (g) 20,000× magnification, and (h) EDS analysis of CS/SP/Cu2+-coated polyester fiber.
Coatings 14 01236 g002
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Figure 3. FT-IR spectroscopy of (a) original, (b) CS-coated, (c) CS/SP-coated, and (d) CS/SP/Cu2+-coated polyester fiber samples.
Figure 3. FT-IR spectroscopy of (a) original, (b) CS-coated, (c) CS/SP-coated, and (d) CS/SP/Cu2+-coated polyester fiber samples.
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Figure 4. The water contact angle data of (a) different LBL self-assembly structures, (b) the numbers of assembly layers, (c) the concentrations, and (d) the assembly durations of the assembly substances affecting the wettability of the polyester fibers.
Figure 4. The water contact angle data of (a) different LBL self-assembly structures, (b) the numbers of assembly layers, (c) the concentrations, and (d) the assembly durations of the assembly substances affecting the wettability of the polyester fibers.
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Table 1. Variation in surface resistance of polyester fibers with different numbers of assembly layers, assembly durations, and concentrations of assembly substances.
Table 1. Variation in surface resistance of polyester fibers with different numbers of assembly layers, assembly durations, and concentrations of assembly substances.
LBL Self-Assembly StructureConcentration
(g/L)		Impregnation Time(min)LayersSurface Resistance
Value (Ω)
CSSPCuCl2
original/////outrange
CS1//9011012
CS5//9011011
CS10//9011010
CS/SP11/9061011
CS/SP55/9061010
CS/SP1010/9061010
CS/SP/Cu2+111906109
CS/SP/Cu2+555906108
CS/SP/Cu2+101010906106
CS/SP/Cu2+101010306108
CS/SP/Cu2+101010606107
CS/SP/Cu2+101010901108
CS/SP/Cu2+101010903107
CS/SP/Cu2+ after washing 10 times101010906108
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MDPI and ACS Style

Wang, W.; Zhang, J.; Liu, Y.; Weng, M.; Fu, Y. Preparation of Antistatic Polyester Fiber via Layer-by-Layer Self-Assembly. Coatings 2024, 14, 1236. https://doi.org/10.3390/coatings14101236

AMA Style

Wang W, Zhang J, Liu Y, Weng M, Fu Y. Preparation of Antistatic Polyester Fiber via Layer-by-Layer Self-Assembly. Coatings. 2024; 14(10):1236. https://doi.org/10.3390/coatings14101236

Chicago/Turabian Style

Wang, Wei, Jialong Zhang, Yifan Liu, Mengyun Weng, and Yanchun Fu. 2024. "Preparation of Antistatic Polyester Fiber via Layer-by-Layer Self-Assembly" Coatings 14, no. 10: 1236. https://doi.org/10.3390/coatings14101236

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