Facile Preparation of Acid-Resistant Polyester Fabrics With Organic/Inorganic Nanocomposites

Abstract

A facile method to prepare acid-resistant fabric with fluoropolymer/silicon dioxide (SiO₂) nanocomposite is presented in this study. Response surface methodology (RSM) was employed to understand the influence factors of the optimized protocol for the acid-resistant fabric. During the preparation process, the effect level of the factors was agent concentration > curing temperature > curing time. The treated fabric showed a remarkable acid repellency, having a contact angle greater than 137°. Additionally, when the fabric was immersed in 80% sulfuric acid (H₂SO₄) for 5 min, it had a 4% and 9% decrease in breaking force in the warp and weft directions, respectively. We believe that the acid-resistant fabric developed as part of this study will receive more opportunities to the application of protective clothing, and the regression analysis provided by RSM can be extended into other procedures for textile preparation.

Keywords

acid-resistant fabric polyester fabrics one-step coating response surface methodology

The demand for comfortable, protective, and healthy fabrics (e.g., those that are ultraviolet (UV)-resistant, antibacterial, and fire retardant) drives researchers to develop newer functional textiles (De, Sankhe, Chaudhari, & Mathur, 2005). Acid-resistant fabric is one of the most important categories of protective textiles, and it can be applied in areas ranging from chemistry and metallurgy to electroplating, among other applications. When considering personal safety, protective apparel, such as acid-resistant clothing, would be desired in order to avoid acid corrosion during the manufacturing, transportation, or utilization of the strong acids.

Currently, most frequently used acid-resistant textiles are prepared by coating hydrocarbon resins or rubber, which can block the gap between fibers and form a continuous resin film (Forsberg, Van den Borre, Henry, & Zeigler, 2014). Still, such fabrics are not comfortable to wear due to the poor air permeability of the resin film. Compared to other protective fabrics, including flame-retardant textiles and UV-resistant apparel, few researchers have studied the fabrication of acid-resistant fabrics (Attia, El Ebissy, & Hassan, 2015; Hu, Gao, Chen, & Chen, 2014; Shahidi & Ghoranneviss, 2016). Corrosive acid solutions are primarily composed of a water-based phase, and consequently, many researchers have applied the hydrophobic mechanism to the acid-proof theory. In the case of acidic solutions, Gal’braikh and coworkers (2005) have demonstrated that low surface energy molecules such as fluorochemicals could effectively offer resistant properties to the corrosive solution while simultaneously repelling water due to the hydrophobicity of specially treated fluorochemicals. However, the standard requirements for protective attire for those who work with acids on a day-to-day basis still cannot be reached if the textile was treated with fluorochemicals only (according to Chinese National Standard GB 24540-2009, Protective clothing—Protective clothing against liquid acid and alkalis).

It has been reported that superhydrophobic surfaces can be achieved by organic/inorganic nanocomposites, which hold low surface energy due to organic polymers and the surface roughness offered by inorganic nanoparticles (Wu et al., 2015; Zhang et al., 2015). For example, Sun et al. (2011) presented an excellent superhydrophobic surface achieved by vinyl groups functioned silica nanoparticles. Cui et al. (2010) reported that fluorinated polyacrylate–silica nanocomposites can offer a stable organic/inorganic nanocoating. Albeit, most researchers mainly focus on the water-repellent property, and only a few have studied corrosion-resistant surfaces related to organic/inorganic nanocomposites. For instance, Hu, Gao, Chen, and Chen (2014) studied the durability, stability, and water-repellent properties of a new material created from polyethylene terephthalate via an acidic aqueous solution with different pH values. Additionally, Li et al. (2010) gave a superhydrophobic surface chemical resistance by applying fluorinated blocks on the cotton fabric. Deng, Wang, Mao, Wang, and Chen (2014) prepared a superhydrophobic fabric through a polydimethylsiloxane (PDMS) coating solution containing TiO₂–SiO₂ nanoparticles, and the obtained fabric was stable at acidic (pH = 2) conditions. Wet chemical coating methods involving the coating of a finishing agent solution via dip-pad-cure process offer a simple, convenient strategy to create superhydrophobic, acid-resistant fabrics (Bellanger, Darmanin, Givenchy, & Guittard, 2014). However, only some advances have been presented in literature that detail the application of wet chemical agents to prepare acid-proof fabric. Recently, Zeng, Wang, Zhou, and Lin (2015) prepared the superhydrophobic cotton fabric with a good repellency against organic solvents and acid solutions (pH = 1) by using fluorinated alkyl silane and silica nanoparticles. Zhou, Wang, Niu, Gestos, and Lin (2013) fabricated the superamphiphobic fabric by a two-step wet chemistry coating of fluorinated nanocomposites. The coated fabrics were durable to strong acid attacks with pH = 1 (Wang et al., 2011). Still, most researchers only report acidic stability at a pH ≥ 1 instead of concentrated acid. For instance, Zou et al. (2013) prepared the solvent-resistant cotton fabric against an acidic solution (pH = 1) by grafting a diblock copolymer on the fabric surface. Yoo, You, Choi, and Lm (2013) reported the solvent resistance of a polyester (PET) fabric coated with a stacked polymer film through initiated chemical vapor deposition, which displayed chemical robustness including H₂SO₄ (pH = 2). Additionally, Zhou et al. (2015) produced a fabric that could withstand a 98% concentrated sulfuric acid and strong alkaline solution by using a coating solution of poly(vinylidene fluoride-co-hexafluoropropylene) and fluoroalkyl silane.

In this work, we employed the fluoropolymer/SiO₂ organic/inorganic nanocomposites as the acid-proof agent to prepare the acid-resistant fabric. Here, the fluoropolymer was used as the organic part, and the nanosilica was used as the inorganic constituent. The chemical agent solution was applied onto the PET fabric by a simple dip-pad-cure procedure. We first used response surface methodology (RSM) to analyze the influence factors (such as agent concentration, curing temperature, and curing time) during the preparation of the acid-proof fabrics, which allowed for a reasonable regression model. The obtained functionalized fabric held excellent acid-resistant properties and water repellency rate. We believe this method can broaden the applications of acid-resistant fabric, while the RSM can be extended to other processes involved in textile industry.

Experimental Method

Materials

Bleached twill woven PET fabric (150 denier [D]/144 filament [f] × 100D/72f) was used as the substrate. The weight per unit area of the fabric was 128 g/m². H₂SO₄ (95–98%), hydrochloric acid (HCl) (36–38%), nitric acid (HNO₃) (65–68%), methyl methacrylate (MMA), butyl acrylate (BA), 2-hydroxyethyl acrylate (HEA), ammonium persulfate (APS), and anionic composite surfactant sodium dodecyl benzenesulfonate (SDBS) were analytical reagents purchased from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China). Nonionic surfactant aliphiatic alcohol polyoxyethylene ether (AEO-9) and dodecafluoroheptyl methacrylate (DFMA) were obtained from Harbin Xeogia Fluorine-Silicon Chemical Co., Ltd. (Hangzhou, Heilongjiang, China).

Acid-Resistant Finish for PET Fabric

The main component of the acid-resistant agent was a fluoropolymer/SiO₂ (organic/inorganic) nanocomposite obtained using a protocol developed by our lab (Xu, Shen, Wang, Ding, & Cai, 2015). First, vinyl silica hydrosols were used as seeds and prepared by a one-step water-based solgel method. Then, the fluorinated acrylic polymer/nanosilica were synthesized by semicontinuous seeded emulsion polymerization. The AEO-9 and SDBS were used as emulsifier, and the BA, MMA, HEA, and fluoroacrylic monomer DFMA were used as acrylate monomers for the synthesis of the fluoropolymer/SiO₂ nanocomposite under the initiator APS, as developed by our former researchers (Xu et al., 2015). The acid-resistant fabric was coated with the organic/inorganic agent by the dip-pad-cured process. For a standard synthesis, the PET fabric was immersed in the fluoropolymer/SiO₂ solution (50 g/L) for 10 min (pH 8–9), then the fabric was padded (Rapid Labortex Co., Ltd., Taipei, Taiwan) through two dips and two nips with a nip pressure of 1 kg/cm². The fabric was then dried at 100°C for 150 s and cured at 170°C in an oven for 120 s. To analyze the impact of the experimental factors on the properties of acid-resistant fabric, we varied the agent concentration from 30 g/L to 110 g/L, optimized the curing temperature from 110°C to 190°C, and then changed the curing time from 60 s to 180 s. The dosage and working conditions of the process were optimized by RSM, from which the functional relationship between the influence factors (concentration of the agent, curing temperature, and curing time) and response values (contact angle [CA] of 80% H₂SO₄) could be built. The RSM was designed with three factors and three levels as shown in Table 1, and the results were analyzed by Design-Expert software (Li, Wang, Wang, & Cai, 2016).

Table 1.

The Response Surface Methodology Design.

Influence Factors	Levels
Influence Factors	−1	0	1
Agent concentration (g/L)	30	50	70
Curing temperature (°C)	130	150	170
Curing time (s)	90	120	150

Characterization

Acid CA was determined on an OCA40 CA system (Dataphysics, Germany) by placing a 10-µl droplet of acid (80% H₂SO₄, 30% HCl, 40% HNO₃, determined according to GB 24540-2009) onto the substrate at ambient temperature. The testing was repeated 5 times for each sample and then the average CA was obtained. The dynamic shedding angle (SA) was measured using a 10-µl acid droplet according to the technique introduced by Zimmermann, Seeger, and Reifler (2009). The spray testing was conducted based on standard AATCC 22-2005. The water repellency rating (WRR) was used to examine the extent of the wetting; the higher rating indicates higher hydrophobicity.

The mechanical property was determined by a universal testing machine (H10K-S, America Tinius Olsen, Horsham, PA) in tensile mode, according to ASTM standard D5035-06 (the standard test method for breaking force and elongation of the textile fabrics strip method). After being immersed in an acid solution (80% H₂SO₄, 30% HCl, and 40% HNO₃) for 5 min and dried at room temperature, the samples were air-conditioned at 25°C ± 2°C and 65% ± 2% relative humidity for 24 hr. Then the samples were stretched at a crosshead speed of 300 ± 10 mm/min to reach a constant strain rate. Five specimens were measured to obtain the average values. The loss in breaking force can be calculated according to the following equation:

D = (\bar{F} a - \bar{F} b) / \bar{F} a \times 100 %,

where D is the decrease in breaking force, $\bar{F} a$ and $\bar{F} b$ represent the average breaking force of the treated fabric before and after the acid contact, respectively. Then, the dissolution of a single yarn under H₂SO₄ (80%) was tested by an optical microscope (E400POL, Nikon, Japan). The thermal stability was characterized by thermal gravimetric (TG) analysis, which was conducted under a nitrogen atmosphere at a heating rate of 10°C/min with a TG209F1 thermogravimetric analyzer (Netzsch Scientific Instruments, Germany).

Results and Discussion

The acid-proof finishing agent was the fluoropolymer/SiO₂ nanocomposite emulsion, which was prepared by semicontinuous seeded emulsion polymerization according to our previous research (Xu, Cai, Shen, Wang, & Ding, 2014; Xu et al., 2015). The acid-resistant fabric was coated with the organic/inorganic agent using a dip-dry technique and subsequently cured under high temperatures. The core–shell structure, element composition of the nanocomposites, and the surface morphology of fabric have been confirmed (Xu et al., 2014, 2015). In this study, we extended the application of the fluoropolymer/SiO₂ nanocomposite to the preparation of acid-resistant fabric. The achievement of acid resistance for the fabric can be attributed to the cooperation of the surface roughness provided by nano-silica, the low surface energy derived from fluoropolymer, and the high chemical stability of the film. During the functionalization process, we took the concentration of the acid-proof agent, curing temperature, and curing time as the main influence factors to optimize working conditions for the preparation.

The surface properties of the nanostructured fabrics depend on the chemical composition of the material. Thus, the fluoropolymer/SiO₂ nanocomposite played an important role in lowering the surface energy. First, we employed the acid CA, SA, and WRR for each acid as the indicator to test the acid-resistant property. Figure 1 shows the acid-proof properties of the treated fabric obtained from the standard protocol, varying the concentration of the nanocomposite from 30 g/L to 110 g/L. As shown in Figure 1a and b, the CAs of the functional fabric were increased and the SAs were decreased with each increment in the acid-proof agent dosage from 30 g/L to 50 g/L, which can be attributed to the better ability of film formation under the higher agent concentration—thus obtaining a lower surface energy. And at the same time, the WRR reached to 95 until 50 g/L (Figure 1c), with only a slight acid droplet observed on the fabric surface. The WRR was maintained at 95, even when the concentration was further increased to 110 g/L, suggesting an inconspicuous influence with the concentration higher than 50 g/L. We then tested the breaking forces of fabrics treated under different concentrations of the acid-proof agent. Both of the breaking forces of warp and weft direction slightly decreased after the acid-proof treatment (Figure 1d), which suggests that the ester bond of PET fiber may be degraded under the high temperature curing.

Figure 1.

Effect of the concentration of acid-proof agent (fluoropolymer/SiO₂ nanocomposites) on the acid contact angle, shedding angle, the breaking force of fabric and fabric water repellency rate. The curing temperature and time were fixed at 170°C for 120 s. The color schemes in (a) also apply to (b).

We also examined the effect of the curing temperature on the properties of acid-resistant fabric. The samples were prepared at temperatures ranging from 110°C to 190°C, with all other conditions kept the same with standard protocol. As shown in Figure 2, the CAs of the three kinds of acid gradually increased and the SAs gradually decreased as the curing temperature was changed from 110°C to 170°C. The WRR changed from 75 to 95, which means that the acid-proof property is impacted by curing temperatures under 170°C. When the temperature was over 170°C, the SA and WRR were no longer improved with the increase in curing temperature. It has been demonstrated in literature that a heating procedure is critical to obtain an optimized repellent effect for fluoropolymers after the wetting procedure, where densely arranged fluorinated layers were formed on the fabric after specific curing processes (Khoddami, Gong, & Ghadimi, 2012; Vedeneeva, Gal’braikh, Redina, Sletkina, & Movchan, 2005). Thus, curing temperature play vital roles during the fabrication process. Higher temperatures are helpful for film formation on the fabric surface. It was demonstrated that increasing curing temperature led to a slight decrease in breaking force (Figure 2d). As a result, we fixed the temperature at 170°C to further study the effect of curing time. Figure 3 shows the impact of curing time on the acid CA, SA, and WRR breaking force, where the curing time was optimized between 60 s and 180 s. The acid CA and SA were gradually improved when the curing time increased from 60 s to 120 s. The curing time had nearly no effect on the fabric breaking force and WRR, as shown in Figure 3. When the time was increased to 180 s, we can observe enhancement in the acid-proof property. From Figures 1 –3, it can be concluded that the acid-resistance properties were exhibited in the following order: H₂SO₄ < HNO₃ < HCl, which was consistent with the corrosivity order of these acidic solutions.

Figure 2.

Effect of curing temperature on the acid contact angle, shedding angle, the breaking force of fabric, and fabric water repellency rate. The agent concentration and curing time were fixed at 50 g/L for 120 s. The color schemes in (a) also apply to (b).

Figure 3.

Effect of curing time on the acid contact angle, shedding angle, the breaking force of fabric, and fabric water repellency rate. The agent concentration and curing temperature were fixed at 50 g/L and 170°C. The color schemes in (a) also apply to (b).

As discussed above, we further optimized the working conditions via RSM. As a main indicator of the anti-acid property, acid CA (80% H₂SO₄) was collected as the response value by RSM. The relevant results were shown in Table 2 and Figure 4. According to the regression analysis by Design-Expert software, a simulation equation was achieved:

CA = 121.325 + 0.0658 A + 0.0600 B + 0.00556 C,

Table 2.

Results of Regression Analysis by Response Surface Methodology.

Coefficient	p Value	Remark
Agent concentration (A)	.0033	**
Curing temperature (B)	.0046	**
Curing time (C)	.4702
Model	.0072	**
Lack of fit	.096
R ²	.95

**Extremely remarkable level: p < .01. *Significant level: p < .05.

Figure 4.

(a) 3-D model graph by response surface methodology. (b) Actual response versus predicted response. The color schemes in (b) also apply to (a).

where A is the concentration of acid-resistant agent; B and C represent the curing temperature and time, respectively. As exhibited in Table 2, both the agent concentration and curing temperature have a p value much less than .05, indicating that these factors strongly affect the CA. On the other hand, the curing time did not obviously affect the CA, which is consistent with the results presented in Figure 3. The lack of fit p > .05 and the correlation coefficient R ² = .95 suggest that the model was reasonable and the regression equation adequately described the influence factors involved in this coating process. Additionally, the effect levels for these factors are agent concentration > curing temperature > curing time. We then focused on agent concentration and curing temperature (fixed curing time at 120 s) to obtain the 3-D model graph. As shown in Figure 4a, the relationship between agent concentration and curing temperature is linearity, and Figure 4b shows the comparison between the predicted and actual responses based on the model equation. This model provides a good explanation of the experimental records, and it successfully compares the correlation between the variables, such as agent concentration and curing temperature. Taking cost and environmental issues into account, the experimental conditions could be optimized to 50 g/L of the acid-proof agent and 170°C of curing temperature for 120 s. The optimized actual value and the calculated value (based on the regression equation) were compared, analyzed, and presented in Table 3. The optimized experimental values are in good agreement with the calculated values, which indicates that the obtained model was effective.

Table 3.

The Comparative Analysis of Optimized Actual Value and Calculated Value.

	Optimal Experiment
Contact angle (°)	Actual Value	Calculated Value	Relative Error
80% H₂SO₄	137.1	135.4	1.24%

To evaluate the acid repellency for the fabrics, we prepared the acid-proof fabric samples under the optimized protocol. Compared to the untreated fabric where the droplet of acid was absorbed rapidly, the acid CAs of the treated fabric were over 137°, SAs reached 9.3°, and WRR was 95 (Table 4), suggesting an excellent acid repellency due to the combination of low surface energy and surface roughness provided by the nanocomposite agent. The wetting property of textile surface by liquid is mainly governed by the surface characteristic and liquid surface tension. We further explored the acid CA of the treated fabric at different pH values (the pH was adjusted by addition of HCl or sodium hydroxide (NaOH) in water). As shown in Figure 5, the liquid CA did not change obviously, because the surface tension of water is essentially constant from pH = 1 to pH = 13 (Beattie et al., 2014). On the other hand, the surface tension decreases significantly (80% H₂SO₄, 66 mN/m) when pH < 0, which is why the CA dropped to 137.1°, as shown in Table 4 (Myhre, Nielsen, & Saastad, 1998).

Table 4.

The Acid-Resistant Property Before and After the Agent Treatment.

Fabric	Contact Angle (°)			Shedding Angle (°)			Water Repellency Rate
Fabric	80% H₂SO₄	40% HNO₃	30% HCl	80% H₂SO₄	40% HNO₃	30% HCl	Water Repellency Rate
Untreated fabric	0	0	0	0	0	0	0
Acid-proof fabric	137.1	139.5	141.2	9.3	10.2	12.3	95

Figure 5.

The effect of pH value on the wetting property of the treated polyester fabric.

We then measured the breaking force before and after immersion in different acid solutions, as shown in Figure 6. For the pristine PET fabric, the breaking force in weft direction decreased 15%, 11%, and 7.5%, after immersion in 80% H₂SO₄, 40% HNO₃, and 30% HCl, respectively. On the other hand, after being treated with the acid-proof agent, the breaking force of the fabric was maintained except for a slight decrease: 9% (80% H₂SO₄), 6% (40% HNO₃), and 4.5% (30% HCl), respectively. The decrease in breaking force in warp direction also shows the same trend as weft direction, suggesting that an excellent acid-resistant fabric was obtained by this coating method.

Figure 6.

The loss of breaking force (%) of the untreated fabric and acid-proof fabric after the immersion in 80% H₂SO₄, 40% HNO₃, and 30% HCl for 5 min. (a) Warp direction and (b) weft direction.

Figure 7 shows the images of untreated and acid-proof treated yarns that were immersed in 80% H₂SO₄ for 10 min. The pristine PET fibers were partially dissolved in the sulfuric acid. In stark contrast, there were minimal changes when the acid-resistant yarn was immersed in H₂SO₄ (80%), indicating an improved acid-resistant property. To further investigate the thermal resistance of the fabrics, TG analysis was performed on each sample. The TG curves of the acid-resistant fabric and the untreated fabric are presented in Figure 8. The remaining weight of resistant fabric was 13.5% after being heated to 900°C, which was higher than that of untreated pristine fabric with a remaining weight of 9.5%. These values can be attributed to the excellent thermal stability of the inorganic nano-SiO₂, which remains after the decomposition of the polymers.

Figure 7.

The status of a single yarn from untreated fabric and acid-resistant fabric, after the immersion in 80% H₂SO₄.

Figure 8.

Thermal gravimetric curves of (a) acid-resistant fabric with the nanocomposites coating and (b) the untreated polyester fabric.

Conclusions

In summary, we developed a simple and robust method for the preparation of acid-resistant fabric by simply coating the fluoropolymer/SiO₂ nanocomposites via a dip-pad-cure method, which is convenient for large-scale production. Agent concentration and curing temperature play important roles during the fabrication of acid-resistant film on the fabric. Compared to untreated fabric, the acid CA, SA, and water repellency rate demonstrate an outstanding acid repellency property. The acid-resistant fabric exhibited a smaller decrease in breaking force after immersion in different acid solutions, which further suggests a true potential for the organic/inorganic nanocomposites to prepare acid-resistant fabrics. Further developments in nanostructured films will play an important role in the fabrication of acid-resistant textiles, which will ultimately increase workplace safety.

Footnotes

Declaration of Conflicting Interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: This work was supported by the Program for Specialized Research Fund for the Doctoral Program of Higher Education in China (No.20130075130002), the National Natural Science Foundation of China (No. 51303022), and the Shanghai Municipal Natural Science Foundation (No. 12ZR1400400). As a PhD student, H.W. was also partially supported by the China Scholarship Council.

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