Protective Textiles against Biological Threats

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This entry is adapted from the peer-reviewed paper 10.3390/polym14081599

The development of protective clothing is crucial nowadays, as there are increased levels of harmful biological threats, both for military forces and civilians.

advanced protection protective textiles biological warfare agents antimicrobial

1. Biological Protective Textiles

The development of protective clothing is crucial nowadays, as there are increased levels of harmful biological threats, both for military forces and civilians ^[1]. The main purpose of barrier textiles is to protect the user against external hazards such as BWAs while maintaining safety and comfort next to the skin ^[2]. Figure 1 illustrates, in a simple manner, the different types of conventional biological protection, namely an impermeable membrane (A), an air-permeable shell layer (B), a semipermeable shell layer (C), and a selectively permeable membrane (D). However, most of the available protective clothing systems rely on passive protection, acting as a full barrier against air, vapors, and liquids, as in hazardous materials (HAZMAT) suits (Figure 1A) ^[1]. Materials that are chemically or mechanically unresponsive to the environment must be engineered to meet performance specifications under worst-case-scenario conditions, often sacrificing performance for the sake of other parameters ^[3]. Air-permeable overgarments are most frequently composed of an activated-carbon layer to adsorb toxic vapors, designed to be worn over battledress duty uniforms (Figure 1B) ^[1]^[2]. Although activated-carbon adsorption material has protective properties, it is limited by a nonselective adsorption, poor protection performance against large toxic liquid droplets, and secondary pollution. Hence, current needs, new materials, and new technologies are acting together to promote the advances of permeable protective suits in pursuit of high performance, multifunctionality, lightweightness, and comfort ^[4]. The development of new protective clothing with different features that can adsorb hazardous agents is envisioned, which can be accomplished by using different fibrous materials and by following a specific design. Selectively permeable fabrics are important to improving the user’s comfort by reducing the airflow through the fabric layers while keeping a high water-vapor permeability ^[4]. As an example, the integration of electrospun nanofiber membranes in textile fibrous structures produces a high aerosol filtration efficiency, good air permeability, low surface density, and low-pressure loss, thanks to the small but highly interconnected pores and large surface area of built nanofibers ^[4]^[5]. In addition, active protection appeared as a promising concept to detect and inactivate/degrade microorganisms and BWAs, while considering that materials capable of responding to their environment may achieve optimal performance under a much wider set of conditions ^[3]^[5]. This can be achieved either by using fibers such as the ones prepared via electrospinning or by functionalizing textiles with nanomaterials that possess those capabilities.

Figure 1. Schematic representation of the different types of conventional biological protection: (A) impermeable membrane; (B) air-permeable shell layer; (C) semipermeable shell layer; (D) selectively permeable membrane (adapted from ^[1]^[2]).

The development of biological protective clothing depends on a combination of different requirements, such as a barrier to liquids, water vapor permeability, and stretch properties. However, it also depends on parameters such as weight and comfort for the wearer, which will ultimately influence the level and durability of the protection. The type of biological threat also impacts this selection and constitutes one of the reasons why the requirements must be established beforehand ^[6].

2. Fibrous Materials

Protective clothing can be achieved through the usage of several different fibrous materials, which are listed in this subsection with regard to the current solutions and the new developments.

3. Fibrous Structures

Different fibrous structures can be developed, and these are presented in this subsection with respect to conventional and active innovative protection.

4. Bioactive Agents

The latest research has directed its efforts at the study of metal–organic frameworks (MOFs); quantum dots; and inorganic particles integrating silver (Ag), copper (Cu), zinc (Zn), and titanium (Ti) cations. Glimpses of the potential of natural polymer chitosan (CS) or derivatives as BWA-counteracting agents, applied as a coating layer or in the form of organic particles (loaded or not with plant-derived compounds such as plant extracts and essential oils (EOs)) can be perceived. Hydrogen-bonded organic frameworks (HOFs), which emerged recently, are also showing high potential to act as self-cleaning materials. The following sections will describe the aforementioned bioactive agents, unveiling the details of their biocidal potential, mechanisms of action, and known limitations.

5. Textile Fabric Functionalization Methods

Textiles can carry microorganisms and also promote their survival, proliferation, and endurance. When a fabric is used for clothing, an infestation may create infections and constitute a biological threat. Antimicrobial functional finishes are therefore applied to textiles to protect the wearer and the fabric itself ^[7]. Various techniques exist to immobilize bioactive agents onto textile fibers, each one carrying its specifications, advantages, and limitations, with the fabric being previously treated and functionalized in order to improve the impregnation of the selected bioactive agents, as well as their durability within the textile. The dip-pad-cure method, the dip-and-dry method, the exhaustion method, the spray-dry method, the spray-cure method, the pad-batch method, and sol-gel and sonochemical coatings are a few relevant examples of the impregnation methods of bioactive agents ^[8]^[9]. However, coating and laminating procedures are increasingly important techniques for adding value to textiles, including coating approaches such as the lick-roll method; direct coating (knife on air, knife over table, knife over roller, knife over rubber blanket); foam coating; foam and crushed-foam coating; transfer coating; kiss-roll coating; rotary-screen printing; spray coating; calendar coating; hot-melt extrusion coating; and rotogravure ^[10].

Starting with MOFs, recent antimicrobial stars, some interesting studies have been performed. The work of Cheung and colleagues ^[11] stands out, as PET textiles had UiO-66-NH₂ MOFs grown in situ following chlorination with a hypochlorite bleach solution to obtain regenerable N–chlorine MOFs coating the textile. The same occurred elsewhere ^[12], but this time ZIF(Ni), ZIF-8(Zn), and ZIF-67(Co) were the MOFs synthesized into cotton fabrics. A silicate modification acted as a crosslinker between cotton on one side and ZIF-MOFs on the other, thereby increasing the number of MOFs adsorbed onto the fabrics. The fabrics were scoured for dirt removal or even bleached for discoloration ^[11]^[12], and sometimes functionalized to gain functional dopamine moieties ^[13] or the previously mentioned silicate modification ^[12] to reinforce binding with the bioactive agents through covalent bridges.

The same trend has been observed with inorganic NPs, with most of the NPs being grown in situ following textile incubation with metallic precursors. Despite their well-known handicaps, Ag NPs continue to be the most studied inorganic NPs in protective textiles, although often in combination with other microbicidal enhancers. Textile functionalization with the bioactive agents occurs mostly via the in situ formation of NPs ^[8]^[14]^[15]^[16]^[17]. As an example, El-Naggar and colleagues ^[8] showed that bleached and mercerized (an alkaline treatment to improve affinity towards subsequent chemical modifications) cotton fabric was rendered more hydrophilic through plasma treatment, then washed with a nonionic detergent to remove impurities and silanized to encourage metal–ligand binding with the Ag NPs. Silanization treatment forms silane groups that act as fiber–NP coupling agents, creating a siloxane bridge between the two components ^[18]. Finally, the treated fabric was immersed in a solution carrying metallic precursors, sonicated, padded, squeezed, and cured for thermal reduction to form Ag NPs. Görgülüer et al. ^[19] washed rayon fabric in an acetic acid solution and in a wet surfactant so that any chemical finishing, such as silicon, and softening on the fabric could be efficiently removed. Afterwards, the fabric was immersed in TiO₂ NPs; poly(dimethylsiloxane) (PDMS) to functionalize the later NPs with hydrophobic moieties; AgNO₃ and NaBH₄ as metallic precursor and reducing agent, respectively; and finally, tetrahydrofuran (THF) to assist in the production of compact and spherical Ag NPs. Samples were ready for characterization following a drying step. While using ZnO NPs to guarantee bacterial cell death in desized and bleached cotton fabrics, Noorian et al. ^[20] also washed the fabric in nonionic detergent, before performing oxidization by periodate and treatment with 4-aminobenzoic acid ligands (PABA). NPs were similarly built in situ after the immersion of the fabric in a ZnO precursor, ultrasonication, and chemical reduction.

The integration of CQDs into cotton fabric that had been scoured, bleached, and cationized with 3–chloro–2–hydroxypropyl trimethyl ammonium chloride (C₆H₁₅Cl₂NO), was indeed very simple ^[21]; it was achieved by dissolving previously prepared CQDs, impregnating the fabric with them while stirring, and drying. The addition of an rGO coating through a dip-dry process onto fabrics composed of cotton or silk ^[15] that had been previously washed with acetone and hot water and functionalized with a silane derivative allowed increased quantities of Ag and Cu NPs to be added subsequent to the composition, particularly with cotton, which is richer in hydroxyl groups than silk.

Botelho and team ^[14] washed PA taffeta and submitted it to plasma treatment. CS was then added through the dip-dry method, followed by the already prepared Ag NPs. Dip-pad-dry was the immobilization technique also selected by Verma et al. ^[22] to integrate dissolved CS, along with citric acid (C₆H₈O₇) to act as a linker to the enzymatically desized and scoured cotton fabric, with sodium hypophosphite (NaPO₂H₂) as the catalyst; this worked as a mordant to enhance the dyeability of the cotton. Samples were then padded, dried, and cured. A final step included a dyeing process with onion-skin dye. Some studies have additionally integrated plant-derived molecules into/onto CS-based small-scale particles ^[23]^[24]^[25]. Singh et al. ^[25] used the emulsification of gelatin and rosemary EO followed by ionic gelation between gelatin and CS to encapsulate the EO and produce a stable shell. Linen fabric was dipped in a microcapsule (MC) dispersion and low-temperature curable acrylic binder, padded, and dried. Verma and colleagues ^[23] encapsulated cinnamon EO within CS MCs produced by simple complexation with Tween 20. Dense taffeta cotton fabrics, which had been desized, bleached, and mercerized, were dipped into an MC dispersion and a binding agent (dimethyloldihydroxyethylene urea, DMDHEU), padded, dried, and cured; they were then autoclaved and stored. In another study, Wang and colleagues ^[26] explored HOFs that carried building units incorporating CH₃-, F-, or NH₂-groups on the ortho-position of the phenyl ring of the benzoic acid and were produced via a sol-gel method. These were spray-coated onto woven and knitted cotton fabric, as well as commercial chirurgical disposable face masks; dried; washed in acetone to remove unbound agent and solvent; and then dried again.

As mentioned above, multiple bioactive agents have been tested with textiles, alone or combined in order to obtain synergistic effects in the fight against pathogens. Many authors are also aware of the need to obtain durable bioactive effects, namely by retaining the bioactive compounds attached to fibers ^[11]^[19]^[26]. It is, however, noticeable that the past two years, during the COVID-19 pandemic situation, have been key for attempts to control the washing durability of finished fabrics, thereby responding to a major concern of the textile finishing industry ^[23]. Some authors have even followed standardized protocols to assess such features (the KS K ISO 6330 ^[15], IS: 3361-979 ^[22], AATCC-61 ^[27], or AATCC 2010 ^[21] standards), thus proving that the required bioactivity is present even after laundering activity. Table 1 summarizes the main, and representative, antimicrobial protective textiles designed for military purposes or for general use.

Table 1. Recent trends (2020–2022) in antimicrobial protective textiles designed for military purposes or for general use.

Fabric		Bioactive Agent	Impregnation Method	AM Testing				Protective Textile	Ref.
Details	Cleaning and/or Pretreatment	Bioactive Agent	Impregnation Method	Cell	Method	Main Results	Durability	Protective Textile	Ref.
Woven and knitted cotton fabric, plus commercial chirurgical disposable face masks	-	HOF-101-R (R=H, CH₃, F, NH₂), obtained by sol-gel method	Spray coating: HOF-101 tecton derivatives (1 mg/mL in DMF) were sprayed on various fiber materials (1 × 1 cm²) for 10 s and dried (100 °C, 1 h). The procedure was repeated enough times until the sprayer was empty. Fibers were washed by acetone 3 times and dried (100 °C, 1 h).	S. aureus, E. coli, K. pneumoniae, and M. marinum	Shake-flask method, under simulated daylight and dark conditions	After illumination under simulated daylight for 2.5 min, the HOF-101-F/fiber killed 95% of E. coli. Following 12 h of solar irradiation and exposure to bacteria for 2 h, cell death was ≈46%. Performance maintained after light irradiation and dark treatments for 5 cycles. Over 99.99% of bacteria was eliminated after daylight treatment for 30 min. Antibacterial performance under complete dark conditions without preirradiation was much slower.	Washed in water without observable HOF loss.	Face masks	^[26]
PET	Scoured in 3% NaOH solution (90 °C, 20 min), then washed with water	Regenerable N-chlorine, loaded into Zr-MOF UiO-66-NH₂	In situ MOF synthesis: PET textile (20 cm × 20 cm), BDC-NH₂ (90 mmol, 16.2 g) and ZrOCl₂·8H₂O (60 mmol, 19.4 g) mixed in water (400 mL) and TFA (200 mL) in a sealed 1 L Schott bottle, sonicated for 0.5 h, placed at 100 °C for 6 h, cooled to RT, washed by water (2 × 500 mL) and acetone (3 × 500 mL), dried at RT, and activated at 110 °C for 24 h under dynamic vacuum.	S. aureus, E. coli, and SARS-CoV-2	Modified AATCC 100–2004 (with textile “sandwiched” using another identical sample for full contact), SEM of harvested bacteria, anti-SARS-CoV-2 virus test	Bacteria: 7-log reduction within 5 min. SARS-CoV-2: 5-log reduction within 15 min.	23% loss in chlorine content after 40 days storage, sealed, under ambient conditions, still enabling total sterilization.	Cloth against BWAs and CWAs	^[11]
100% plain-woven cotton, 185 gm/ m²	Scoured, bleached, then cationized with C₆H₁₅Cl₂NO (50 °C, 2 h)	CQDs clustered from synthesized TM	Dip-dry: 0.25 g of prepared components (TM or CQDs) dissolved in 25 mL of CHCl₃. Fabric (0.25 g) impregnated in 0.25 g of TM or CQDs (1 h, continuous stirring), then air-dried.	S. aureus, E. coli, and C. albicans	Kirby–Bauer disk diffusion technique, MIC determination	82%, 71%, and 62% growth inhibition, respectively, in 24 h.	68%, 63%, and 67% growth inhibition, respectively, after 10 washing cycles.	Military clothing	^[21]
Pristine CNWs fabricated from pulp and lyocell fibers	Drying (90 °C, 5 h) and hydrofobization with CI, plus UV-induced grafting of PTB	PHMG or NEO	Outer layer: grafting of antiviral/antibacterial agents by the ring-opening reaction of the PTB with -NH₂ of PHMG or NEO onto hydrophobic CI-functionalized CNWs. Middle layer: the same onto pristine CNWs.	S. aureus, E. coli, HcoV-229E virus, and SARS-CoV-2 virus	Colony count method and antiviral testing	Bacteria: >99.99%, 99.99 ± 0.01% growth inhibition rate after 10 min of incubation with CNWs-PTB-PHMG. Sars-Cov-2: 16.23 ± 1.69% survival after ~0.1 min with CNWs-PTB-NEO, 99.84% ± 0.14% after 30 min with CNWs-PTB-PHMG.	-	Face masks	^[28]
100% plain-weave cotton fabric: 80 ends/inch, 75 picks/inch, and 168 (g/m²)	Scoured, bleached, and C₈H₁₁NO₂-modified (immersion in C₈H₁₁NO₂.HCl solution at pH 8.5, 24 h)	Ag NPs	Dip-dry: immersion in 10 mM AgNO₃ (continuous stirring, 30 °C, 8 h) and vacuum-drying (12 h, 40 °C).	S. aureus and E. coli	ASTM E2149-01	Bacterial reduction of 86% for S. aureus and 93% for E. coli following 1 h of incubation, 100% after 24 h.	~98% bacterial reduction after 20 washes.	Functional textiles	^[17]
Woven viscose (120 g/m²)	Fabric phosphorylation: immersion in DAPH at a molar ratio of 1:1; urea was also included as 3 equiv of DAHP, then rinse with water	ZPT	Dip-pad-dry: padding with 0.5 wt % aqueous solution of N₂O₆Zn·6H₂O via the 2-dip-2-nip method. Then, water-soluble NaZPT was added at a molar ratio of 1:2 with respect to the metal precursor. Immersion in a ZPT ligand solution (2 h, 40 °C, orbital shaking at 120 rpm). Drying (80 °C, 10 min), curing (150 °C, 2 min), and rinsing with water.	S. aureus, E. coli, and C. albicans	Qualitative Kirby−Bauer disk diffusion method; quantitative AATCC-100, OD600, and bacteria survival (CFU) measurement methods; SEM and quantitative antifungal assay	Viscose-ZPT induced high ZoI (48 or 53 mm, respectively, against S. aureus or E. coli).	Viscose-ZPT induced high ZoI after 20 washes (38 or 43 mm, respectively, against S. aureus or E. coli). 96–97% growth inhibition (20 washes).	Protective clothing	^[27]
100% cotton or silk	Acetone and hot water (60 °C) washed; air-dried; soaking in coupling-agent solution (pH 4–5, C₉H₂₀O₅Si:water = 1:15) for 4 h at 60 °C; air-dried	rGO and Ag/Cu NPs	Immersion in 0.25 mg/mL rGO suspension (RT, 4 h), air drying (3 times), separately soaked in 0.05 M AgNO₃ and CuSO₄·5H₂O solutions (2 h), air-dried, immersion in 2% wt/V Na₂S₂O₄ solution (chemical reduction, 4 h, 80 °C, 100 rpm), washed in water, dried (hotplate at 60 °C), and heat-treated in a vacuum oven (20 min, 175 °C).	S. aureus, E. coli, P. aeruginosa, and C. albicans	CFU counts	69–99% (S. aureus), 92–100% (E. coli), and 97–100% (P. aeruginosa) growth inhibition, especially with Ag NPs after 24 h; 63–69% C. albicans growth inhibition with Cu NPs (50% with Ag NPs), namely using cotton.	85−99% growth inhibition against Gram-negative bacteria; 62 to 90% against S. aureus after 10 washing cycles.	Protective clothing	^[15]
Woven cotton fabric (areal mass density: 280 g/m²; threads/cm: warp 48 ± 2; weft 37 ± 1; and CIE whiteness 80)	Desized, bleached, and mercerized	CS MCs, prepared by simple emulsion (with Tween 20) and loaded with cinnamon bark EO	Immersed in MCs (80 g/L) and the binding agent (40 g/L, DMDHEU), padded (wet pick up of 80%), dried (90 °C, 15 min), cured (150 °C, 5 min), autoclave-sterilized, and stored at RT.	S. aureus and E. coli	Diffusion assay method	90% (S. aureus) and 97% (E. coli) growth inhibition.	69% MC remaining after 5 washes, 12.5% after 10 washes.	Protective textiles	^[23]
100% cotton knitted fabric (194 g/m²) with (1 x 1) interlock structure	Cleaned with acetone and water, mercerized	Ag NPs	Immersed into a solution of C₆H₈O₆ (5 min), dried (5 min, 80 °C); immersed into AgNO₃ solution (5 min), dried (5 min, 80 °C); 1–3 cycles. Encapsulation in a silicone binder solution in acetone at a ratio of 1:7 for 5 min (1 time), dried (10 min, 80 °C).	S. aureus and E. coli	AATCC 147, agar diffusion assay	Higher ZoI for 1-cycle samples after 24 h (0.531 mm with S. aureus, 0.25 mm with E. coli).	-	Protective textiles	^[16]
Woven cotton fabric	Enzymatic desizing and scouring	CS and onion-skin dye	Dip-pad-dry: dip within CS (4%), C₆H₈O₇ (6%), and NaH₂PO₂ (5%) at 1:30 material:liquor ratio (pH 5, 90 °C, 45 min), pad (P = 2 kg/cm, expression of 70–75%), dry (100 °C, 5 min), and cure (140 °C, 4 min). Dyeing with onion-skin dye (exhaustion method): 6% dye, pH 5.5, 90 °C, 75 min, 1:30 material:liquor ratio.	S. aureus and E. coli	AATCC Test Method100, shake-flask	S. aureus (98.03%) and E. coli (97.20%) growth reduction after 24 h.	Reduction in S. aureus growth from 96.84 to 80.14% and E. Coli from 93.20 to 80.74% after 5–20 washing cycles.	Protective textiles	^[22]
Rayon fabric	Acetic acid (3 g/L) and TEGO^® wet surfactant (2 g/L) (Evonik) solution in DW (pH 3.5, 20 min), oven-drying	TiO_2, Ag NPs	Dip-dry: immersion in coating mixture (60 mL of 5% TiO₂ NPs + 9.7 mL PDMS + 8 mL of 1 M AgNO₃ + 10 mL 0.017 M NaBH₄ + 30 mL THF) 10 min, drying (70 °C, 4 h).	S. aureus and E. coli	Agar diffusion assay	ZoI of 14.44 mm (S. aureus) and 13.12 mm (E. coli) after 24 h.	Water contact angle remained nearly constant (152.3°) after 20 laundering cycles.	Multifunctional textiles	^[19]
Polyamide taffeta (52 warp and 32 weft yarns, 100 g/m²)	Washing, plasma treatment (RT, atmospheric pressure, width of 50 cm, gap distance of 3 mm, 10 kV, 40 Hz, 5 times, both sides)	Ag NPs, CS	Dip-dry: dip in each solution (5 min, RT) and dry (50 °C, 20 min).	S. aureus and P. aeruginosa	ASTM-E2149-01, shake-flask	S. aureus (80%) and P. aeruginosa (60%) growth reduction after 2 h.	-	Face masks	^[14]
Bleached and mercerized cotton fabric	O₂ plasma treatment (13.56 MHz, 3 min, 400 W, 200 cm³/min, 0.003 mbar); washing with nonionic detergent (C₃₂H₆₆O₉, 10 mmol); sonication (30 min); air-drying and washing with water; dipping in acetone solution of C₉H₂₂O₃SSi (1%, 24 h); curing (75 °C, 30 min); rinsing with water	Ag NPs	In situ synthesis of Ag NPs: dip in 0.1–4 wt % CH₃AgNO₂, sonication (15 min), padding, squeezing, and curing (130 °C, 5 min).	S. aureus, E. coli, and C. albicans	Agar diffusion assay	Clear and large ZoI after 24–48 h.	-	Multifunctional textiles	^[8]
Plain cotton fabric (135 g/m²)	Immersion in 4 mg/mL C₈H₁₁NO₂. HCl (pH 8.5)	ZIF-8	Immersion in Zn(NO₃)₂.6H₂O (0.893 g, 15 mL) solution + C₄H₆N₂ (0.985 g, 15 mL) solution, autoclaving (100 °C, 12 h), washing, and drying (60 °C).	E. coli	Disc diffusion method	Defined ZoI after 24 h.	-	Multifunctional textiles	^[13]
Cotton fabrics (shibeka, honeycomb, and crepe)	Bleached	CS or Ag NPs	Dip-dry: immersion in CS solution (10 min), squeezing for 100% wet pickup (constant pressure), drying (80 °C, 4 min), and curing (140 °C, 2 min); immersion in Ag NP dispersion (100–300 ppm), squeezing for 100% wet pickup (constant pressure), drying (80 °C, 3 min), and curing (140 °C, 2 min).	S. aureus, P. aeruginosa, C. albicans, and A. niger	Disc diffusion method	20 or 13 (S. aureus), 15 or 11 (P. aeruginosa), 13 or 21 (C. albicans), and 12 or 11 mm (A. niger) with 6% CS (Crepe) or 300 ppm Ag NPs (Shebika), respectively, after 24 h.	-	Protective textiles	^[29]
Desized and bleached cotton fabric (100% cellulose, 117.5 g/m²)	Washed (30 min, 50 °C, nonionic detergent Adrasil HP P-836, 1 g/L, 1:60 L:G), water-rinsed, dried at RT; periodate oxidation in phosphate buffer (pH 8, L:G 1:50, dark), addition of NaIO₄ (5 g/L, 30 min, ultrasonication at 20 kHz, 750 W at 70% efficiency), water-washed, dried at RT; PABA treatment (10 g/L, 2 h) using acetate buffer solution (pH 5.5, ultrasonication), water-washed, dried at RT	ZnO NPs	In situ synthesis of ZnO NPs: immersion in 1 mM ZnCl₂ solution (30 min) and ultrasonication (pH 10 for 30 min by adding 4 g/L NaOH). Ultrasonication (extra 30 min, 60 °C), water washing, and drying (120 min, 110 °C).	S. aureus and E. coli	AATCC 100-2004, 24 h	99.9% (S. aureus) and 99.4% (E. coli) growth inhibition.	93.7% or 95.3% (S. aureus) and 93.4% or 95.4% (E. coli) after abrasion or washing process, respectively.	Protective textiles	^[20]
Scoured and bleached plain-woven 100% cotton fabrics (165 gm/m²)	Silicate modification: immersion in 100 mL of 5% NaOH (50 °C, 5 h, stirring), addition of 6 mL C₃H₅ClO (5 h reaction), water and anhydrous ethanol washing, drying (60 °C); silicate mixture synthesized by dropwise addition of SiC₈H₂₀O₄ (12 mL) and methanol (80 mL) to a flask with 30 mL of ammonia and 320 mL of methanol; stirring 3 h, curing (110 °C, 1 h)	ZIF(Ni), ZIF-8(Zn), and ZIF- 67(Co) MOFs	In situ synthesis of MOFs: immersion, separately, in 50 mL of methanol with metal salts (0.736 g of Ni(NO₃)₂, 0.758 g of Zn(NO₃)₂, and 0.733 g of Co(NO₃)₂), stirring 1 h at RT; pour three solutions individually from C₄H₆N₂ (1.623 g in 50 mL of methanol) above the three mixtures, stir 8 h; ethanol-wash and dried (vacuum, 60 °C, 12 h).	S. aureus, B. cereus, E. coli, and C. albicans	Kirby−Bauer disk diffusion method, overnight	ZoI: 25 (S. aureus), 23 (B. cereus), 15 (E. coli), 22 (C. albicans) for cotton–silicate–ZIF(Ni).	ZoI: 19 (S. aureus), 18 (B. cereus), 12 (E. coli), 18 (C. albicans) for cotton–silicate–ZIF(Ni) after 5 washing cycles.	Protective textiles	^[12]
Inner layer: polystyrene fiber 3-ply twisted yarns (tex: 0.058, 0.115, or 0.230); outer layer: 3-ply twisted single yarns with PCMs, including use of functional fibers Resistex^® Silver	Washed with 2.5 g/L nonionic detergent Felosan RG-N, 2.0 g/L Na₂CO₃, 3.0 g/L water softener CalgonVR Power (60 °C, 60 min), rinsed with 1 g/L acetic acid solution, centrifuged, air-dried	Silver	None	S. aureus, E. coli, and K. pneumoniae	EN ISO 20645	Low bacterial growth.	-	Multifunctional socks	^[30]

PET: poly(ethylene terephthalate);TFA: trifluoroacetic acid; RT: room temperature; AATCC (American Association of Textile Chemists and Colorists); TM: 4–(2,4–dichlorophenyl)–6–oxo–2–thioxohexahydropyrimidine–5–carbonitrile; MIC: minimum inhibitory concentration; CNWs: cellulose nonwovens; CI: cyclohexyl isocyanate; UV: ultraviolet; PTB: poly(thiiran-2-yl methyl methacrylate-2-(4-benzoyl phenoxy)ethyl methacrylate; PHMG: polyhexamethyleneguanidine; NEO: neomycin sulfate; DAPH: diammonium hydrogen phosphate; ZPT: zinc pyrithione; ZoI: zone of inhibition; CFU: colony-forming units; DMDHEU: dimethyloldihydroxyethylene urea; ZIF-8: zeolite imidazole skeleton-8; PABA: 4-aminobenzoic acid ligand; L:G: liquor-to-fabric ratio; PCMs: phase-change materials.

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