Multifunctional,Hydrophobic and Flame-retarded Cotton Fabrics Modified with Liner Piperzine/Phosphorous/Polysiloxane Copolymer

α,ω-di[(4-butoxy-piperazin-1-yl)-phosphinic acid methyl ether]-terminated linear polysiloxane (PNPDMS) was synthesized and utilized as the flame retardant and hydrophobing agent. The flame retardance and thermal decomposition behaviors of cotton fabrics were systematically estimated by limiting oxygen index (LOI), thermogravimetric analysis and vertical burning test, respectively. It was found that the LOI of cotton fabric treated with PNPDMS enhanced to 29.82 % compared with cotton fabric without treatment, whose LOI was only 18.00 %. The treated cotton fabric showed a shorter char length, a shorter After-flame time, and no After-glow time as revealed in vertical burning test. The mechanical property in treated cotton fabric was slightly decrease. Furthermore, the grade of water repellency of treated cotton fabric reached to 90 and water contact angle (WCA) increased to 141.90° compared with cotton fabric without treatment whose WCA was 62.80°. The result showed that the cotton fabric treated with PNPDMS exhibited excellent flame retardance and hydrophobic properties.     

Flame retardant properties of triazine phosphonates derivative with cotton fabric

The flame retardant behavior of cotton fabric treated with phosphorus-nitrogen containing triazine compound was evaluated. It was found that cyanuric chloride (2,4,6-trichloro-1,3,5-triazine) is an excellent starting material for the preparation of phosphonate flame retardants that interact well with cotton to improve flame resistance (FR) performance. Tetraethyl 6-chloro-1,3,5-triazine-2,4-diyldiphosphonate (TECTDP) has been prepared by a simple one-step reaction in high yield (98.0 %). Cotton fabrics treated with TECTDP result in covalent bond formation between TECTDP and hydroxyl groups in cotton fabrics. This FR system provides an efficient flame retardant for cotton textiles at low cost to meet government mandates. In this study, the FR material was synthesized and characterized by ¹H and ¹³C nuclear magnetic resonance (NMR), and LC-MS spectroscopy. The chemical structure of cotton twill fabric treated with TECTDP by pad-dry-cure method was analyzed by FT-MIR and SEM. Furthermore, the thermal and flammability properties were evaluated by thermogravimetric analysis (TGA), limiting oxygen index (LOI, ASTM D-2863-09), and a vertical flame test (ASTM D-6413-08).     

Development of UV Protective,Superhydrophobic and Antibacterial Textiles Using ZnO and TiO<Subscript>2</Subscript> Nanoparticles

In this research work, multifunctional cotton fabric comprising of UV protection, superhydrophobicity and antibacterial activity has been developed using facile pad-dry-cure method. In the first step, the concentration of repellent chemical has been optimized. Then, formulations containing nanoparticles of ZnO or TiO₂ along with optimized concentration of repellent chemical and organic-inorganic binder have been applied to cotton fabric followed by the evaluation of functional properties. The surface morphology and elemental composition of treated fabric has been characterized through SEM and EDX, respectively. The treated samples have shown promising UV protection, superhydrophobicity and antibacterial properties durable upto 20 washing cycles.     

Effect of nano SrTiO3 supporting nano TiO2 on self-cleaning of cotton fabric

This study reports the results of an investigation aiming at finding what affect nano titania (TiO₂) and nano strontium titanate (SrTiO₃) on self-cleaning of cotton fabrics. The photocatalytic activity of nano strontium titanate has been examined on cotton fabric under UV irradiation in various concentrations in mixing of nano titania. The amount of loaded nano titania and nano strontium titanate particles on cotton fabrics were investigated using X-ray fluorescence spectrometry (XRF) and crystallinity of coatings by X-ray diffraction spectroscopy (XRD). The treated cotton fabrics, which were stained with two common synthesized dyes, were exposed to 400 W UV radiation for 30 hours and their self-cleaning property was investigated by a reflectance spectrophotometer. Scanning electron microscope (SEM) images show pervasion of nano materials on the surface of the treated cotton. Adding nano strontium titanate to nano titania showed the most promising photocatalytic activity toward dye degradation.     

A Novel Green Stabilization of TiO<Subscript>2</Subscript> Nanoparticles onto Cotton

Facile embedding of TiO₂ nanoparticles onto cotton fabric has been successfully attained by ultraviolet light irradiations. The adhesion of nanoparticles with fibre surface, tensile behaviour and physicochemical changes before and after ultraviolet treatment were investigated by scanning electron microscopy, energy dispersive X-ray and inductive couple plasma-atomic emission spectroscopy. Experimental variables i.e. dosage of TiO₂ nanoparticles, temperature of the system and time of ultraviolet irradiations were optimised by central composite design and response surface methodology. Moreover, two different mathematical models were developed for incorporated TiO₂ onto cotton and tensile strength of cotton after ultraviolet treatment and used further to testify the obtained results. Self-clean fabric through a synergistic combination of cotton with highly photo active TiO₂ nanoparticles was produced. Stability against ultraviolet irradiations and self-cleaning properties of the produced fabric were evaluated.     

Preparation and characterization of intumescent flame retardant biodegradable poly(lactic acid) nanocomposites based on sulfamic acid intercalated layered double hydroxides

A novel sulfamic acid intercalated MgAl-LDH (SA-LDH) was prepared by intercalating NH₃SO₃^? into MgAl-layered double hydroxides (LDH), and it was then introduced into poly(lactic acid) (PLA) resin in association with intumescent flame retardant (IFR) by melt blending to prepare a flame-retardant biodegradable PLA composite. The effects of SA-LDH on the flame retardancy of PLA composites were characterized by limiting oxygen index (LOI), vertical burning test (UL-94) and cone calorimeter test (CONE). The results showed that the composite sample containing 19.0 wt% IFR and 1.0 wt% SA-LDH achieved the maximal LOI value of 48.7 %, passed the UL-94 V-0 rating, and significantly decreased the peak heat release rate from 306.3 kW/m² of neat PLA to 58.1 kW/m². Thermogravimetric analysis showed that both the thermal stability and the char formation were enhanced. The char morphology observation revealed that SA-LDH was beneficial to form dense and compact char layers. It was demonstrated that there existed a synergistic effect between IFR and SA-LDH in promoting the char formation and enhancing the fire resistance. The mechanical and crystallization properties were also tested and discussed.     

Robust Water-Repellent Treatment of Cotton Fabrics with Polysiloxane Modified via Thiol-Ene Click Reaction

A facile and inexpensive way to prepare self-crosslinkable poly(dimethylsiloxane) (PDMS) for superhydrophobic treatment of cotton fabrics is reported in the study. Through thiol-ene click reaction between mercaptopropyltrimethoxysilane (MPTMOS) and vinyl-containing poly(dimethylsiloxane) (VPDMS), PDMS-g-TMOS can be simply and quickly synthesized. The trimethoxysilane group of PDMS-g-TMOS can react with hydroxyl group on cotton fabric and other -Si(OCH₃)₃ groups. The synthesized polysiloxane (PDMS-g-TMOS) was identified by FT-IR and ¹H-NMR. The morphology of the treated cotton fabric was observed by SEM and XPS was used to analyze the elemental composition on the surface of cotton fabric. The analysis results indicated that the surface was fully covered with PDMS. Due to the low surface energy of PDMS and the rough surfaces of cotton fabric, the optimized water contact angle (WCA) and sliding angle were respectively 154°±0.4° and 14°±0.5°, indicating superhydrophobicity. Moreover, water spray test (AATCC Test Method 22-2010) was also applied to evaluate the water repellency of treated cotton fabric and a score of 90 was assigned according to AATCC Test Method 22-2010. The durability of treated cotton fabric was tested by 50 laundering cycles. The resultant WCA barely decreased and the score of water spray test dropped from 90 to 80, showing the reasonable wash durability.     

Properties of flame-retardant cellulose fibers with ionic liquid

Flame-retardant cellulose fibers were prepared by dissolving cellulose in tetrabutylammonium acetate and dimethyl sulfoxide, and blending with amino silicone oil (ASO). The ASO was used as a novel fabric softener and flame retardant for cellulose fibers. Fourier-transform infrared spectroscopy showed that blending with ASO did not adversely affect the cellulose fibers. The flame retardancy of the cellulose fibers blended with ASO was determined based on the limiting oxygen index (LOI). Cellulose fibers blended with 8 wt% (add-on) ASO gave the best flame retardancy, with an LOI of 28, which was higher than that of the virgin fibers. The thermal properties of the flame-retardant cellulose fibers were investigated using differential scanning calorimetry and thermogravimetric analysis. The results showed that ASO prevented degradation of the cellulose fibers, hindered the formation of volatile species, and favored char formation. The mechanical properties of the flame-retardant cellulose fibers were better than those of virgin cellulose fibers.     

Highly flame retardancy of cotton fabrics with a novel phosphorus/nitrogen/silicon flame-retardant treating system

A novel reactive flame retardant (FR) containing phosphorus, nitrogen, and silicon was synthesized successfully, and its chemical structure was fully characterized by Fourier transform infrared spectrometry and nuclear magnetic resonance spectrometry (¹H-NMR and ³¹P-NMR). Then it was used to impart flame resistance to cotton fabrics. Vertical flammability and limiting oxygen index test were used to evaluate the flame retardancy of the cotton fabrics treated with FR. When the cotton treated with 150 g/l FR and 50 g/l sodium hypophosphite, the finished cotton can pass the vertical flammability test. Thermogravimetry (TG) was used to evaluate thermal behavior of FR and cotton fabrics. TG results demonstrated that the FR has good thermostability and char-forming ability. After treatment with FR, the thermal stability of the cotton fabrics was clearly improved, indicating that the FR can protect cotton fabric from fire to a certain degree. Furthermore, attenuated total reflection Fourier transform infrared spectroscopy was utilized to characterize the chemical structure of FR treated cotton fabrics. Finally, the surface morphology in different regions of the treated cotton was observed using scanning electron microscopy.     

Properties of basic dyes on polyacrylonitrile treated m-aramid fabrics

Treatment of polyacrylonitrile (PAN) onto m-aramid fabric was carried out by pad-dry-cure method using dimethylformamide (DMF) dissolved acrylic fiber solution. The obtained PAN treated m-aramid fabric was dyed using exhaustion method with basic dyes. The effect of PAN treatment on fabric stiffness property was acceptable with acrylic fiber solutions ranging from 1 wt% to 4 wt%. Whilst, more than 4 wt% PAN treated fabrics exhibited undesirable stiffness. The dyeing results showed that PAN treated m-aramid fabrics exhibited a significant increase in color strength when compared to untreated fabric, arising from an increase in anionic dye sites (styrene SO₃ ^? group). Wash fastness was comparable to that of untreated fabric, indicating the strong interaction between dye molecules and the PAN. Rubbing fastness of treated fabrics was not affected by treatments with PAN concentrations lower than 4 wt%. Further increase in PAN concentration led to poorer rubbing fastness property due to the problem of surface dyeing. For light fastness, the PAN treatment failed to improve the light fastness property which is the main disadvantage of basic dyeing of aramid fabric. Finally, in case of PAN treatments with the range of 1 wt% to 4 wt%, the flame retardancy property of PAN treated m-aramid fabrics was found not affected by the percent add-on. However, above 4 wt% PAN treatment, the flame retardancy performance became deteriorated.     

Preparation of PET using homogeneous catalysts. II. Effect of BHPP, NPG and PD in Sb2O3 glycol solution catalysts

In the polycondensation reaction of polyethyleneterephthalate(PET), Sb₂O₃ can react effectively as a catalyst, if physically transformed. Sb₂O₃ powder is transformed into liquid solution by dissolving in ethylene glycol(EG). Homogeneous catalyst is made by mixing this liquid solution with glycols having different solubility. The efficient reaction of PET polymerization is expected by using homogeneous catalyst. PET was synthesized using homogeneous catalysts of 4 wt.% Sb₂O₃ solution dissolved in glycol[EG, 2,2-bis(4-(2-hydroxyethoxy)phenol)propane(BHPP), neopentyl glycol(NPG), and 1,3-propandiol(PD)]. PET using EG-BHPP(Sb₂O₃) catalysts shows the highest I.V. within a reaction time of 120 min. In the p-d analysis, PET using EG-BHPP(Sb₂O₃) catalysts has the fastest propagation rate and slowest degradation rate. EG-BHPP(Sb₂O₃) catalysts are more efficient than EG(Sb₂O₃) catalysts and Sb₂O₃ powder catalysts.     

Preparation of electroconductive,magnetic, antibacterial,and ultraviolet-blocking cotton fabric using reduced graphene oxide nanosheets and magnetite nanoparticles

The main goal of present study was the fabrication of cotton fabric with special functions, including electrical conductivity, magnetic, antibacterial, and ultraviolet (UV) blocking. In this regard, the cotton fabric was primarily coated with graphene oxide and then reduction of graphene oxide and synthesis of magnetite nanoparticles accomplished in one step. The alkaline hydrolysis of magnetite precursors and reduction of graphene oxide was simultaneously performed using sodium hydroxide to produce reduced graphene oxide/Fe₃O₄ nanocomposite on the fabric surface. The prepared cotton fabrics were characterized with field emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). The treated fabrics with reduced graphene oxide/Fe₃O₄ nanocomposite displayed a low electrical resistivity i.e. 80 kΩ/sq. Furthermore, the coated fabrics showed reasonable magnetic properties due to the presence of magnetite nanoparticles on the surface of cotton fabrics. Moreover, this process imparted proper antibacterial properties and UV blocking activity to cotton samples.     

Durable multifunctional properties on acrylic fabric using nano TiO2 and polysiloxane

Producing fabric with multifunctional properties has been recently a center of research and utilizing nanoparticles is an efficient approach to gain this purpose. Here, nano TiO₂ photo catalyst and polysiloxane softener were utilized as stabilizer on the acrylic fabric to obtain soft handle, hydrophilic, and self-cleaning features on the fabric. The effect of various concentrations of nano TiO₂ and polysiloxane on the fabric handle, water droplet absorption time, and self-cleaning properties of the fabric has been mathematically modeled based on the response surface methodology (RSM). The optimized treatment conditions indicated that treated acrylic fabric with 2.19 % polysiloxane and 0.68 % nano TiO₂ produced the rigidity of 26.8 g.cm, water absorption time of 15.8 s and self-cleaning of ΔE _T *=18.1. Also increasing the concentration of polysiloxane enhanced both wettability and photoactive properties of nano TiO₂ treated acrylic fabrics. Further, the nano TiO₂/polysiloxane treated acrylic fabrics is significantly enable to absorb the light with wavelength lower than 400 nm and improve discoloration of C.I. Reactive Yellow 1.     

Synthesis and Application of Phosphorus-containing Flame Retardant Plasticizer for Polyvinyl Chloride

A novel phosphorus-containing flame retardant plasticizer (PFRP) derived from castor oil acid methyl ester (COME) was synthesized to substitute dioctyl phthalate (DOP) for plasticizing polyvinyl chloride (PVC) products. The chemical structures of PFRP were confirmed by fourier transform infrared spectroscopy (FTIR) and ¹H nuclear magnetic resonance (¹H NMR). Meanwhile, the plasticizing effect, flammability and thermal stability of plasticized PVC films were investigated by dynamic mechanical analyzer (DMA), limiting oxygen index (LOI) test, scanning electron microscope (SEM) and thermogravimetric analysis (TGA). As the PFRP content increasing from 0 wt% to 50 wt% amount of plasticizers, the plasticizing efficiency and the mechanical properties showed a slightly decreasing tendency compared with that of DOP, while the LOI value of plasticized PVC increased remarkably from 21.5 % to 25.2 %, showing a combined plasticizing efficiency and flame retardancy. SEM and TGA analysis indicated that PFRP had little effect on thermal stability but was effective to promote the formation of compact carbon residue.     

Self-cleaning Properties of Nylon 6 Fabrics Treated with Corona and TiO<Subscript>2</Subscript> Nanoparticles under Both Ultraviolet and Daylight Irradiations

Nylon 6 fabric with self-cleaning properties was prepared by corona discharge pre-treatment and coating with TiO₂ nanoparticles (NPs) using pad-dry-cure technique. The self-cleaning property was studied by discoloration of methylene blue (MB), ketchup, tea and coffee stains from the corona+TiO₂ treated nylon-6 fabric. Color difference (ΔΕ*), reflectance (R) and K/S of MB stain were investigated by diffuse reflectance spectrophotometry. The MB stain was almost completely removed from the corona+TiO₂ treated nylon surface after 24 h under UV light/daylight irradiation. Both of these phenomena (corona and TiO₂) led to an increase in the discoloration of stains under UV and daylight irradiations. The EDS analysis showed an increase in the concentration of deposited TiO₂ NPs coating after corona treatment. The FE-SEM images revealed that the surface of nylon 6 was coarser after the corona treatment. Also, the FE-SEM micrographs exhibited that a uniform layer of TiO₂ NPs was formed on the corona treated nylon fabric. The corona+TiO₂ treated nylon illustrated antibacterial activity against E. coli and B. subtillis microorganisms. The EDS and FE-SEM analysis confirmed that after 5 washing cycles, the amount of TiO₂ NPs was higher on the surface of corona+TiO₂ treated nylon than that of the fabric only treated with TiO₂ without corona pretreatment. This result justifies that the corona+TiO₂ treated nylon fabric with appropriate self-cleaning property can be applied cost-effectively in the textile industry.     

Synthesis of cationic core-shell fluorine-containing polyacrylate soap-free latex and its application on cotton substrate

Fluorinated polyacrylate latexes are preferably potential materials for use in the textile finishing due to their special surface property and especially economical, low-toxic characteristics compared to fluorinated polyacrylate solutions. A novel cationic fluorine-containing polyacrylate soap-free latex (CFMBD) with core-shell structure was accordingly developed by co-polymerizing dodecafluoroheptyl methacrylate (DFMA), methyl methacrylate (MMA), butyl acrylate (BA), and dimethylaminoethyl methacrylate (DM) using a cationic reactive emulsifier, maleic acid double ester-octadecyl poly(ethyleneoxy)₂₀ ether-ethylene trimethyl ammonium chloride (R303). Then CFMBD was utilized to treat the cotton fabric. Results showed that the as-prepared latex had due structure and its particles had uniform spherical core-shell structure with an average diameter of 125 nm. The core-shell CFMBD latex film thus had two T _g and its thermal property was improved due to the introduction of DFMA. CFMBD could form a smooth resin film on the treated fabric/fiber surface under FESEM observation. XPS analysis indicated the fluoroalkyl groups had the tendency to enrich at the film-air interface. Hydrophobicity of the CFMBD treated fabric was slightly superior to that of the fabric treated by general emulsion but their oleophobicity was identical. Contact angles of water and diiodomethane on the CFMBD treated fabric surface could attain 133.5 ° and 105.5 °, respectively. However, washing durability of the treated fabric by CFMBD showed improvement compared to the general emulsion. In addition, CFMBD didn’t influence whiteness of the treated fabric but would make it slightly stiff at high doses.     

Facile fabrication of PVAc-g-PVDF coating on surface modified cotton fabric for applications in oil/water separation and heavy metal ions removal

Selective separation is an effective method for the removal of heavy metal ions and waste oil from wastewater. Polyvinylidene fluoride (PVDF) was functionalized with polyvinyl acetate (PVAc) by in-situ polymerization, and novel PVAc-g-PVDF coating on surface modified cotton fabric were prepared. The contact angle (CA), pure water flux (PWF) and self-cleaning ability of coated cotton fabric were investigated in detail. In addition, the separation performance of coated cotton fabric was reflected by the removal of heavy metal ions in simulated wastewater. The results revealed that the PVAc-g-PVDF-coated cotton fabric was free of waste oil adhesion and was self-cleaning from waste oil in aqueous environment. Meanwhile, this coated cotton fabric can effectively separate oil/water mixtures with a high flux and high oil rejection, and was easily recycled for long-term use. More importantly, the heavy metal ions rejection ratio and adsorption capacity of cotton fabric were also improved with the addition of PVAc-g-PVDF coating. PVAc-g-PVDF-coated cotton fabric exhibited excellent rejection stability and reuse performances after several times fouling and washing tests. It can be expected that the present work will provide insight into a scaled-up fabrication process of PVAc-g-PVDF coating for purifying wastewater.     

Multifunctional modification of wool fabric using graphene/TiO<Subscript>2</Subscript> nanocomposite

In this study, a new finishing technique is introduced through treatment of wool fabric with graphene/TiO₂ nanocomposite. Graphene oxide/titanium dioxide nanocomposite first applied on the wool fabric by hydrolysis of titanium isopropoxide in graphene oxide suspension and then this coating chemically converted by sodium hydrosulfite to graphene/TiO₂ nanocomposite. The homogenous distribution of the graphene/TiO₂ nanocomposite on the fiber surface was confirmed by field emission scanning electron microscopy (FE-SEM), Energy-dispersive X-ray spectroscopy (EDS) and X-ray mapping. X-ray diffraction patterns proved the presence of titanium dioxide nanoparticles with a crystal size of 127 Å on the treated wool fabric. Also, the defect analysis based on X-ray photoelectron spectroscopy (XPS) established the composition of the nanocomposite. Other characteristics of treated fabrics such as antibacterial activity, photo-catalytic self-cleaning, electrical resistivity, ultraviolet (UV) blocking activity and cytotoxicity were also assessed. The treated wool fabrics possess significant antibacterial activity and photo-catalytic self-cleaning property by degradation of methylene blue under sunlight irradiation. Moreover, this process has no negative effect on cytotoxicity of the treated fabric even reduces electrical resistivity and improves UV blocking activity.     

A novel DDPSi-FR flame retardant treatment and its effects on the properties of wool fabrics

A novel flame retardant monomer DDPSi-FR containing organophosphorus and silicon was prepared using 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 4-hydroxybenzaldehyde (HBA), and 3-glycidoxypropyltrimethoxysilane (GPTMS). The chemical structure of DDPSi-FR was characterized by Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). Subsequently, after treating the wool fabrics, the effects of the monomer on the flame retardancy, thermal stability, and mechanical properties were studied. The flame retardant and thermal properties were evaluated by conducting vertical flame tests, limiting oxygen index (LOI) determination, and thermogravimetric analysis (TGA). The results showed that improved flame retardancy and thermal stability were achieved. Notably, the flame retardancy was retained even after 15 washing cycles. The mechanical properties were evaluated using the bursting strength, and the results indicated that DDPSi-FR treatment improved the breaking strength.     

Synthesis of a novel flame retardant containing phosphorus-nitrogen and its comparison for cotton fabric

A new charring agent, a derivative of cyanuric chloride, mono-substituted, dimethyl (4,6-dichloro-1,3,5-triazin-2-yloxy)methylphosphonate (CN), was synthesized in good yield and characterized. Its flame retardant and thermogravimetric properties were compared to those of the di-substituted compound, tetramethyl (6-chloro-1,3,5-triazine-2,4-diyl)bis(oxy)bis (methylene)diphosphonate (CN-1), which was prepared in previous work. All untreated fabric showed limiting oxygen index (LOI) values of about 18 vol% oxygen in nitrogen. Fabrics treated with CN at 5?C21 wt% add-ons had high LOI values of 30?C40 vol%, while fabrics treated with CN-1 at 5?C19 wt% add-ons had low to high LOI value of 20?C36 vol%. In 45° angle flammability tests, all treated fabrics with CN and CN-1 were passed and some fabrics were not igniting at all. Thermal degradation revealed that onset of degradation and the char yield of CN compound is higher than that of CN-1. Treated fabric with CN, 21 wt% add-on, had an onset of degradation of 240 °C, while fabric treated with CN-1, 19 wt% add-on displayed an onset of degradation of 230 °C. Despite the differences in onset temperature, the two samples provided almost the same char yield at 600 °C, 35 and 36 %. With Fourier transform infrared (FTIR), samples of treated/unburned and treated/burned of CN and CN-1 showed the same functional groups and revealed the disappearance of triazine group and P-O-methyl after burning. Additionally, scanning electron microscopy (SEM) showed that both CN and CN-1 acted as flame retardants by the same mechanism and characterized the surface morphology of the flame retardant treated twill fabrics.