Electrospun in-situ hybrid polyurethane/nano-TiO<Subscript>2</Subscript> as wound dressings

By combining the organic-inorganic hybridization, wet phase inversion, and electrospinning, novel electrospun polyurethane (PU) membranes with in-situ generated nano-TiO₂ were prepared, which satisfied the requirements of an ideal wound dressing. The morphology of the PU-TiO₂ mats and the cross sectional morphologies of the membranes were characterized by a scanning electron microscopy (SEM). The average diameter of the individual fibers obtained from the solutions was 341±12 nm. SEM micrographs with higher magnification further showed that the in-situ generated TiO₂ particles were well-separated and dispersed homogeneously in the membranes. The average sizes of TiO₂ particles were increased from 31 to 57 nm, with the increase of nano-TiO₂ concentration. The water vapor transmission rates (WVTRs) of the membranes were in the range of 373.55–3121.86 g/m²·d and decreased gradually with the increase of nano-TiO₂ concentration. The water absorption of various PU membranes was in the range of 210.90–397.98 % which was enough to prevent wound beds from exudate accumulation. Shake flask testing indicated that the PU membrane exhibited antibacterial efficiency against Pseudomonas aeruginosa (Ps. aeruginosa) and Staphylococcus aureus (S. aureus) due to in-situ generated of nano-TiO₂. These electrospun nanofibrous membranes also had no toxic effect and showed good and immediate adherence to L929 cells.     

Modification and Characterization of Nano-TiO<Subscript>2</Subscript> for Efficient Fixation on Cotton Fibers

In this paper, a silane coupling agent, 3-aminopropyltriethoxysilane, was reacted with nano-TiO₂ to introduce amino group onto it which was then reacted with trichlorotriazine to obtain a dichlorotriazine functionalized nano-TiO₂ for the firm fixation of it on cotton fibers. The reaction process was monitored by the titration of primary and secondary amino groups, and the reaction conditions were optimized with orthogonal method accordingly. The dichlorotriazine functionalized nano-TiO₂ was reacted with cotton fabric by the nucleophile substitution reaction to afford nano-TiO₂ functionalized cotton fabric, the structure and surface morphology of the nano-TiO₂ finished cotton fibers were studied by FT-TR and SEM. In addition, the fixation duration of the nano-TiO₂ modified cotton was studied according to AATCC test method 61–2010. The results show that the washing fastness of the nano-TiO₂ is excellent.     

Preparation and properties of Nano-TiO2 photo-catalytic silk respirator paper

In order to obtain paper respirator with dust resistance performance and antibacterial property, silk photo-catalytic respirator paper was made by loading nano-TiO₂ photo-catalyst on silk based respirator paper. The pore structure, surface topography and TiO₂ distribution, and the filtration performance of silk respirator paper were studied by using a pore size meter (PSM), a field emission scanning electron microscope (FESEM), and a filter tester, respectively. In addition, the antibacterial property of silk respirator paper was also investigated. The results showed that the pore structure and filtration performance of silk respirator paper could be controlled by changing the degree of beating of silk pulp and the basis weight of silk paper. Silk respirator paper of 45 g/m² made from silk pulp having beating degree of 85 ^oSR had high filtration efficiency and appropriate filtration resistance. Nano-TiO₂ particles were mainly attached to the surface of silk paper, and the loading of nano-TiO₂ photo-catalyst resulted in a slight decrease in filtration resistance and filtration efficiency of silk respirator paper. It, however, improved the antibacterial property of silk respirator paper effectively.     

In situ loading TiO<Subscript>2</Subscript> and its photocatalysis and UV resistance on cotton fabric

Anatase TiO₂ nanoparticles was in-situ formed on the cotton fabric by using tetrabutyl titanate (TBT) as a precursor through the normal pressure hydrothermal method. X-ray diffraction (XRD), Scanning electron microscopy (SEM), UV visible spectra (UV-VIS), ATR-IR were used as the characterization techniques. Photocatalytic performance of TiO₂ on the fabric surface was evaluated by methylene blue (MB), 4 kinds of the common living stains and three dyes under ultraviolet and visible light radiation. XRD analysis found that the TiO₂ loaded on the fabric was mainly anatase crystalline phase with particle size of 6.4 nm. SEM observed that a large number of nano TiO₂ particles are distributed on the fabric surface. UV-VIS test indicated that theTiO₂-coated fabric possessed an obvious absorption for ultraviolet. ATR-IR analysis indicated that the nano-TiO₂ possesses a strong affinity with the hydroxyl group of the cotton fabric, and the soaping tests showed that the TiO₂ was firmly bonded with the fabrics. The treated fabrics have good degradation ability for MB aqueous solution, and could degrade azo, anthraquinone and phthalocyanine dyes. The order of degradation of the common life stains was: pepper oil> tea > coffee > soy sauce.     

Photocatalytic degradation of formaldehyde by silk mask paper loading nanometer titanium dioxide

Silk mask paper with different adsorbability was prepared by changing the beating degree of silk pulp and the basis weight of silk paper, and photocatalytic silk mask paper was prepared by loading nanometer titanium dioxide (nano-TiO₂) on the silk mask paper, then degradation of formaldehyde by silk mask paper loading nano-TiO₂ under daylight lamps and ultraviolet lamps were investigated, respectively. Results showed that silk mask paper could adsorb formaldehyde and had higher adsorption efficiency in the initial stage, and the adsorption/desorption equilibrium could be basically achieved in 60 minutes. The adsorption capacity of silk mask paper made from silk pulp with beating degree of 45 ^oSR was relatively low, and it increased with the increase of beating degree, but there was little change in adsorption when the beating degree of silk pulp exceeded 65 ^oSR. Under daylight lamps, 26.61 %, 31.42 % and 38.21 % of formaldehyde could be degraded in 180 minutes by silk mask paper loading 1 wt%, 3 wt% and 5 wt% nano-TiO₂, respectively. However, under ultraviolet (UV) lamps, 46.23 %, 55.47 % and 66.38 % of formaldehyde could be degraded within the same time, respectively. More formaldehyde could be degraded by photocatalytic silk mask paper under UV lamps than under daylight lamps, and the more the load of nano-TiO₂ on the silk mask paper, the higher the degradation rate of formaldehyde within the same time.     

Fabrication and characterization of nano Al<Subscript>2</Subscript>O<Subscript>3</Subscript> filled PVA:NH<Subscript>4</Subscript>SCN electrolyte nanofibers by electrospinning

Present paper reports a method of preparing polymer composite electrolyte nanofiber mat using polyvinyl alcohol (PVA), ammonium thiocynate (NH₄SCN) salt, and aluminium oxide (Al₂O₃) nano particles based on electrospinning technique. Two-stage process of preparation of nanofibers, namely, preparation of nano particles filled PVA electrolyte gel solution followed by its electrospinning has been used. The so obtained nanofibers have been characterized by XRD, DSC, SEM, and Conductivity measurements. XRD patterns affirm the formation of nanocomposite while SEM pictures reveal formation of fibers on a nano scale format (300–800 nm). Fibers of the electrolytes are seen to be thermally stable. Ionic conductivity of electrolyte fiber is seen to improve in the presence of nano filler at room temperature with a maximum at 5.31×10⁻³ Scm⁻¹ for 4 wt% filler concentration, which is comparable to that for corresponding dried gel electrolyte films.     

Characterization of plant and animal based natural fibers reinforced polypropylene composites and their comparative study

Natural fibers are largely divided into two categories depending on their origin: plant based and animal based. Plant based natural jute fiber reinforced polypropylene (PP) matrix composites (20 wt% fiber) were fabricated by compression molding. Bending strength (BS), bending modulus (BM), tensile strength (TS), Young’s modulus (YM), and impact strength (IS) of the composites were found 44.2 MPa, 2200 MPa, 41.3 MPa, 750 MPa and 12 kJ/m², respectively. Animal based natural B. mori silk fiber reinforced polypropylene (PP) matrix composites (20 wt% fiber) were fabricated in the same way and the mechanical properties were compared over the silk based composites. TS, YM, BS, BM, IS of silk fiber reinforced polypropylene composites were found 55.6 MPa, 760 MPa, 57.1 MPa, 3320 MPa and 17 kJ/m² respectively. Degradation of composites in soil was measured upto twelve weeks. It was found that plant based jute fiber/PP composite losses its strength more than animal based silk fiber/PP composite for the same period of time. The comparative study makes it clear that mechanical properties of silk/PP composites are greater than those values of jute/PP composites. But jute/PP composites are more degradable than silk/PP composites i.e., silk/PP composites retain their strength for a longer period than jute/PP composites.     

Rapid fabrication and optimization of silk fibers supported and stabilized MnO<Subscript>2</Subscript> catalysts

We report on the in situ synthesis and stabilization of manganese dioxide (MnO₂) onto four different silk yarns (mulberry, tasar, muga and eri silks). A new ultrasound-assisted procedure was used to reduce permanganate (MnO₄ ^?) and yielded MnO₂ nanoparticles (NPs) on/in the different silk fibers. Using a factorial design we assessed the influence of the silk type, manganese precursor concentration, sonication time, and temperature. The results indicated no measurable effect of the process parameters on the silk structures, but significant correlation with the rate of degradation of methylene blue (MB) and the fraction of permanganate consumed. Further optimization of the factorial model identified the optimal process conditions for each silks: mulberry (150 min sonication, 20 mM permanganate), eri (360 min, 10 mM), tasar (150 min, 10 mM) and Muga (20 min, 10 mM). The operational stability (successive catalysis) of the optimum hybrids showed good performance over 5 cycles and most importantly reduced direct dye absorption relatively to dye oxidation. Overall, we found that all silks could template the formation and stabilization of different MnO₂ polymorphs and yielded catalytic instead of stoichiometric hybrid fibers.     

Preparation and characterization of inner-pressure hollow fiber composite membrane via two-way coating technique for CO<Subscript>2</Subscript>/CH<Subscript>4</Subscript> separation

High-selectivity inner-pressure hollow fiber composite (HFC) membrane for CO₂/CH₄ separation was prepared through the Two-way coating (TWC) technique. The blends of poly(vinylamine) (PVAm)/polyvinyl alcohol (PVA) were coated onto porous hollow fiber polysulfone (PSF) ultrafiltration (UF) membrane with an effective membrane area of 0.4 m². The effects of fabrication parameters on the permselectivity of the resultant HFC membrane were investigated and the optimum preparation conditions were obtained as follows: coating time for 30 min and air blowing time for 30 min after the coating. The prepared HFC membrane showed the typical characteristic of fixed carrier membrane with a high selectivity of CO₂ and CH₄: the separation factor of CO₂/CH₄ (40 vol% CO₂ at 25 °C and 0.2 MPa) was 36.6 and the CO₂ permeability was 56.3 GPU. Field emission scanning electron microscopy (FESEM) images indicated that the HFC membrane prepared by TWC technique had a uniform coating layer along the whole hollow fiber. Membrane permselectivity showed almost no difference between different membrane sections. The HFC membrane showed a good stability during the continuous testing process of 540 h. And the HFC membrane preserved at 30 °C and 40 % humidity exhibited a good durability with a basically unchanged separation factor after 30 days.     

Polyaniline-doped TiO<Subscript>2</Subscript>/PLLA fibers with enhanced visible-light photocatalytic degradation performance

A simple and practical strategy has been developed for preparing polyaniline(PANi)-doped TiO₂/poly(l-lactide) (P@TiP-C) fibers by a combination of coaxial-electrospinning and in-situ polymerization. The TiO₂/PLLA composite fibers with TiO₂ located on the surface were fabricated by coaxial-electrospinning, with PLLA as the core phase and a dispersion of TiO₂ particles, a well-known photocatalyst, in the sheath phase. The aniline monomers were also located in the core phase and in-situ polymerized by ammonium persulfate (APS) after electrospinning. SEM images show that TiO₂ particles were located on the surface of PLLA fibers. Photocatalytic degradation tests show that the P@TiP-C fibers exhibit enhanced photocatalytic activity for degradation of methyl orange under visible light, likely due to the synergistic effect of PANi and TiO₂.     

Controlling the Properties of OPEFB/PLA Polymer Composite by Using Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> for Microwave Applications

Microwave-absorptive polymer composite materials provide protection against interference to communication systems caused by microwave-inducing devices. Microwave-absorptive polymer composites were prepared from polylactic acid (PLA) biocomposite blended with oil palm empty fruit bunch (OPEFB) fiber and commercial Iron oxide (Fe₂O₃) as filler using the melt-blending method. The composites characterization was carried out using the scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses. The coefficient of reflection S₁₁ and coefficient of transmission S₂₁ of the composites for various Fe₂O₃ filler percentages were determined using a rectangular waveguide in connection with microwave vector network analyser (HP/Agilent model PNA N5227). These coefficients were then used to calculate microwave-absorption properties (in decibels). XRD analysis showed that increasing amounts of reinforced material (Fe₂O₃) reduces the crystallinity of the composites. SEM data indicated that Fe₂O₃ filler ratio increased in the composites, and adhesion to the cellulose fiber grew gradually until the highest percentage of filler was added. The complex relative permittivity and relative permeability were obtained within the broad frequency range of 8–12 GHz at room temperature for various percentages of filler and were measured by the transmission/reflection method using a vector network analyser. Fe₂O₃ embedment in OPEFB/PLA was observed to have resulted in enhancing the dielectric and magnetic properties. The values of permittivity and permeability increased with increasing Fe₂O₃ filler content. Theoretical simulation studied the relation between ε′ and ε″ of the relative complex permittivity in terms of Cole-Cole dispersion law. The result indicated that the processes of Debye relaxation in Fe₂O₃/OPEFB/PLA, the unique dielectric characteristics of Fe₂O₃ cannot be accounted for by both the Debye dipolar relaxation and natural resonance. Results further showed that the material transmission, reflection, and absorption properties could be controlled by changing the percentage of Fe₂O₃ filler in the composites.     

Prediction of mechanical properties of aging B.mori silk fabric based on grey neural network model

This paper presents a grey neural network model for the prediction of mechanical properties of aging B.mori silk fabric. In the experiment, we obtained outdoor natural aging breaking strength of B.mori silk fabric from 8 samples. Then, a grey neural network GNNM (1,1) model is proposed by the means of combining GM (1,1) model with BP artificial neural network to predict mechanical properties of B.mori silk fabric. At the same time, this paper analyzed and compared the GM (1,1) model and GNNM (1,1) model by using prediction error such as the relative percentage error (RPE) and the root mean square error (RMSE). The experimental results show that the RMSE of GNNM (1,1) model is 0.0284 well below 6.1786, which is the RMSE of GM (1,1) model. It indicates the GNNM (1,1) model were better than the normal grey GM (1,1) model, when taken the prediction error as evaluation parameter.     

Nano-TiO<Subscript>2</Subscript> based multilayer film deposition on cotton fabrics for UV-protection

Nano-TiO₂ based multilayer nanocomposite films were fabricated on cationically modified woven cotton fabrics by layer-by-layer molecular self-assembly technique. Cationization process was used to obtain cationic surface charge on cotton fabrics. Attenuated total reflectance Fourier transform infrared spectroscopy analyses were used to verify the presence of cationic surface charge and multilayer films deposited on the fabrics. Scanning electron microscope micrographs of poly(sodium 4-styrene sulfonate)/TiO₂, nano polyurethane/TiO₂, and TiO₂/poly(diallyldimethylammonium chloride) multilayer films deposited on cotton fabrics were taken. With nano-TiO₂ based multilayer film deposition, the protection of cotton fabrics against UV radiation is enhanced. The UV protection durability of the self-assembled multilayer films deposited on the cotton fabrics was analyzed after 10 and 20 washing cycles at 40 °C for 30 min. Air permeability and whiteness value analysis were performed on the untreated and multilayer film deposited cotton fabrics. The effect of layer-by-layer deposition process on tensile strength properties of the warp and weft yarns was determined.     

Electrospinning of <Emphasis Type="Italic">Bombyx mori</Emphasis> silk fibroin nanofiber mats reinforced by cellulose nanowhiskers

Cellulose nanowhisker (CNW) reinforced electrospun Bombyx mori silk fibroin (SF) nanofibers were fabricated. The morphology, structure, and mechanical properties of nanofibers were investigated by FE-SEM, TEM, FTIR, and tensile testing. It was found that the nanofiber size decreased obviously from 250 nm in the unreinforced mat to 77–160 nm in the CNW reinforced mats depending on the CNW content due to the increased conductivity of spinning dope. In the reinforced mats, the CNWs were embedded in the SF matrix separated from each other, and aligned along the fiber axis. There was a positive correlation between the CNW content and the tensile strength and Young’s modulus of reinforced mats. However the strain at break dropped gradually with the increase of CNW. When the CNW content was 2 w/w%, the tensile strength and Young’s modulus of reinforced SF nanofiber mats were about 2 times higher than those of unreinforced mat.     

Effect of phase transformation on physical and biological properties of PVA/CaFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanocomposite

The thermal treatment method was employed to achieve higher homogeneity of calcium ferrite (CaFe2O4) and Poly (vinyl alcohol) (PVA) nanocomposites. The influences of phase transformation on physical and biological properties of calcined specimens were investigated by various experimental techniques including X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), high resolution Field emission scanning electron microscope (FESEM) and Fourier transform infrared spectroscopy (FT-IR). Heat treatment was conducted at temperatures between 723 and 923 K, so that a phase transformation occurred from cubic to orthorhombic spinel structure at 923 K. The chemical analysis of the PVA/CaFe₂O₄ nanocomposite was performed by energy dispersion X-ray analysis (EDXA), demonstrated the PVA/CaFe₂O₄ nanocomposites contained the elements of C, Ca, Fe, and O. The formed nanocomposites exhibited ferromagnetic behaviors which were confirmed by using a vibrating sample magnetometer (VSM). The calcined specimens were carried out to an antimicrobial or antifungal test.     

Effect of UV irradiation on cellulase degradation of cellulose acetate containing TiO<Subscript>2</Subscript>

Cellulose acetate (CA) films containing anatase type titanium dioxide (TiO₂) nanoparticles were prepared by solution casting. The film surface was modified by UV irradiation using a grid type UV irradiator. The UV irradiation caused slight increase in photodegradation of the CA films with TiO₂ compared to the CA film alone. However, CA films irrespective of TiO₂ content did not show a significant enzymatic degradation by a cellulase fromAspergillus niger without UV irradiation. Upon UV irradiation, the biodegradability remarkably improved even in the CA film without TiO₂. The irradiation of CA films decreased both the water contact angle and the degree of substitution (DS) implying the decrease in acetyl groups of the CA film surface due to the photo-scission of the acetyl group and photooxidation, resulting in more facile biodegradation of the surface film layer. The substantial enhancement in biodegradation of the UV irradiated CA film containing TiO₂ was attributed to the increased hydrophilicity, lowered DS and zeta potential due to the photoscission and the photooxidation effect of UV light. Also the increased surface area of the CA film due to the photocatalysis of TiO₂ particles may encourage the facile biodegradation.     

Quantification of degradation and surface morphology of NB7 silk fibers irradiated by 8 MeV electron beam using XRD and SEM techniques

NB7 silk fiber (Bombyx mori) was irradiated with the maximum dose range of 100 kGy using 8 MeV electron beam at room temperature. Irradiation effect in these fibers is quantified in terms of the changes in microstructural parameters employing X-ray diffraction line profile analysis technique. For this purpose we have used three asymmetric distribution functions for column lengths in a crystal. The decreasing trend of crystallite size values (〈N〉 as well as D _s ) and crystallinity with increasing dosage of radiation clearly indicates the degradation of fiber. Of the several factors responsible for such a behavior, we presume that the chain scission of polymer network is a significant one over others and it is well pronounced here, leading to low molecular weight of the samples. This degradation is attributed to many changes in tensile properties of the polymer. Comparison of SEM photographs also confirms the X-ray results.     

Developing UV-protective cotton fabric based on SiO<Subscript>x</Subscript> nanoparticles

Nano-SiO_x suspension was prepared for its unique optical performance to improve the anti-ultraviolet property of cotton fabric in this paper. The experimental results showed that UV-resistance property of thus treated fabrics had been enhanced significantly. The spectrum of absorption, reflection, and transmittance of the treated fabric was analyzed during the optimized processing. The mechanical property of the treated fabric displayed a little increase compared with the original untreated fabric. The morphology of the treated fabric was studied by SEM. The UPF (Ultraviolet Protection Factor) of the fabric treated with nano-SiO_x suspension reached 62, much higher than that of the original untreated fabric. Moreover, after 50 home launderings, the UV-blocking property of treated fabric changed little due to the strong affinity between the nano-SiO_x particles and cotton fiber.     

Antibacterial Bombyx Mori silk fabric modified with reactive chitosan quaternary ammonium salt and its laundering durability

A new fiber-reactive chitosan derivative was synthesized in two steps from a chitosan of low molecular weight. First, a water-soluble chitosan derivative, N-[(2-hydroxy-3-trimethylammonium)propyl] chitosan chloride (short for HTCC), was prepared by reacting chitosan with 2,3-epoxypropyltrimethylammonium chloride. Second, HTCC was further modified by reacting with N-(hydroxymethyl)-acrylamide to prepare a fiber-reactive chitosan derivative, O-methyl acrylamide quaternary ammonium salt of chitosan (short for NMA-HTCC), which can form covalent bonds with silk fiber under alkaline conditions. The chemical structure of NMA-HTCC was characterized by Fourier transform infrared spectrum (FTIR) and nuclear magnetic resonance (NMR). The substitution degree of HTCC and the double-bond content of NMA-HTCC were tested. Then NMA-HTCC was used for antibacterial finishing of Bombyx Mori silk fabric. The results showed that silk fabric treated with NMA-HTCC had a significantly improved antibacterial activity to Staphylococcus aureus and Escherichia coli, and the antibacterial activity of silk fabric finished by NMA-HTCC was much better than that finished by chitosan and HTCC. Bombyx Mori silk fabric modified with NMA-HTCC demonstrated excellent durable antibacterial activity, even after 50 repeated launderings, the bacterial reduction rate of silk fabric maintained over 95 %.     

Dyeing properties and colour fastness of cotton and silk fabrics dyed with<Emphasis Type="Italic">Cassia tora L.</Emphasis> extract

A natural colorant was extracted fromCassia tora L. using buffer solutions (pH: 2–11) as extractants. The dyeing solution (Cassia tora L. extract) extracted using pH 9 buffer solution was found to give the highest K/S values of dyed fabrics. Cotton and silk fabrics were dyed withCassia tora L. extract at 60°C for 60 min with pre-treatment of various metal salts as mordants. It was found thatCassia tora L. extract was polygenetic dyestuffs and its major components were anthraquinones. Studies have been made on the effects of the kind of mordant on dyeing properties and colour fastnesses of cotton and silk fabrics. The K/S of cotton fabrics increased in the order of the dyeing using FeSO₄>CuSO₄>ZnSO₄>MnSO₄≅Al₂(SO₄)₃>NiSO₄>none, however, the K/S of silk fabrics increased in the order of the dyeing using FeSO₄>CuSO₄>ZnSO₄≅Al₂(SO₄)₃>MnSO₄≅NiSO₄>none. It was found that the K/S values of dyed fabrics were largely affected by the colour difference (ΔE) between mordanted fabric and control fabric. However, they were not depended on the content of mordanted metal ion of the fabrics. Mordants FeSO₄ and CuSO₄ for cotton fabric, FeSO₄, CuSO₄, and Al₂(SO₄)₃ for silk fabric were found to give good light fastness (rating 4).