WO2022190071A1 - Synthèse et fabrication de nanofibres composites d'oxyde de cuivre-oxyde de zinc ayant des propriétés antimicrobiennes et pouvant revêtir divers tissus - Google Patents

Synthèse et fabrication de nanofibres composites d'oxyde de cuivre-oxyde de zinc ayant des propriétés antimicrobiennes et pouvant revêtir divers tissus Download PDF

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Publication number
WO2022190071A1
WO2022190071A1 PCT/IB2022/052231 IB2022052231W WO2022190071A1 WO 2022190071 A1 WO2022190071 A1 WO 2022190071A1 IB 2022052231 W IB2022052231 W IB 2022052231W WO 2022190071 A1 WO2022190071 A1 WO 2022190071A1
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WIPO (PCT)
Prior art keywords
synthesis
zinc oxide
properties
nanofibers
copper oxide
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PCT/IB2022/052231
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English (en)
Inventor
Hamidreza REZAEIAN MEHR
Parisa AFSARI
Original Assignee
Rezaeian Mehr Hamidreza
Afsari Parisa
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Filing date
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Application filed by Rezaeian Mehr Hamidreza, Afsari Parisa filed Critical Rezaeian Mehr Hamidreza
Publication of WO2022190071A1 publication Critical patent/WO2022190071A1/fr

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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning

Definitions

  • PVP polymer has been used as a polymer component for electrospinning.
  • CZCNFMs Composite nanofiber membranes loaded with CuO-ZnO
  • MBE modified bubble electrospinning
  • a heat treatment method a heat treatment method
  • a hydrothermal method The influences of the mass ratio of Cu to Zn on the morphologies, structures, and properties of the CNFMs were studied, and the obtained CNFMs with different mass ratios of Cu to Zn were applied to the photo degradation of methyl orange (MO) and methylene blue (MB).
  • This unique combination has corona anti-virus and antibacterial properties simultaneously.
  • divalent zinc oxide and divalent copper oxide nanofibers have been synthesized.
  • the final application of our design is the preparation of non-woven spun bond fabric with anti-corona and anti bacterial properties simultaneously and its use in the preparation of masks with anti-corona and anti-bacterial media as well as air filters with the same property.
  • the photocatalytic properties in the elimination of organic inks as external sources of water pollution have been studied.
  • the synthesized hollow nanofibers not only use the photocatalytic mechanism to produce free radicals, but also have corona and antibacterial properties in environments without visible light spectrum.
  • the second section of the chapter explains the mechanism of the ultrasound-assisted deposition of nanoparticles on textile.
  • the coating can be performed by an in situ process where the nanoparticles are formed and immediately thrown to the surface of the fabrics. This approach was used for ZnO, CuO, and Zn-CuO nanoparticles.
  • the sonochemical process can be used as a “throwing stone” technique, namely, previously commercially synthesized nanoparticles will be placed in the sonication bath and sonicated in the presence of the fabric.
  • the last achievements in the antimicrobial finishing of textile with metal Nano-oxides by sonochemical method are provided in the third section.
  • One of the proofs that the sonochemical method is one of the best coating methods is that the sonochemically coated fabrics were washed 65 cycles in hospital washing machines (75 or 92 °C) and have shown excellent antibacterial properties at the end of the process.
  • woven linen fabric is used for covering, while in our design, non-woven spunbond fabric is used.
  • the focus is on the antibacterial properties of the final fabric, while in our design, the focus is on the corona anti-virus property with a performance of more than 99% covered by non-woven fabric.
  • An allergen-barrier fabric comprising at least one porous layer of polymeric nanofibers, a fabric layer super jet and adhered to the nanofiber layer, and optionally a fabric layer subjacent and adhered to the nanofiber layer, wherein the superjacent and optional subjacent fabric layers are adhered to said nanofiber layer such that the allergen-barrier fabric has a mean flow pore size of between about 0.01 pm and about 10 pm, and a Frazier air permeability of at least about 1.5 m3-min-m2.
  • Nano fabrics is an emerging and interesting application of nanotechnology, which involves dealing with nanofibers at the atomic and molecular levels to tweak their properties.
  • the increasing demand for sophisticated fabrics with special features and exceptional comfort drives the need for the use of nanotechnology in this industry.
  • Scanning Electron Microscope (SEM) as a magnifying device that uses electrons instead of light, is used in nanotechnology. It uses electron bombardment to create images of objects as small as 10 nanometers. The construction of the SEM has allowed researchers to study larger samples more simply and clearly.
  • the sample bombardment causes electrons to be released from the sample to the positively charged surface, and convert to signals.
  • the movement of the beam on the sample provides a set of signals and causes the microscope to displays an image of the sample surface on the computer screen.
  • FIG. 4 shows the uniform structure of zinc oxide hollow nanofibers and zinc oxide-copper oxide composites with different compositions before and after calcination.
  • Thermal analysis is the measurement of the change that occurs in the physical properties of a material when the temperature is changed according to a special program. Physical properties refer to quantities such as weight, geometric size, heat capacity, electrical conductivity, etc. that change with increasing the sample temperature.
  • a thermal program means heating the sample according to a special temperature program and in a specific environment.
  • Thermogravimetry (TG) and differential thermal analysis (DTA) is thermal analysis methods that are based on measuring the weight of the sample during heating and measuring the temperature difference between the unknown and control samples, respectively.
  • TG and DTA were performed to investigate the thermal behavior of the synthesized fibers at the temperature range of room temperature up to 600 °C, air environment, and heating rate of 5 °C-min.
  • 95% of the sample weight has gradually reduced in several stages. This gradual reduction at 50-100 °C is related to the evaporation of water absorbed in the solvent and acetate groups.
  • Weight loss of about 45% at 170-270 °C is related to the chemical decomposition of metal salts (zinc acetate and copper acetate) and the formation of metal oxide structures in composite nanofibers.
  • weight loss of about 40% is observed in the sample, which indicates the chemical decomposition of PVP.
  • the lack of significant weight loss observed at >450 °C indicates the completion of the PVP decomposition process.
  • the absence of changes at >565 °C indicates the completion of the calcination process and the formation of zinc oxide-copper oxide nanocomposite crystals.
  • ABB, Bomem, MB 100 spectrometer was used to evaluate the samples using infrared spectroscopy. To do this, first, the tablets were made from potassium chloride as the reference material, as well as from the powder sample, and then irradiated with light.
  • the wavelength of 730.97 cm 1 can be related to the (C-C) bond of the paraffin hydrocarbon chain.
  • the absorptions at 1375.27 and 2854.45-2954.74 cm-1 indicate the flexural (C-H) and tensile (C-H) bonds of paraffin, respectively.
  • Synthesis is a chemical reaction that is designed to provide a pure product with the desired efficiency to solve previous problems and optimize them. Moreover, the design of these reactions should be such that they have no operational complexity. There are several methods for producing materials and reaching the final material. Even the basic methods are used in some cases. For these methods to be useful, they must be highly efficient and suitable for a wide range of materials. Among the applications of nanomaterials used in this project are their antibacterial and antiseptic properties because they are in direct contact with microbes. These nanomaterials are used as antiviral, antifungal, and antibacterial agents when added to the solution. Copper nanoparticles are also widely used in this new science and have many applications in various fields. Zinc oxide is a nanoparticle with unique properties.
  • the most essential application of XRD is to determine the phases in an unknown sample.
  • the location and intensity of peaks contain information from the sample, which can be used to determine the atomic structure and phase of the dispersing surfaces, and thus determine the type and structure of the unknown sample. This is performed by comparing the resulting diagram with the existing standards.
  • the crystalline structural properties, or the crystalline order are not completely observed in the material, rather, the materials are a combination of amorphous and crystalline forms.
  • Amorphous spheres form wide peaks and crystalline spheres form sharp peaks in the diagram.
  • the intensity ratio of these peaks can be used to determine crystallinity.
  • the mean size of the crystals is calculated by the Debye-Scherer relationship at full width half maximum (FWHM) according to the following equation:
  • D represents the average size of the crystals perpendicular to the X-ray
  • K is the Debye-Scherer constant (0.9)
  • l is the X-ray wavelength (0.154178 nm)
  • b is the peak width of half-maximum.
  • the internal strain of the sample is calculated by the Williamson-Hall relationship as follows:
  • b is the full width of the Bragg peak at half maximum
  • k is the Scherer constant
  • D is mean crystallite size
  • l is the radiated X-ray wavelength
  • e is strain
  • Q is peak angle
  • the crystal size is calculated using the peak width of half-maximum in the Debye-Scherer relationship and is as follows (Table 2).
  • the produced fibers were collected from the collector and evaluated at X1000 magnification using the TEM ( Figure 2). It can be seen that the samples are in the form of fibers with a large length to diameter ratio and are reached as a shell-core. Therefore, according to the obtained images, the core-shell morphology (hollow nanofibers) can be observed in addition to solid nanofibers. Due to the limited magnification of the optical microscope and the more detailed study of the dimensions and morphology of the fibers obtained before and after calcination, a scanning electron microscope (SEM) was used.
  • SEM scanning electron microscope
  • FIG. 3 Device components without side cover
  • FIG. 4 Electrical device parameters
  • FIG. 5 Sample Z100, (a) before and (b) after calcination
  • FIG. 6 Specifications of ZnO - (x% wt) CuO samples and their corresponding CuO weight percentages
  • FIG. 7 X-ray diffraction spectrum of Z100, ZC5, ZC25, ZC50, ZC75 samples prepared by electrification method
  • FIG. 8 The average size of crystals is calculated by Debye-Scherer method
  • FIG. 9 Transient optical microscope images
  • FIG. 10 SEM images and EDX test results obtained from solid and hollow synthesized fiber samples (a) Z100 before calcination, (b) Z100, (c) ZC5, (d) ZC25, (e) ZC50 after calcination [0059]
  • FIG. 11 The TG and DTA thermal analysis diagram shows the ZC25 sample
  • FTIR chart (A) Z100 sample before calcination, (B) Z100 sample after calcination and (C) ZC2 sample after calcination
  • FIG. 1 1. Potential difference supply device 2. Syringe pump 3.
  • FIG. 6 Specifications of Z n O - (x% wt ) CuO samples and their corresponding CuO weight percentages
  • FIG. 7 X-ray diffraction spectrum of Z100, ZC5, ZC25, ZC50, ZC75 samples prepared by electrification method
  • FIG. 8 The average size of crystals is calculated by Debye-Scherer method
  • FIG. 9 Transient optical microscope images
  • FIG. 10 SEM images and EDX test results obtained from solid and hollow synthesized fiber samples (a) Z100 before calcination, (b) Z100, (c) ZC5, (d) ZC25, (e) ZC50 after calcination
  • FIG. 11 The TG and DTA thermal analysis diagram shows the ZC25 sample
  • FTIR chart (A) Z100 sample before calcination, (B) Z100 sample after calcination and (C) ZC2 sample after calcination
  • the proposed design can be produced and used as a coating to add anti-viral, anti-bacterial, and anti-fungal properties to various woven and nonwoven fabrics in different medical and general masks, gowns, air filters, etc. Padding, exhaustion, spray, cavitation, ultrasonic bath, and coating layer using foam are among the methods of coating this product on fabrics.
  • the industrial application of this design is related to the field of fabrics, protective clothing, and fabric filters. Since this design can be applied on all kinds of clothes, breathing masks, hospital clothes, sheets, furniture, carpets, air conditioning system filters for industrial, hospital, home, & car use, as well as industrial and home water purification system filters, because, in addition to increasing the filtration power, they will also have antimicrobial (antiviral, antibacterial, and antifungal) properties.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Catalysts (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

La présente invention concerne un procédé de synthèse et de production de nanofibres composites d'oxyde de zinc-oxyde de cuivre ayant une formulation d'AZnO-BCuxO (A = 0,95, B = 0,05, X = 1,2) pouvant revêtir tous les types de tissus ayant des propriétés antimicrobiennes. Selon l'invention, les précurseurs d'acétate de zinc, d'acétate de cuivre ont été utilisés comme principaux fournisseurs d'oxyde de zinc et d'oxyde de cuivre, respectivement ; l'éthanol a été utilisé en tant que solvant et la polyvinylpyrrolidone était le polymère formant des fibres pour la synthèse. La production de nanofibres ZC5 composites creuses ayant la formulation chimique AZnO-BCuxO (A = 0,95, B = 0,05, X = 1,2) a des propriétés anti-coronavirus (n-SRAS-CoV2) avec un rendement > 99 % et la production de tissu anti-coronavirus selon un procédé de pulvérisation à jet sans air et pressage à chaud (simultanément) présente une efficacité > 99 % contre le coronavirus.
PCT/IB2022/052231 2021-03-10 2022-03-12 Synthèse et fabrication de nanofibres composites d'oxyde de cuivre-oxyde de zinc ayant des propriétés antimicrobiennes et pouvant revêtir divers tissus WO2022190071A1 (fr)

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IR13993011071 2021-03-10
IR139950140003011071 2021-03-10

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100137633A (ko) * 2009-06-23 2010-12-31 건국대학교 산학협력단 금속-유리 나노 복합체 분말
KR20150030289A (ko) * 2013-09-09 2015-03-20 인하대학교 산학협력단 산화주석-산화아연 나노섬유 이종구조물, 이의 제조방법 및 이를 이용한 환원가스 검출방법
AU2017203883A1 (en) * 2011-08-30 2017-06-29 Cornell University Metal and ceramic nanofibers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100137633A (ko) * 2009-06-23 2010-12-31 건국대학교 산학협력단 금속-유리 나노 복합체 분말
AU2017203883A1 (en) * 2011-08-30 2017-06-29 Cornell University Metal and ceramic nanofibers
KR20150030289A (ko) * 2013-09-09 2015-03-20 인하대학교 산학협력단 산화주석-산화아연 나노섬유 이종구조물, 이의 제조방법 및 이를 이용한 환원가스 검출방법

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