EP4127150A1 - Electrospun nanofibrous polymer membrane for use in personal protective equipment - Google Patents
Electrospun nanofibrous polymer membrane for use in personal protective equipmentInfo
- Publication number
- EP4127150A1 EP4127150A1 EP21780536.5A EP21780536A EP4127150A1 EP 4127150 A1 EP4127150 A1 EP 4127150A1 EP 21780536 A EP21780536 A EP 21780536A EP 4127150 A1 EP4127150 A1 EP 4127150A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- membrane
- layers
- textile material
- electrospinning
- winding speed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920005597 polymer membrane Polymers 0.000 title description 36
- 230000001681 protective effect Effects 0.000 title description 13
- 239000012528 membrane Substances 0.000 claims abstract description 143
- 238000001914 filtration Methods 0.000 claims abstract description 37
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 33
- 239000003443 antiviral agent Substances 0.000 claims abstract description 25
- 229920000642 polymer Polymers 0.000 claims abstract description 23
- 239000002121 nanofiber Substances 0.000 claims description 43
- 239000004753 textile Substances 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 39
- 238000004804 winding Methods 0.000 claims description 31
- 238000001523 electrospinning Methods 0.000 claims description 30
- 239000011148 porous material Substances 0.000 claims description 30
- 239000000835 fiber Substances 0.000 claims description 20
- 230000001775 anti-pathogenic effect Effects 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000002033 PVDF binder Substances 0.000 claims description 13
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims description 10
- 239000002105 nanoparticle Substances 0.000 claims description 10
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- 239000002114 nanocomposite Substances 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- -1 Zn2+ cations Chemical class 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- 150000001455 metallic ions Chemical class 0.000 claims description 5
- 239000002086 nanomaterial Substances 0.000 claims description 5
- 229930014626 natural product Natural products 0.000 claims description 5
- MRUAUOIMASANKQ-UHFFFAOYSA-O carboxymethyl-[3-(dodecanoylamino)propyl]-dimethylazanium Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC(O)=O MRUAUOIMASANKQ-UHFFFAOYSA-O 0.000 claims description 4
- 229940075468 lauramidopropyl betaine Drugs 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001508 alkali metal halide Inorganic materials 0.000 claims description 3
- 150000008045 alkali metal halides Chemical class 0.000 claims description 3
- 229960000800 cetrimonium bromide Drugs 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000007787 electrohydrodynamic spraying Methods 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000004711 α-olefin Substances 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229940069445 licorice extract Drugs 0.000 claims 1
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- 239000010410 layer Substances 0.000 description 40
- 239000000243 solution Substances 0.000 description 15
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- 239000002575 chemical warfare agent Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 5
- 239000000443 aerosol Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 5
- 206010022000 influenza Diseases 0.000 description 5
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000012266 salt solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 231100000481 chemical toxicant Toxicity 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
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- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 3
- 235000017382 Glycyrrhiza lepidota Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 229940010454 licorice Drugs 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 230000000241 respiratory effect Effects 0.000 description 3
- 235000014692 zinc oxide Nutrition 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 241001076416 Dendrobium tosaense Species 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002953 phosphate buffered saline Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000012552 review Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229960001296 zinc oxide Drugs 0.000 description 2
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 241000701386 African swine fever virus Species 0.000 description 1
- 208000035742 Air-borne transmission Diseases 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 241000711573 Coronaviridae Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000709661 Enterovirus Species 0.000 description 1
- 108010022355 Fibroins Proteins 0.000 description 1
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- 238000012695 Interfacial polymerization Methods 0.000 description 1
- 241001547436 Larrea nitida Species 0.000 description 1
- 241000351643 Metapneumovirus Species 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 239000004693 Polybenzimidazole Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 241000293869 Salmonella enterica subsp. enterica serovar Typhimurium Species 0.000 description 1
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- 235000013330 chicken meat Nutrition 0.000 description 1
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- 230000032798 delamination Effects 0.000 description 1
- 230000036557 dermal exposure Effects 0.000 description 1
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- 238000003618 dip coating Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005182 global health Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
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- 238000011065 in-situ storage Methods 0.000 description 1
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- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000003544 oxime group Chemical group 0.000 description 1
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- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical compound COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920001339 phlorotannin Polymers 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 229920006001 poly(vinyl alcohol-co-ethylene) Polymers 0.000 description 1
- 229920002480 polybenzimidazole Polymers 0.000 description 1
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- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 235000015277 pork Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 235000013594 poultry meat Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960003600 silver sulfadiazine Drugs 0.000 description 1
- UEJSSZHHYBHCEL-UHFFFAOYSA-N silver(1+) sulfadiazinate Chemical compound [Ag+].C1=CC(N)=CC=C1S(=O)(=O)[N-]C1=NC=CC=N1 UEJSSZHHYBHCEL-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62B—DEVICES, APPARATUS OR METHODS FOR LIFE-SAVING
- A62B23/00—Filters for breathing-protection purposes
- A62B23/02—Filters for breathing-protection purposes for respirators
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1692—Other shaped material, e.g. perforated or porous sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0004—Organic membrane manufacture by agglomeration of particles
- B01D67/00042—Organic membrane manufacture by agglomeration of particles by deposition of fibres, nanofibres or nanofibrils
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0004—Organic membrane manufacture by agglomeration of particles
- B01D67/00044—Organic membrane manufacture by agglomeration of particles by plasma spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1214—Chemically bonded layers, e.g. cross-linking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D71/06—Organic material
- B01D71/54—Polyureas; Polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/025—Types of fibres, filaments or particles, self-supporting or supported materials comprising nanofibres
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0457—Specific fire retardant or heat resistant properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0471—Surface coating material
- B01D2239/0478—Surface coating material on a layer of the filter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0631—Electro-spun
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0645—Arrangement of the particles in the filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/12—Special parameters characterising the filtering material
- B01D2239/1216—Pore size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2323/00—Details relating to membrane preparation
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- B01D2323/216—Surfactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2323/217—Emulgator or emulsion/foam forming agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/15—Use of additives
- B01D2323/218—Additive materials
- B01D2323/2181—Inorganic additives
- B01D2323/21817—Salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/39—Electrospinning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Definitions
- the present disclosure relates to materials for use in personal protective equipment.
- CARV infections include infections caused by a variety of viruses, including coronaviruses, rhinoviruses, influenza viruses, and metapneumovirus . See, e.g., Versluys, A.B., et al. “Morbidity and Mortality Associated With Respiratory Virus Infections in Allogeneic Hematopoietic Cell Transplant: Too Little Defense or Harmful Immunity?” Front, Microbiol 2018, 9, 2795-2795, doi;10.3389/ftnicb.2018.02795. Many CARV infections result in significant morbidity and mortality. For example, the Spanish flu pandemic of 1918 killed between 20 million and 50 million people worldwide.
- influenza pandemics are known to emerge cyclically.
- SARS-CoV-2 severe acute respiratory syndrome coronavirus 2
- Infectious respiratory pathogens are typically transmitted by droplet, aerosol, or airborne transmission of particles expelled from the respiratory tract of an infected person by coughing or sneezing, or in some cases by simple exhalation.
- facemasks and respirators have been developed that either mechanically intercept the infectious particles or that disarm the infectious particles using a variety of mechanisms. Therefore, many research and development efforts have been made to enhance the filtering efficiency Of facemasks and respirators.
- Nonwoven and woven materials commonly used as the base for type 5 CBPC have several disadvantages, such as poor permeability and filterability. See, e.g., Liu, Y crayon et al. , supra; Wingert, L., et al. “Filtering Performances of 20 Protective Fabrics against Solid Aerosols,” J. Occup. Environ . Hyg. 2019, 16, 592-606.
- antiviral agents are known that may be suitable for use in coatings or that may otherwise be integrated into personal protective equipment. See, eg., Tran, ⁇ . ⁇ ., ei al. “Silver Nanoparticles as Potential Antiviral Agents against African Swine Fever Virus,” Mater. Res . Express , 2020, 6(12), doi: 10.1Q88/2O53-1591/ab6ad8; Moreno, M.A., el al “Active Properties of Edible Marine Polysaccharide-Based Coatings Containing Larrea nitida Polyphenols Enriched Extract,” Food Hydrocoil.
- Electrospinning is a very useful technique that provides efficiency and uniformity of pore size. See, e.g., Ray, S.S., et al. “A Comprehensive Review: Electrospinning Technique for Fabrication and Surface Modification of Membranes for Water Treatment Application,” RSC Adv. 2016, 6(88), 85495-85514, doi: 10.1O39/C6RA14952A.
- Electrospinning is a process that uses an electric field to generate continuous fibers on a micrometer or nanometer scale. Electrospinning «tables direct control of the microstructure of a scaffold, including characteristics such as the fiber diameter, orientation, pore size, and porosity.
- Electrospun nanofibers have a wide range of applications. These include antibacterial food packaging, biomedical applications, and environmental applications. See, e.g., Lin, L., et at. “Cold Plasma Treated ' thyme Essential Oil/Silk Fibroin Nanofibers against Salmonella Typhimurium in Poultry Meat,” Food Packag. Shelf Life, 2019, 21, 100337; Zhu, Y., et at. “A Novel Polyethylene Oxi de/Dendrobium officinale Nanofiber: Preparation, Characterization and Application in Pork Packaging,” Food Packag. Shelf Life , 2019, 21, 100329; Surendhiran, D., et at.
- Electrospun nanofiber textiles have been considered promising candidates for CBPC. See, e.g., Lee, S vigorous et al. “Transport Properties of Layered Fabric Systems Based on Electrospun Nanofibers,” Fibers Polym. 2007, 8, 501-06; Bagherzadeh, R., et al. “Transport Properties of Multi-Layer Fabric Based on Electrospun Nanofiber Mate as a Breathable Barrier Textile Material,” Text. Res . J. 2012, 82, 70-76.
- Electrospun polymeric nanofibers may exhibit very high external surface area, excellent water vapor transport properties, and good mechanical strength. See, e.g., Huang,
- Choi, et al disclose fabricated polyurethane nanofibers functionalized by N- chloro hydantoin (NCH-PU). These nanofibers successfully decontaminated a simulant for V-type nerve gas (demeton-S-methyl). Choi, J., et al “N-Chloro Hydantoin Functionalized Polyurethane Fibers Toward Protective Cloth against Chemical Warfare Agents,” Polymer , 2018, 138, 146-55.
- Lee, et ah disclose functional PAN nanofiber webs to protect users from a simulant of a chemical warfare agent (CWA).
- CWA chemical warfare agent
- Zhao, et ah disclose metal-organic frameworks (MOFs) integrated into polyamide-6 nanofibers.
- MOFs metal-organic frameworks
- the MOF-nanofiber composites exhibited extraordinary reactivity for detoxifying CWAs.
- Zhao, J M et ah “Ultra-Fast Degradation of Chemical Warfare Agents Using MOF-Nanofiber Kebabs,” Angew. Chem . ini. Ed. 2016, 55, 13224-28.
- Antiviral agents have been incorporated into electrospun fibers for prevention of
- the membrane may be treated with one or more antimicrobial or antiviral agents.
- the membrane may be treated with an antiviral agent selected from the group consisting of graphene, nanoparticies, nanocomposites, multivalent metallic ions, and medicinal or other extracts from natural products.
- the treatment may preferably be a coating of one or more antiviral agents on the surface of the membrane.
- one or more antiviral agents may be impregnated into the nanofibrous membrane.
- the membrane may additionally or alternatively be impregnated with one or more metal-organic frameworks (MOFs).
- MOFs metal-organic frameworks
- the one or more MOFs may, for example, be one or more zirconium MOFs.
- the MOFs may provide filtration of chemical warfare agents (CWAs) and other toxic chemical agents and, in some embodiments, may also provide additional or alternate filtration of small particulates and pathogens.
- the disclosed membrane may preferably have a high filtering efficiency. ' Che porosity of the disclosed membrane may preferably be sufficient to provide breathabiliiy characteristics suitable for use as a facemask or respirator.
- the disclosed membrane is suitable for use in making facemasks and respirators that are highly resistant to infectious pathogens and/or other small particulates.
- FIG. I shows representative scanning electron microscopy (SEM) images of embodiments of the disclosed nanofibrous polymer membranes.
- FIG. 2 shows fiber diameter measurements and distribution for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 3 shows pore size distribution for representative samples of an embodiment of the disclosed nanofibrous polymer membrane as determined by mercury porosimeter analysis.
- FIG. 4 shows average porosity and the distribution of mean porosity for representa tive samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 5 shows mechanical tensile strength test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 6 shows filtration efficiency test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 7 shows latex filtration test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 8 shows viral filtration efficiency test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 9 shows bacteria filtration efficiency test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 10 shows flammability test results for a representative sample of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 11 shows antiviral properties test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 12 shows antibacterial properties test results for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- FIG. 13 shows how filtration efficiency is affected by the flow rate of aerosols through the membrane.
- FIG. 14 shows how the pressure drop across the membrane is affected by the flow rate of aerosols through the membrane.
- the membrane may be treated with one or more antimicrobial or antiviral agents.
- the membrane may be treated with an antiviral agent selected from the group consisting of graphene, nanoparticles, nanocomposites, multivalent metallic ions, and medicinal or other extracts from natural products.
- the treatment may preferably be a coating of one or more antiviral agents on the surface of the membrane.
- one or more antiviral agents may be impregnated into the nanofibrous membrane.
- the membrane may additionally or alternatively be impregnated with one or more metal-organic frameworks (MOFs).
- MOFs may, for example, be one or more zirconium MOFs.
- the MOFs may provide filtration of chemical warfare agents (CWAs) and other toxic chemical agents and, in some embodiments, may also provide additional or alternate filtration of small particulates and pathogens.
- CWAs chemical warfare agents
- the disclosed membrane may preferably have a high filtering efficiency.
- the porosity of (he disclosed membrane may preferably be sufficient to provide breathability characteristics suitable for use as a facemask or respirator.
- the disclosed membrane is suitable for use in making facemasks and respirators that are highly resistant to infectious pathogens and/or other small particulates.
- the disclosed membrane may preferably have a filtering efficiency of at least
- the disclosed membrane may preferably be capable of intercepting and exterminating infectious pathogens on its surfaces.
- the disclosed membrane is non-flammable.
- the disclosed membrane may be suitable for the production of non-flammable high-performance textiles.
- the disclosed membrane is ullrathin and lightweight
- the disclosed membrane does not degrade upon exposure to water or selected organic solvents such as ethanol or acetone.
- products made using the membrane may be washed and reused.
- the nanofibrous polymer membrane may be made from polyvinylidene fluoride (PVDF). In some alternate embodiments, the nanofibrous polymer membrane may be made from one or more TecophilicTM thermoplastic polyurethanes (TPlis). In some other alternate embodiments, the nanofibrous polymer membrane may be made from a blend of polyvinylidene fluoride and one or more TecophilicTM thermoplastic polyurethanes.
- PVDF polyvinylidene fluoride
- TPlis TecophilicTM thermoplastic polyurethanes
- e nanofibrous polymer membrane may be made using electrospinning techniques.
- a polymer is dissolved in a solvent prior to electrospinning.
- the solvent may preferably be selected from the group consisting of dimethyifonnamide (DMF), dimethylacetamide (DMA), hexafl uoroisopropanol (HFIP), acetone, water, or a combination thereof.
- a surfactant may be added to the polymer solution. Adding a surfactant to the polymer solution may promote a smaller fiber diameter and thus yield a membrane which has a smaller pore size and thus higher filtration efficiency.
- the surfactant may be one or more surfactants selected from the group consisting of cetrimomum bromide (CTAB), lauramidopropyl betaine (LAPS), and alpha olefin sulfonate (AOS).
- a salt or salt solution may be added to the polymer solution. Adding a salt or salt solution to the polymer solution may promote formation of thinner and more uniform fibers and may also reduce bead formation. By increasing charge density and conductivity, the presence of salts in the polymer solution promotes elongation of the spinning jet, which leads to the generation of thinner fibers.
- the salt or salt solution may be one or more salts or salt solutions selected from the group consisting of alkali metal halides and phosphate-buffered saline (PBS).
- the salt or salt solution may be one or more salts selected from the group consisting of sodium chloride (NaCl), lithium chloride (LiCI), and potassium chloride (KC3).
- the nanofibrous polymer membrane may be a single layer membrane or may alternatively be an integrated multi-layer membrane.
- the membrane may be composed of multiple integrated layers with distinguishable microstructure characteristics.
- a membrane that is composed of multiple integrated layers may provide enhanced filtration efficiency and high breathability.
- the enhanced filtration efficiency of an integrated multi-layer membrane may result from superior barrier protection against small pathogen particles.
- the integrated multi-layer membrane is composed of two layers with different pore sizes. In some alternate embodiments, the integrated multi-layer membrane is composed of three layers with two layers of equal pore size separated by a layer with a different pore size.
- the pore size may preferably be between 1 and 20 pm for the Iayer(s) with smaller pore size and between 20 and 200 pm for the iayer(s) with larger pore size.
- the layers of equal size may preferably have a larger pore size and foe layer in between these two layers may preferably have a smaller pore size. This configuration decreases the likelihood of delamination and also decreases the pressure drop that is generated as a gas passes through the multi-layer membrane, which corresponds to increased breathabiiity, without appreciably reducing the filtration efficiency of the membrane.
- the integrated multi-layer membrane is composed of three layers with three different pore sizes
- the pore size of the layers in integrated multi-layer membranes may be adjusted by adjusting the viscosity of the polymer solution and the electrospinning process conditions. Electrospinning process conditions may be adjusted to further stabilize the spinning jet used in the electrospinning setup. Solutions with lower viscosity will typically generate smaller pore size layers, and solutions with higher viscosity will typically generate larger pore size layers.
- the mechanical integrity and binding forces between layers of the membrane may be enhanced by electrospraying short fibers prior to electrospinning the subsequent layer. In some other embodiments, the mechanical integrity and binding forces between layers of the membrane may be enhanced by eiectrospinning wet fibers by decreasing the screen distance to generate a “tacky surface” prior to electrospinning the subsequent layer.
- the disclosed nanofibrous polymer membrane may be laminated onto a textile material.
- the nanofibers may be directly electrospun on nonwoven fabrics such as polyethylene terephthalate (PET), polypropylene (PP), and PET copolymers.
- PET copolymers results in enhanced adhesion between the nanofibers and textile, which thereby reduces peeling.
- the disclosed nanofibrous polymer membrane may be treated with an anti- pathogenic agent such as an antiviral agent selected from the group consisting of graphene, nanoparticles, nanocomposites, multivalent metallic ions, and medicinal or other extracts from natural products.
- the nanoparticles may preferably be metal nanoparticles such as silver nanoparticles or zinc nanoparticles.
- the nanocomposites may preferably be silver- doped titanium dioxide nanomaterials,
- multivalent metallic ions may preferably be metal ions such as Cu 2 + or Zn 2 + cations.
- the extracts from natural products may preferably be licorice extracts.
- the anti-pathogenic agent(s) may be physically coated on the surface of the membrane.
- the coating may be applied using chemical or electrochemical methods such as atomic layer deposition, vapor deposition methods such as physical vapor deposition (PVD) or chemical vapor deposition (CVD), spray coating methods such as plasma spraying or spray painting, or physical coating methods such dip-coating or spin-coating.
- chemical or electrochemical methods such as atomic layer deposition, vapor deposition methods such as physical vapor deposition (PVD) or chemical vapor deposition (CVD), spray coating methods such as plasma spraying or spray painting, or physical coating methods such dip-coating or spin-coating.
- the anti-pathogenic agent(s) may alternatively be incorporated into the membrane by blending the anti-pathogenic agents) into the polymer solution prior to electrospinning, thereby generating a membrane impregnated with the anti-pathogenic agenl(s).
- the disclosed nanofibrous polymer membrane may be impregnated with one or more metal-organic frameworks (MOFs), such as zirconium MOFs.
- MOFs metal-organic frameworks
- the MOFs may be incorporated into the membrane by blending the MOFs into the polymer solution prior to electrospinning, thereby generating a membrane impregnated with the MOFs.
- MOF-impregnation into the membrane may be in addition to coating with or impregnation of anti-pathogenic agent(s). In other embodiments, MOF- impregnation into the membrane may be an alternative to coating with or impregnation of anti-pathogenic agentfs).
- Membranes impregnated with MOFs may provide filtration of chemical warfare agents (CWAs) and other toxic chemical agents. In some embodiments, membranes impregnated with MOFs may also exhibit antiviral, antibacterial, or other anti- pathogenic properties.
- the MOFs described herein are necessarily distinct from the anti-pathogenic agents, such as antiviral or antibacterial agents, described herein. Rather, the anti-pathogenic agent may be a MOF or may alternatively be one of the other anti-pathogenic agents described herein. It is also not intended that the MOFs described herein wilt necessarily exhibit antiviral, antibacterial, or other anti-pathogenic properties. MOFs that are impregnated in the disclosed membranes may provide filtration of chemical warfare agents (CWAs) and other toxic chemical agents but, in some embodiments, may not exhibit antiviral, antibacterial, or other anti-pathogenic properties or provide filtration of small particulates.
- CWAs chemical warfare agents
- a textile material that is in the form of a textile material roll may be coated with one or more nanofiber layers by electrospinning, in some embodiments, one or more first nanofiber layers are electrospun on a first side of a textile material at a first winding speed, the textile material roll is flipped, and one or more second nanofiber layers are electrospun on a second side of the textile material at a second winding speed, where the first winding speed is different from the second winding speed.
- one or more first nanofiber layers are electrospun on a first side of a textile material at a first winding speed, and one or more second nanofiber layers are then electrospun on the first side of tire textile material at a second winding speed, where the first winding speed is different from the second winding speed.
- one or more first nanofiber layers are electrospun on a first side of a textile material at a first winding speed
- one or more second nanofiber layers are then electrospun on the first side of the textile material at a second winding speed
- the textile material roll is then fl ipped
- one or more third nanofiber layers are electrospun on a second side of the textile material at a third winding speed, where the first winding speed is different from the second winding speed.
- additional electrospinning steps may be added to include additional nanofiber layers of different thicknesses on one or both sides of the textile material.
- a facemask or respirator made from the disclosed nano fibrous polymer membrane is also disclosed herein.
- the facemask or respirator may preferably have a high filtration capacity and suitable breathability characteristics for comfortable use by a wearer.
- the disclosed facemask or respirator may preferably have a filtering efficiency of at least 95%, more preferably at least 98%, even more preferably at least 99%, and most preferably at least 99.9%.
- a method of making a facemask or respirator from the disclosed nanotibrous polymer membrane is also disclosed herein.
- the method may preferably allow the anti- pathogenic, physical, chemical, and mechanical properties to be fine-tuned according to the requirements of the specific application.
- sample preparation materials and methods are exemplary. Other suitable materials and methods may be used within the scope of the invention.
- Antiviral Treatment Two antiviral treatment methods were used: (I) the membranes were submerged in an aqueous dispersion containing antiviral particles, or (2) the antiviral agents were added to the polymer solutions to directly fabricate antiviral nanofibrous membranes.
- the antiviral agents used were 2% citric acid and silver, Ag-TtO 2 and Zn-Cu nanoparticles, and licorice extracts.
- membrane Fabrication was a roll-to-roll system, where a textile material was wound from one side to the other side and the nanofiber layer was laminated on the textile during the winding process. The thickness of the nanofiber layers was controlled by controlling the winding speed.
- Nanofibrous polymer membranes were characterized using scanning electron microscopy (SEM) imaging.
- FIG. 1 shows representative SEM images of an embodiment of the disclosed nanofibrous polymer membrane. The larger images show 2000X magnification, while each inset shows the respective 5000X magnification image. As shown in FIG. 1, the internal and external surfaces of each nanofiber membrane display consistent morphology between samples.
- FIG. 2 shows fiber diameter measurements and distribution for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- the average fiber diameter of representative samples was 0.224 pm, with a median fiber diameter of 0.210 pm and a standard deviation of 0.196.
- the average orientation was 79°, and the area coverage was 16%.
- FIG. 3 shows pore size distribution for representative samples of an embodiment of the disclosed nanofibrous polymer membrane as determined by mercury porosimeter analysis. The mean pore diameter was found to be 0.0025 pm.
- FIG. 4 shows average porosity and the distribution of mean porosity for representative samples of an embodiment of the disclosed nanofibrous polymer membrane.
- the average porosity as determined by gravimetric measurements was shown to be distributed around a center point of 78.5%. As shown in FIG. 4, all samples showed consistent porosity in the range of 75% to 83%, High porosity of the membrane is a critical requirement to increase the breathabiiity of a facemask or filter made from the membrane.
- FIG. 5 shows mechanical tensile strength test results tor representative samples of an embodiment of the disc l osed nanofibrous polymer membrane.
- a representative sample of an embodiment of the disclosed nanofibrous polymer membrane was also tested for filtration efficiency. The observed efficiency was 99.61% for 30 L/min, with a pressure loss of 1.265 mbar, and 99.85% for 95 L/min, with a pressure loss of 4.3 mbar.
- Table 1 shows a summary of test results for representative samples of an embodiment of the membrane.
- FiGs. 6-12 show test results for filtration efficiency, flammability, and antiviral and antimicrobial properties for representative samples of an embodiment of the disclosed nanofihrous polymer membrane.
- FIG. 13 shows how filtration efficiency is affected by the flow rate of aerosols through the membrane.
- FIG. 14 shows how the pressure drop across the membrane, which is a measure of breathability of the membrane, is affected by the flow rate of aerosols through the membrane.
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Ipc: B01D 39/16 20060101ALI20240305BHEP Ipc: B01D 71/54 20060101ALI20240305BHEP Ipc: B01D 71/34 20060101ALI20240305BHEP Ipc: B01D 71/02 20060101ALI20240305BHEP Ipc: A62B 23/02 20060101ALI20240305BHEP Ipc: A41D 13/11 20060101ALI20240305BHEP Ipc: B01D 67/00 20060101ALI20240305BHEP Ipc: C12Q 1/54 20060101ALI20240305BHEP Ipc: C12Q 1/00 20060101ALI20240305BHEP Ipc: C12N 9/04 20060101AFI20240305BHEP |