WO2022223062A1 - A method of preparing a continuous layer of porous carbon fibers, a continuous layer of porous carbon fibers prepared in this manner, an air filter and personal protective equipment comprising at least one such layer - Google Patents

A method of preparing a continuous layer of porous carbon fibers, a continuous layer of porous carbon fibers prepared in this manner, an air filter and personal protective equipment comprising at least one such layer Download PDF

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Publication number
WO2022223062A1
WO2022223062A1 PCT/CZ2022/050029 CZ2022050029W WO2022223062A1 WO 2022223062 A1 WO2022223062 A1 WO 2022223062A1 CZ 2022050029 W CZ2022050029 W CZ 2022050029W WO 2022223062 A1 WO2022223062 A1 WO 2022223062A1
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continuous layer
fibres
porous carbon
copper
layer consisting
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PCT/CZ2022/050029
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English (en)
French (fr)
Inventor
Jiri Militky
Jakub Wiener
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Technicka Univerzita V Liberci
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Priority to DE112022000011.2T priority Critical patent/DE112022000011B4/de
Publication of WO2022223062A1 publication Critical patent/WO2022223062A1/en

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • AHUMAN NECESSITIES
    • A41WEARING APPAREL
    • A41DOUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D13/00Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
    • A41D13/05Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
    • A41D13/11Protective face masks, e.g. for surgical use, or for use in foul atmospheres
    • AHUMAN NECESSITIES
    • A62LIFE-SAVING; FIRE-FIGHTING
    • A62BDEVICES, APPARATUS OR METHODS FOR LIFE-SAVING
    • A62B23/00Filters for breathing-protection purposes
    • A62B23/02Filters for breathing-protection purposes for respirators
    • AHUMAN NECESSITIES
    • A62LIFE-SAVING; FIRE-FIGHTING
    • A62BDEVICES, APPARATUS OR METHODS FOR LIFE-SAVING
    • A62B9/00Component parts for respiratory or breathing apparatus
    • A62B9/06Mouthpieces; Nose-clips
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055Carbonaceous material
    • B01D39/2065Carbonaceous material the material being fibrous
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01CCHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
    • D01C5/00Carbonising rags to recover animal fibres
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4209Inorganic fibres
    • D04H1/4242Carbon fibres
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282Addition polymers
    • D04H1/43Acrylonitrile series
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04Physical treatment combined with treatment with chemical compounds or elements
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/84Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising combined with mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/0241Types of fibres, filaments or particles, self-supporting or supported materials comprising electrically conductive fibres or particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04Additives and treatments of the filtering material
    • B01D2239/0407Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04Additives and treatments of the filtering material
    • B01D2239/0442Antimicrobial, antibacterial, antifungal additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04Additives and treatments of the filtering material
    • B01D2239/0464Impregnants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04Additives and treatments of the filtering material
    • B01D2239/0471Surface coating material
    • B01D2239/0492Surface coating material on fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/12Special parameters characterising the filtering material
    • B01D2239/1216Pore size
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/12Special parameters characterising the filtering material
    • B01D2239/1291Other parameters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/26Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof

Definitions

  • the invention relates to a method of preparing a continuous layer consisting of porous carbon fibres which is capable of being sterilized by Joule heat.
  • the invention further relates to a continuous layer consisting of porous carbon fibres functionalized with copper particles, which is prepared by this method.
  • the invention relates to an air filter and personal protective equipment for filtering inhaled and/or exhaled air comprising at least one continuous layer consisting of porous carbon fibres and functionalized with copper particles prepared by this method.
  • the object of the invention is to propose a method of preparing a continuous layer consisting of porous carbon fibres which would be in terms of practical use more suitable than a discontinuous layer.
  • the method of preparing a continuous layer consisting of porous carbon fibres according to the invention is based on carbonization of a continuous fibrous structure consisting entirely or at least of 80 % by weight of acrylic fibres under controlled heating conditions (carbonization temperature, heating rate and holding time).
  • the initial structure used is preferably a fibrous structure, which is otherwise unusable waste from various textile technologies.
  • Suitable initial fibrous structures include especially different types of non-woven structures, such as non-woven fabrics and webs - reinforced, bonded (e.g., needle-punched), cross-laid, vertically laid and/or laid in folds (e.g., by the method according to CZ 306111), having a total surface weight of 1200 to 36000 g/m 2 and a thickness of preferably 1 to 50 mm or more. Carbonization of such a structure takes place under the layer of charcoal or in an atmosphere of an oxidation-inhibiting gas, such as CO2, nitrogen, etc., at a temperature between 1200 and 1500 °C. The initial fibrous structure is gradually heated to this temperature at a rate of 300 to 400 °C/min and is kept at it for 3 to 10 minutes.
  • non-woven structures such as non-woven fabrics and webs - reinforced, bonded (e.g., needle-punched), cross-laid, vertically laid and/or laid in folds (e.g., by the method according to CZ 3061
  • This process results in carbonization during which hydrogen and part of the nitrogen and oxygen are removed from the structure of acrylic fibres and a structure consisting of 80 to 95 % by weight of carbon is produced; in some parts of the structure, under these conditions, graphitization occurs, during which the last nitrogen atoms are removed from the acrylic fibrous structure, resulting in the formation of more perfect carbon microcrystals and the formation of a more organized carbon structure - the so-called turbostratic structure, with controlled electrical conductivity, which consists of at least 99 % by weight of carbon.
  • the resulting continuous layer thus consists of microporous carbon fibres and retains the fibrous character and morphology of the initial fibrous structure; at the same time, it keeps approximately 45 to 60 % of its original weight and thickness and is thermally and electrically conductive, which allows, for example, its heating by Joule heat, e.g., for the purpose of sterilization (see below).
  • the resulting continuous layer suitably combines rugged interfibrous spaces with a diameter of approximately 50 nm to 3 pm, depending on the initial structure, with porous fibres with pores having a diameter of 2 to 50 nm formed by the escaping of gaseous products of carbonization from the fibrous material, which makes it possible for the continuous layer to reliably capture not only mechanical impurities, but also microorganisms, especially bacteria and some viruses from 50 nm in size, chemical contaminants in gaseous and liquid form, as well as odours of biological origin or generated by some chemicals, such as ammonia, formaldehyde, volatile organic compounds, etc., while having its original or even higher breathability.
  • some chemicals such as ammonia, formaldehyde, volatile organic compounds, etc.
  • a suitable method of stabilization is to expose the layer to a temperature of 250 to 320 °C in a pre-stressed state (under tensile stress) for 10 to 30 minutes in an oxidizing medium (e.g. in presence of air).
  • an oxidizing medium e.g. in presence of air.
  • the bonds in the macromolecule chain cyclize and crosslink the macromolecules by oxygen bridges, which is accompanied by a change in colour, a reduction in weight, and gas escape, whereby individual fibres become non-meltable.
  • the initial layer is heated to stabilization temperature at a rate of 35 °C per minute.
  • At least one copper precursor with a positive redox potential such as copper hydroxide (Cu(OH) 2 ), which is easily reduced to metal particles due to its positive redox potential, is incorporated into the initial structure.
  • the metal particles then bind to the fibres of the carbon structure being formed by means of van der Waals forces and complex bonds with nitrile groups (-CoN) and carboxyl groups (-COOH).
  • this precursor is introduced into the structure of the initial layer in the form of an aqueous reaction mixture using one of the known methods - for example, by immersion in a bath, by spraying, padding, etc.
  • the reaction mixture contains, per 1 litre, 3 to 10 g of at least one divalent copper salt, such as copper sulphate pentahydrate (CuS0 4 .5H 2 0), which subsequently forms copper hydroxide Cu(OH) 2 in the alkaline aqueous environment of the reaction mixture, 0.5 to 1 g of a reducing agent from the group consisting of sodium borohydride (NaBH 4 ), glucose, furfural and formaldehyde, 10 to 18 g of triethanolamine (TEA) acting as a complexing agent preventing copper separation from the reaction mixture, 5 to 10 g of salt containing sulphure and sodium from the group consisting of sodium thiosulphate (Na 2 S 2 0 3 ) and sodium sulphite (Na 2 S0 3 ), which stabilizes the reaction mixture and ensures the deposition of copper only on the surface of the fibres, and an addition of a base which adjusts the pH of this mixture to pH « 9.5.
  • a divalent copper salt
  • a preferred base is, for example, sodium hydroxide (NaOH), which at the same time also loosens the compact surface of acrylic fibres, helps to open pores and partially hydrolyzes nitrile groups (-CoN) in the structure of acrylic fibres and converts them to amide (-NH 2 ) and carboxyl groups (-COOH), resulting subsequently in increased copper deposition.
  • NaOH sodium hydroxide
  • This structure with the reaction mixture applied is then heated to a temperature of 80 °C to 95 °C for 10 to 30 minutes, reducing the copper precursor and attaching the formed copper particles to the fibrous surface of the initial layer.
  • reducing the copper precursor copper nanoparticles are formed, aggregating into larger units, and the agglomerates thus formed are deposited mainly on the surface of individual fibres and possibly also in their pores (see Fig. 3).
  • this process can be performed simultaneously or successively with two or more precursors of the same or different metal/metals.
  • a suitable combination is, for example, a combination of a copper precursor with a nickel precursor, e.g. nickel hydroxide (Ni(OH) 2 ), which in the alkaline environment of the reaction mixture is formed from a divalent nickel salt, such as nickel sulphate hexahydrate (NiS0 4 .6H 2 0), wherein during the reduction of these precursors, the nickel particles bind by means of van der Waals forces and complex bonds via nitrile groups (-CoN) and carboxyl groups (-COOH) by physical forces to the fibres of the fibrous structure, part of the copper particles subsequently binding to the nickel particles.
  • Ni(OH) 2 nickel hydroxide
  • NiS0 4 .6H 2 0 nickel sulphate hexahydrate
  • Nickel also acts as a fibre surface activator and copper reduction catalyst.
  • the amount of the copper precursor applied corresponds to 2 to 15 mg of elemental metal per 1 g of the continuous layer consisting of porous carbon fibres.
  • the amount of the nickel precursor in the reaction mixture is preferably equal to or less than the amount of the copper precursor in the reaction mixture, i.e., 1 to 15 mg (with a content of 1 to 10 g of divalent nickel salt in the reaction mixture).
  • the continuous layer consisting of porous carbon fibres according to the invention has a basis weight of 540 to 21600 g/m 2 and a thickness of 0.45 to 50 mm, wherein the copper particles are attached to the carbon fibres of the continuous layer in an amount of 2 to 15 mg per 1 g of the continuous layer.
  • the copper particles are attached to the carbon fibres of this continuous layer in an amount of 2 to 15 mg per 1 g of the continuous layer and nickel particles in an amount of 1 to 15 mg, wherein at least some of the copper particles are bound to the fibres of the layer through the nickel particles.
  • the thus prepared continuous layer consisting of porous carbon fibres has a wide range of uses. Due to its properties and high breathability, it can be used mainly as an active layer (i.e., layer with antimicrobial properties) of various types of gas filters, especially air filters, from air conditioning filters and similar systems of buildings or vehicles to filters of personal protective equipment for filtration of inhaled and/or exhaled air, including masks, half masks, surgical masks, face masks, etc. Thanks to a suitable combination of fibres with pores having a diameter of 2 to 50 nm and interfibrous spaces having a diameter of approximately 50 nm to 3 pm with high fragmentation
  • the continuous layer can reliably capture and eliminate microorganisms, especially bacteria, fungi and viruses in sizes from 50 nm, due to the action of copper with antimicrobial effect, its breathability being sufficient for comfortable breathing of the user, even at thicknesses above 30 mm.
  • this layer can adsorb some gaseous and liquid chemicals and remove odours of different origins, such as those generated by some chemicals, e.g., by ammonia, formaldehyde, volatile organic compounds, etc.
  • this layer is preferably provided with two electrical contacts on opposite sides, such as metal strips, flat or longitudinal textiles made of electrically conductive fibres (silver, carbon, copper, stainless steel of Inox type, etc.).
  • the form of attachment can typically be by conductive adhesives or encapsulation in a package with conductive contacts.
  • the air filter based on the use of the continuous layer of porous carbon fibres according to the invention comprises at least one such layer with a thickness of 1 to 50 mm, or even more, in combination with at least one layer of any filter material (preferably a HEPA type material or a filter material based on polymer fibres and/or nanofibres) with a melting point preferably above 170 ° C.
  • the layer of filter material serves to trap the mechanical impurities contained in the filtered air and at the same time provides mechanical support and protection to the continuous layer consisting of porous carbon fibres.
  • the binder used and the material of the other layers of the air filter must then have a softening point higher than the temperature to which the continuous layer consisting of porous carbon fibres is heated during sterilization.
  • a face mask for filtration of inhaled and/or exhaled air based on the use of the continuous layer consisting of porous carbon fibres according to the invention comprises at least one such layer with a thickness of 1 to 50 mm, optionally even more, in combination with at least one layer of any filter material (preferably a HEPA type material).
  • the layer of filter material serves to capture mechanical impurities contained in the inhaled and/or exhaled air and at the same time provides mechanical support and protection to the continuous layer consisting of porous carbon fibres.
  • the continuous layer consisting of porous carbon fibres is arranged between two layers of filter material (identical or different layers), wherein it is mechanically attached to at least one of them, preferably by means of dots of a suitable binder - either circumferentially or over the entire surface.
  • the binder used and the material of the other layers of the air filter must then have a softening point higher than the temperature to which the continuous layer consisting of porous carbon fibres is heated during sterilization.
  • Fig. 1 is a photograph of a needle punched non-woven fabric made from acrylic fibres
  • Fig. 2 is a photograph of a continuous layer consisting of porous carbon fibres prepared by carbonizing the non-woven fabric of Fig. 1
  • Fig. 3 is an SEM image of this continuous layer with indication of resolution.
  • Example 1 A needle-punched non-woven fabric made from acrylic fibres having a basis weight of 1300 g/m 2 (Fig. 1) was immersed for 1 minute in a reaction mixture which contained, per 1 litre, 14 g of triethanolamine, 0.5 g of sodium borohydride (NaBFU), 5 g of sodium sulphite (Na 2 S0 3 ), 1 g of sodium hydroxide (NaOFI), copper hydroxide (Cu(OFI)2) formed from 5 g of copper sulphate pentahydrate (CUSO4.5FI2O) and nickel hydroxide (Ni(OFI)2) formed from 1 g of nickel sulphate hexahydrate (NiSC .OFhO).
  • NaBFU sodium borohydride
  • Na 2 S0 3 sodium sulphite
  • NaOFI sodium hydroxide
  • Cu(OFI)2 copper hydroxide
  • Ni(OFI)2 nickel hydroxide
  • NiSC .OFhO nickel hydroxide
  • the non-woven fabric was heated to a temperature of 85 °C, at which temperature it was kept for 20 minutes, whereby the copper and nickel precursors were reduced and the formed nickel and copper particles attached to the surface of acrylic fibres, wherein some of the copper particles attached to the nickel particles on the surface of the acrylic fibres.
  • the surface area of the thus prepared layer consisting of porous carbon fibres was 210 m 2 /g.
  • the layer was electrically conductive, wherein, when connected to a 4 W power source, it was heated to a temperature of 140 °C in 3 minutes.
  • Example 2 The same non-woven fabric made from acrylic fibres as in Example 1 , after immersion in the same bath for 1 minute in a pre-stressed state, was stabilized at a temperature of 320 °C, at which temperature it was kept for 10 minutes. This layer was then heated at a rate of 300 ° C/min under the layer of charcoal to a temperature of 1300 °C, at which temperature it was kept for 5 minutes, during which it was carbonized and partially graphitized.
  • the surface area of the thus prepared layer consisting of porous carbon fibrous structures was 278 m 2 /g.
  • the layer was electrically conductive, wherein, when connected to a 4 W power source, it was heated to a temperature of 170 °C in 3 minutes.
  • Example 3 The same non-woven fabric made from acrylic fibres as in Example 1 , after immersion in the same bath for 1 minute in a pre-stressed state, was stabilized at a temperature of 320 °C, at which temperature it was kept for 30 minutes. The layer was then heated at a rate of 310 °C/min under the layer of charcoal to a temperature of 1200 °C, at which temperature it was kept for a period of 7 minutes, during which it was carbonized and partially graphitized. The surface area of the thus prepared layer consisting of porous carbon fibrous structures was 190 m 2 /g. The layer was electrically conductive, wherein, when connected to a 4 W power supply, it was heated to a temperature of 110 °C in 3 minutes.
  • Example 4 The same non-woven fabric made from acrylic fibres as in Example 1 , after immersion in the same bath for 1 minute in a pre-stressed state, was stabilized at a temperature of 320 °C, at which temperature it was kept for 30 minutes. The layer was
  • the surface area of the thus prepared layer consisting of porous carbon fibres was 257 m 2 /g.
  • the layer was electrically conductive, wherein, when connected to a 4 W power supply, it was heated within 3 minutes to a temperature of 125 °C.
  • a needle-punched non-woven fabric made from acrylic fibres with a basis weight of 2300 g/m 2 was immersed for 1 minute in a reaction mixture which contained, per 1 litre, 10 g of triethanolamine, 1 g of glucose, 7 g of Na 2 SC> 3 , 1 g of NaOH, CU(OH) 2 formed from 8 g of CuS0 4 .5H 2 0 a Ni(OH) 2 formed from 3 g of NiS0 4 .6H 2 0.
  • the non-woven fabric was heated to a temperature of 90 °C, at which temperature it was kept for 30 minutes, whereby the copper and nickel precursors were reduced and the formed nickel particles attached to the surface of acrylic fibres and the copper particles attached to the nickel particles.
  • the surface area of the thus prepared layer consisting of porous carbon fibres was 272 m 2 /g.
  • the layer was electrically conductive, wherein, when connected to a 4 W power supply, it was heated to 120 °C in 3 minutes.
  • a non-woven fabric made from acrylic fibres folded by the method according to CZ 306111 with a basis weight of 36000 g/m 2 was immersed for 5 minutes in a reaction mixture which contained, per 1 litre, 18 g of triethanolamine, 0.7 g of NaBH 4 , 10 g of Na 2 S 2 C> 3 , 1 g of NaOH, Cu(OH) 2 formed from 10 g of CuS0 4 .5H 2 0 and Ni(OH) 2 formed from 4 g of NiS0 4 .6H 2 0.
  • the fabric was heated to a temperature of 95 °C, at which temperature it was kept for 30 minutes, wherein the copper and nickel precursors were reduced and some of the nickel and copper particles formed attached to the surface of acrylic fibres, whereby some of the copper particles attached to the nickel particles on the surface of the acrylic fibres.
  • the surface area of the thus prepared layer consisting of porous carbon fibres was 326 m 2 /g.
  • the layer was electrically conductive, wherein, when connected to a 4 W power supply, it was heated to 140 °C in 3 minutes.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Business, Economics & Management (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Pulmonology (AREA)
  • Molecular Biology (AREA)
  • Wood Science & Technology (AREA)
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  • Manufacturing & Machinery (AREA)
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  • Physical Education & Sports Medicine (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
PCT/CZ2022/050029 2021-04-19 2022-03-11 A method of preparing a continuous layer of porous carbon fibers, a continuous layer of porous carbon fibers prepared in this manner, an air filter and personal protective equipment comprising at least one such layer WO2022223062A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE112022000011.2T DE112022000011B4 (de) 2021-04-19 2022-03-11 Verfahren zur Vorbereitung einer zusammenhängenden durch poröse Kohlenstofffasern gebildeten Schicht, zusammenhängende durch poröse Kohlenstofffasern gebildete und durch dieses Verfahren vorbereitete Schicht, Luftfilter und Mittel zur Filtration der eingeatmeten und/oder ausgeatmeten Luft

Applications Claiming Priority (2)

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