CN111501199B - Gradient electrostatic spinning composite fiber material for N95 mask - Google Patents

Gradient electrostatic spinning composite fiber material for N95 mask Download PDF

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Publication number
CN111501199B
CN111501199B CN202010335066.1A CN202010335066A CN111501199B CN 111501199 B CN111501199 B CN 111501199B CN 202010335066 A CN202010335066 A CN 202010335066A CN 111501199 B CN111501199 B CN 111501199B
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spinning
electrostatic spinning
polyether
fiber layer
ketone
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CN111501199A (en
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王文爽
沈文齐
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Guangxi baolingkang Medical Equipment Co.,Ltd.
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Guangxi Baolingkang Medical Equipment Co ltd
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    • 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
    • D04H1/70Non-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
    • D04H1/72Non-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
    • D04H1/728Non-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
    • 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
    • A41WEARING APPAREL
    • A41DOUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D31/00Materials specially adapted for outerwear
    • A41D31/02Layered materials
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • 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
    • 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
    • D04H1/4326Condensation or reaction polymers
    • 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
    • D04H1/4326Condensation or reaction polymers
    • D04H1/435Polyesters
    • 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
    • D04H1/4374Non-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 using different kinds of webs, e.g. by layering webs
    • 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
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005Synthetic yarns or filaments
    • D04H3/007Addition polymers
    • 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
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005Synthetic yarns or filaments
    • D04H3/009Condensation or reaction polymers
    • 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
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005Synthetic yarns or filaments
    • D04H3/009Condensation or reaction polymers
    • D04H3/011Polyesters
    • 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
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/10Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/06Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyethers
    • D10B2331/061Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyethers polyetherketones, polyetheretherketones, e.g. PEEK

Abstract

The invention discloses a gradient electrostatic spinning composite fiber material for an N95 mask, which sequentially comprises the following components from inside to outside: the composite material comprises a polyacrylonitrile electrostatic spinning fiber layer, a first polyether-ether-ketone electrostatic spinning fiber layer, a second polyether-ether-ketone electrostatic spinning fiber layer, a third polyether-ether-ketone electrostatic spinning fiber layer and a polymethyl methacrylate electrostatic spinning fiber layer. The gradient electrostatic spinning composite fiber material for the N95 mask can improve the filtering efficiency of the mask and prolong the effective service time of the mask.

Description

Gradient electrostatic spinning composite fiber material for N95 mask
Technical Field
The invention relates to the technical field of protective filtering layered materials, in particular to a gradient electrostatic spinning composite fiber material for an N95 mask.
Background
Model N95 mask is one of 9 types of particle protection masks certified by NIOSH (National Institute for Occupational Safety and Health, National Institute). N95 is not a specific product name, and as long as the product meets the N95 standard and passes NIOSH examination, the product can be called an N95 type mask, and the filtering efficiency of the product on particles with the aerodynamic diameter of 0.075 μm +/-0.020 μm can reach more than 95%.
The prior art CN107354585A discloses an electrostatic spinning membrane with adsorption and filtration properties, and a preparation method and application thereof. The preparation method of the electrostatic spinning membrane comprises the following steps: (1) dissolving polylactic acid-glycolic acid and/or polycaprolactone in hexafluoroisopropanol solvent, and stirring to obtain solution A; (2) stirring the solution A at room temperature overnight, and then carrying out electrostatic spinning treatment on the solution A to obtain a membrane; (3) the obtained membrane was freeze-dried and vacuum-dried. The membrane material of the invention is characterized by a multi-layer porous membrane material consisting of fibers with the diameter range of 400-900 nm.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a gradient electrostatic spinning composite fiber material for an N95 mask, which can improve the filtering efficiency of the mask and prolong the effective service time of the mask.
In order to achieve the above object, the present invention provides a gradient electrospinning composite fiber material for N95 mask, which comprises, from inside to outside: the composite material comprises a polyacrylonitrile electrostatic spinning fiber layer, a first polyether-ether-ketone electrostatic spinning fiber layer, a second polyether-ether-ketone electrostatic spinning fiber layer, a third polyether-ether-ketone electrostatic spinning fiber layer and a polymethyl methacrylate electrostatic spinning fiber layer.
In a preferred embodiment, the polyacrylonitrile electrospun fiber layer is prepared by the following method: dissolving polyacrylonitrile in a DMF solvent and uniformly stirring to obtain a polyacrylonitrile spinning solution, wherein the concentration of the polyacrylonitrile spinning solution is 20-25 wt%; and (3) carrying out electrostatic spinning by using the polyacrylonitrile spinning solution to form a polyacrylonitrile electrostatic spinning fiber layer.
In a preferred embodiment, the formation of the polyacrylonitrile electrospun fiber layer by electrospinning specifically comprises: the spinning voltage is 20-25kV, the injection speed of the spinning solution is 3-5mL/h, the spinning distance is 10-15cm, the receiving speed of a winding roller is 70-90r/min, and the thickness of the polyacrylonitrile electrostatic spinning fiber layer is 40-50 microns.
In a preferred embodiment, the first polyetheretherketone electrospun fiber layer is prepared by the method of: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a first polyether-ether-ketone spinning solution, wherein the concentration of the first polyether-ether-ketone spinning solution is 15-20 wt%; and (3) carrying out electrostatic spinning by using the first polyether-ether-ketone spinning solution to form a first polyether-ether-ketone electrostatic spinning fiber layer.
In a preferred embodiment, the first polyetheretherketone electrospun fiber layer formed by electrospinning is specifically: the spinning voltage is 20-25kV, the injection speed of the spinning solution is 1-3mL/h, the spinning distance is 20-25cm, the receiving speed of a winding roller is 50-60r/min, and the thickness of the first polyether-ether-ketone electrostatic spinning fiber layer is 30-40 micrometers.
In a preferred embodiment, the second polyetheretherketone electrospun fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a second polyether-ether-ketone spinning solution, wherein the concentration of the second polyether-ether-ketone spinning solution is 30-35 wt%; and (3) carrying out electrostatic spinning by using the second polyether ether ketone spinning solution to form a second polyether ether ketone electrostatic spinning fiber layer.
In a preferred embodiment, the second polyetheretherketone electrospun fiber layer formed by electrospinning is specifically: the spinning voltage is 30-35kV, the injection speed of the spinning solution is 1-3mL/h, the spinning distance is 10-15cm, the receiving speed of a winding roller is 100-120r/min, and the thickness of the second polyether ether ketone electrostatic spinning fiber layer is 70-80 microns.
In a preferred embodiment, the third polyetheretherketone electrospun fiber layer is prepared by the process of: dissolving polyether-ether-ketone in a hexafluoroisopropanol solvent and uniformly stirring to obtain a third polyether-ether-ketone spinning solution, wherein the concentration of the third polyether-ether-ketone spinning solution is 21-26 wt%; and (3) carrying out electrostatic spinning by using the third polyether ether ketone spinning solution to form a third polyether ether ketone electrostatic spinning fiber layer.
In a preferred embodiment, the third polyetheretherketone electrospun fiber layer formed by electrospinning is specifically: the spinning voltage is 25-30kV, the injection speed of the spinning solution is 2-4mL/h, the spinning distance is 15-20cm, the receiving speed of a winding roller is 80-90r/min, and the thickness of the third polyether ether ketone electrostatic spinning fiber layer is 40-50 microns.
In a preferred embodiment, the polymethyl methacrylate electrospun fiber layer is prepared by the following method: dissolving polymethyl methacrylate in dimethyl siloxane and uniformly stirring to obtain a polymethyl methacrylate spinning solution, wherein the concentration of the polymethyl methacrylate spinning solution is 35-40 wt%; performing electrostatic spinning by using the polymethyl methacrylate spinning solution to form a polymethyl methacrylate electrostatic spinning fiber layer;
the polymethyl methacrylate electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 15-20kV, the injection speed of the spinning solution is 2-4mL/h, the spinning distance is 10-15cm, the receiving speed of a winding roller is 70-90r/min, and the thickness of the polymethyl methacrylate electrostatic spinning fiber layer is 40-50 microns.
Compared with the prior art, the gradient electrostatic spinning composite fiber material for the N95 mask has the following advantages:
the N95 mask, and even the more protective N99 mask, is the most important device to protect individuals and physicians during major outbreaks of infection. For the general environment, it can be said that the N95 mask is the most important sharp instrument for preventing the widespread spread of respiratory infectious diseases. The problems of the existing N95 mask mainly include several aspects, the first is that the air resistance of the mask material is large, which causes the breathing of people wearing the mask to be unsmooth; secondly, the filtration efficiency of the mask material degrades rapidly during use, leading to the need for frequent replacement of the mask by the user or to the infection of the user without knowing the failure of the mask. To the problem of gauze mask air resistance, the theory that is generally acknowledged at present is that gauze mask filtration efficiency and gauze mask resistance are positive correlation, and the general resistance of the big gauze mask of filtration efficiency is also big, in order to solve this problem, need provide a filtration efficiency and improve the material that speed is higher than resistance improvement speed, in addition, hope this kind of material can not take place rapid deterioration in the use performance, guarantee the effective live time of gauze mask. The invention provides a mask material which can basically meet the requirements of the two aspects.
Drawings
Fig. 1 is a schematic structural view of a gradient electrospun composite fibrous material for an N95 mask according to an embodiment of the present invention.
Fig. 2 is an SEM photograph (x5000) of a second peek electrospun fiber layer prepared according to the proposed method of the invention.
Fig. 3 is an SEM photograph (x5000) of a first peek electrospun fiber layer prepared according to the proposed method of the invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component. All raw materials of the chemical reagent can be purchased by chemical product stores, and the purity grade of the reagent can be adjusted according to actual needs. As used herein, the molecular weight determination method of a polymer may be a direct consultation with a reagent store that is generally capable of providing data on the molecular weight of the polymer required for the electrospinning process. It should be clear to those skilled in the art that what is proposed herein is only the material used for the core filter portion of the N95 mask, and not the mask itself, and what components the final mask product specifically includes (e.g., whether or not to include the metal strips of the nasal prong portions, etc.) is common general knowledge in the art and is not of concern in this application, and will not be described in detail herein. The test standard of the application refers to the standard of national standard GB2626-2006 self-priming filtering type particulate-proof respirator for respiratory protection articles, which defines the standard of N95 respirator in China, wherein the requirement that the resistance of the N95 respirator with the filtering efficiency higher than 95% must be less than 250Pa is included. The method for testing the filtering efficiency and the mask resistance is carried out according to the national standard GB 2626-2006.
Fig. 1 is a schematic structural view of a gradient electrospun composite fibrous material for an N95 mask according to an embodiment of the present invention. As shown in the figure, the gradient electrospinning composite fiber material for the N95 mask of the present invention sequentially comprises from inside to outside: polyacrylonitrile electrospun fiber layer 101, first polyetheretherketone electrospun fiber layer 102, second polyetheretherketone electrospun fiber layer 103, third polyetheretherketone electrospun fiber layer 104, and polymethylmethacrylate electrospun fiber layer 105.
Fig. 2 is an SEM photograph (x5000) of a second peek electrospun fiber layer prepared according to the proposed method of the present invention, wherein the contrast of the photograph is adjusted by the shooting unit as required in order to better represent the morphology of the fiber filament of the present application. Fig. 3 is an SEM photograph (x5000) of a first peek electrospun fiber layer prepared according to the proposed method of the invention. It will be understood by those skilled in the art that the photographic samples were prepared by preparing a single layer of the second or first peek electrospun fiber layer on a receiving roll according to the methods of the present application and then taking SEM photographs of the samples directly.
Example 1
The gradient electrostatic spinning composite fiber material for the N95 mask sequentially comprises from inside to outside: the composite material comprises a polyacrylonitrile electrostatic spinning fiber layer, a first polyether-ether-ketone electrostatic spinning fiber layer, a second polyether-ether-ketone electrostatic spinning fiber layer, a third polyether-ether-ketone electrostatic spinning fiber layer and a polymethyl methacrylate electrostatic spinning fiber layer. The polyacrylonitrile electrostatic spinning fiber layer is prepared by the following method: dissolving polyacrylonitrile in a DMF solvent and uniformly stirring to obtain a polyacrylonitrile spinning solution, wherein the concentration of the polyacrylonitrile spinning solution is 20 wt%; and (3) carrying out electrostatic spinning by using the polyacrylonitrile spinning solution to form a polyacrylonitrile electrostatic spinning fiber layer. The formation of the polyacrylonitrile electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 20kV, the injection speed of the spinning solution is 3mL/h, the spinning distance is 10cm, the receiving speed of a winding roller is 70r/min, and the thickness of the polyacrylonitrile electrostatic spinning fiber layer is 40 microns. The first polyetheretherketone electrospun fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a first polyether-ether-ketone spinning solution, wherein the concentration of the first polyether-ether-ketone spinning solution is 15 wt%; and (3) carrying out electrostatic spinning by using the first polyether-ether-ketone spinning solution to form a first polyether-ether-ketone electrostatic spinning fiber layer. The first polyether-ether-ketone electrostatic spinning fiber layer formed through electrostatic spinning specifically comprises the following steps: the spinning voltage is 20kV, the injection speed of the spinning solution is 1mL/h, the spinning distance is 20cm, the receiving speed of a winding roller is 50r/min, and the thickness of the first polyether-ether-ketone electrostatic spinning fiber layer is 30 micrometers. The second poly ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a second polyether-ether-ketone spinning solution, wherein the concentration of the second polyether-ether-ketone spinning solution is 30 wt%; and (3) carrying out electrostatic spinning by using the second polyether ether ketone spinning solution to form a second polyether ether ketone electrostatic spinning fiber layer. The second polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 30kV, the injection speed of the spinning solution is 1mL/h, the spinning distance is 10cm, the receiving speed of a winding roller is 100r/min, and the thickness of the second polyether ether ketone electrostatic spinning fiber layer is 70 micrometers. The third polyether ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in a hexafluoroisopropanol solvent and uniformly stirring to obtain a third polyether-ether-ketone spinning solution, wherein the concentration of the third polyether-ether-ketone spinning solution is 21 wt%; and (3) carrying out electrostatic spinning by using the third polyether ether ketone spinning solution to form a third polyether ether ketone electrostatic spinning fiber layer. The third polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following steps: the spinning voltage is 25kV, the injection speed of the spinning solution is 2mL/h, the spinning distance is 15cm, the receiving speed of a winding roller is 80r/min, and the thickness of the third polyether ether ketone electrostatic spinning fiber layer is 40 micrometers. The polymethyl methacrylate electrostatic spinning fiber layer is prepared by the following method: dissolving polymethyl methacrylate in dimethyl siloxane and uniformly stirring to obtain a polymethyl methacrylate spinning solution, wherein the concentration of the polymethyl methacrylate spinning solution is 35 wt%; performing electrostatic spinning by using the polymethyl methacrylate spinning solution to form a polymethyl methacrylate electrostatic spinning fiber layer; the polymethyl methacrylate electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 15kV, the injection speed of the spinning solution is 2mL/h, the spinning distance is 10cm, the receiving speed of a winding roller is 70r/min, and the thickness of the polymethyl methacrylate electrostatic spinning fiber layer is 40 micrometers.
Example 2
The gradient electrostatic spinning composite fiber material for the N95 mask sequentially comprises from inside to outside: the composite material comprises a polyacrylonitrile electrostatic spinning fiber layer, a first polyether-ether-ketone electrostatic spinning fiber layer, a second polyether-ether-ketone electrostatic spinning fiber layer, a third polyether-ether-ketone electrostatic spinning fiber layer and a polymethyl methacrylate electrostatic spinning fiber layer. The polyacrylonitrile electrostatic spinning fiber layer is prepared by the following method: dissolving polyacrylonitrile in a DMF solvent and uniformly stirring to obtain a polyacrylonitrile spinning solution, wherein the concentration of the polyacrylonitrile spinning solution is 25 wt%; and (3) carrying out electrostatic spinning by using the polyacrylonitrile spinning solution to form a polyacrylonitrile electrostatic spinning fiber layer. The formation of the polyacrylonitrile electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 25kV, the injection speed of the spinning solution is 5mL/h, the spinning distance is 15cm, the receiving speed of a winding roller is 90r/min, and the thickness of the polyacrylonitrile electrostatic spinning fiber layer is 50 microns. The first polyetheretherketone electrospun fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a first polyether-ether-ketone spinning solution, wherein the concentration of the first polyether-ether-ketone spinning solution is 20 wt%; and (3) carrying out electrostatic spinning by using the first polyether-ether-ketone spinning solution to form a first polyether-ether-ketone electrostatic spinning fiber layer. The first polyether-ether-ketone electrostatic spinning fiber layer formed through electrostatic spinning specifically comprises the following steps: the spinning voltage is 25kV, the injection speed of the spinning solution is 3mL/h, the spinning distance is 25cm, the receiving speed of a winding roller is 60r/min, and the thickness of the first polyether-ether-ketone electrostatic spinning fiber layer is 40 micrometers. The second poly ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a second polyether-ether-ketone spinning solution, wherein the concentration of the second polyether-ether-ketone spinning solution is 35 wt%; and (3) carrying out electrostatic spinning by using the second polyether ether ketone spinning solution to form a second polyether ether ketone electrostatic spinning fiber layer. The second polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 35kV, the injection speed of the spinning solution is 3mL/h, the spinning distance is 15cm, the receiving speed of a winding roller is 120r/min, and the thickness of the second polyether ether ketone electrostatic spinning fiber layer is 80 microns. The third polyether ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in a hexafluoroisopropanol solvent and uniformly stirring to obtain a third polyether-ether-ketone spinning solution, wherein the concentration of the third polyether-ether-ketone spinning solution is 26 wt%; and (3) carrying out electrostatic spinning by using the third polyether ether ketone spinning solution to form a third polyether ether ketone electrostatic spinning fiber layer. The third polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following steps: the spinning voltage is 30kV, the injection speed of the spinning solution is 4mL/h, the spinning distance is 20cm, the receiving speed of a winding roller is 90r/min, and the thickness of the third polyether ether ketone electrostatic spinning fiber layer is 50 micrometers. The polymethyl methacrylate electrostatic spinning fiber layer is prepared by the following method: dissolving polymethyl methacrylate in dimethyl siloxane and uniformly stirring to obtain a polymethyl methacrylate spinning solution, wherein the concentration of the polymethyl methacrylate spinning solution is 40 wt%; performing electrostatic spinning by using the polymethyl methacrylate spinning solution to form a polymethyl methacrylate electrostatic spinning fiber layer; the polymethyl methacrylate electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 20kV, the injection speed of the spinning solution is 4mL/h, the spinning distance is 15cm, the receiving speed of a winding roller is 90r/min, and the thickness of the polymethyl methacrylate electrostatic spinning fiber layer is 50 micrometers.
Example 3
The gradient electrostatic spinning composite fiber material for the N95 mask sequentially comprises from inside to outside: the composite material comprises a polyacrylonitrile electrostatic spinning fiber layer, a first polyether-ether-ketone electrostatic spinning fiber layer, a second polyether-ether-ketone electrostatic spinning fiber layer, a third polyether-ether-ketone electrostatic spinning fiber layer and a polymethyl methacrylate electrostatic spinning fiber layer. The polyacrylonitrile electrostatic spinning fiber layer is prepared by the following method: dissolving polyacrylonitrile in a DMF solvent and uniformly stirring to obtain a polyacrylonitrile spinning solution, wherein the concentration of the polyacrylonitrile spinning solution is 22 wt%; and (3) carrying out electrostatic spinning by using the polyacrylonitrile spinning solution to form a polyacrylonitrile electrostatic spinning fiber layer. The formation of the polyacrylonitrile electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 22kV, the injection speed of the spinning solution is 4mL/h, the spinning distance is 12cm, the receiving speed of a winding roller is 80r/min, and the thickness of the polyacrylonitrile electrostatic spinning fiber layer is 45 micrometers. The first polyetheretherketone electrospun fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a first polyether-ether-ketone spinning solution, wherein the concentration of the first polyether-ether-ketone spinning solution is 18 wt%; and (3) carrying out electrostatic spinning by using the first polyether-ether-ketone spinning solution to form a first polyether-ether-ketone electrostatic spinning fiber layer. The first polyether-ether-ketone electrostatic spinning fiber layer formed through electrostatic spinning specifically comprises the following steps: the spinning voltage is 22kV, the injection speed of the spinning solution is 2mL/h, the spinning distance is 22cm, the receiving speed of a winding roller is 55r/min, and the thickness of the first polyether-ether-ketone electrostatic spinning fiber layer is 35 microns. The second poly ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a second polyether-ether-ketone spinning solution, wherein the concentration of the second polyether-ether-ketone spinning solution is 32 wt%; and (3) carrying out electrostatic spinning by using the second polyether ether ketone spinning solution to form a second polyether ether ketone electrostatic spinning fiber layer. The second polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 32kV, the injection speed of the spinning solution is 2mL/h, the spinning distance is 12cm, the receiving speed of a winding roller is 110r/min, and the thickness of the second polyether ether ketone electrostatic spinning fiber layer is 75 micrometers. The third polyether ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in a hexafluoroisopropanol solvent and uniformly stirring to obtain a third polyether-ether-ketone spinning solution, wherein the concentration of the third polyether-ether-ketone spinning solution is 23 wt%; and (3) carrying out electrostatic spinning by using the third polyether ether ketone spinning solution to form a third polyether ether ketone electrostatic spinning fiber layer. The third polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following steps: the spinning voltage is 27kV, the injection speed of the spinning solution is 3mL/h, the spinning distance is 18cm, the receiving speed of a winding roller is 85r/min, and the thickness of the third polyether ether ketone electrostatic spinning fiber layer is 45 micrometers. The polymethyl methacrylate electrostatic spinning fiber layer is prepared by the following method: dissolving polymethyl methacrylate in dimethyl siloxane and uniformly stirring to obtain a polymethyl methacrylate spinning solution, wherein the concentration of the polymethyl methacrylate spinning solution is 37 wt%; performing electrostatic spinning by using the polymethyl methacrylate spinning solution to form a polymethyl methacrylate electrostatic spinning fiber layer; the polymethyl methacrylate electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 18kV, the injection speed of the spinning solution is 3mL/h, the spinning distance is 12cm, the receiving speed of a winding roller is 80r/min, and the thickness of the polymethyl methacrylate electrostatic spinning fiber layer is 45 micrometers.
Comparative example 1
The composite fiber material sequentially comprises from inside to outside: polyacrylonitrile electrostatic spinning fibrous layer, first polyether ether ketone electrostatic spinning fibrous layer and polymethyl methacrylate electrostatic spinning fibrous layer. Wherein the thickness of the first polyetheretherketone electrospun fiber layer was 105 μm, and the preparation method of the first polyetheretherketone electrospun fiber layer was the same as in example 3. Other parameters, processes and steps are the same as those of example 3.
Comparative example 2
The polyacrylonitrile electrostatic spinning fiber layer is prepared by the following method: and (3) dissolving polyacrylonitrile in a DMF solvent and uniformly stirring to obtain a polyacrylonitrile spinning solution, wherein the concentration of the polyacrylonitrile spinning solution is 30 wt%. Other parameters, processes and steps are the same as those of example 3.
Comparative example 3
The formation of the polyacrylonitrile electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 30kV, the injection speed of the spinning solution is 6mL/h, the spinning distance is 20cm, the receiving speed of a winding roller is 100r/min, and the thickness of the polyacrylonitrile electrostatic spinning fiber layer is 45 micrometers. Other parameters, processes and steps are the same as those of example 3.
Comparative example 4
The first polyetheretherketone electrospun fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a first polyether-ether-ketone spinning solution, wherein the concentration of the first polyether-ether-ketone spinning solution is 30 wt%. Other parameters, processes and steps are the same as those of example 3.
Comparative example 5
The first polyether-ether-ketone electrostatic spinning fiber layer formed through electrostatic spinning specifically comprises the following steps: the spinning voltage is 30kV, the injection speed of the spinning solution is 4mL/h, the spinning distance is 30cm, the receiving speed of a winding roller is 70r/min, and the thickness of the first polyether-ether-ketone electrostatic spinning fiber layer is 50 micrometers. Other parameters, processes and steps are the same as those of example 3.
Comparative example 6
The second poly ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a second polyether-ether-ketone spinning solution, wherein the concentration of the second polyether-ether-ketone spinning solution is 25 wt%. Other parameters, processes and steps are the same as those of example 3.
Comparative example 7
The second polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 25kV, the injection speed of the spinning solution is 1mL/h, the spinning distance is 5cm, the receiving speed of a winding roller is 70r/min, and the thickness of the second polyether ether ketone electrostatic spinning fiber layer is 90 micrometers. Other parameters, processes and steps are the same as those of example 3.
Comparative example 8
The third polyether ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a third polyether-ether-ketone spinning solution, wherein the concentration of the third polyether-ether-ketone spinning solution is 30 wt%. Other parameters, processes and steps are the same as those of example 3.
Comparative example 9
The third polyether ether ketone electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following steps: the spinning voltage is 35kV, the injection speed of the spinning solution is 5mL/h, the spinning distance is 25cm, the receiving speed of a winding roller is 100r/min, and the thickness of the third polyether ether ketone electrostatic spinning fiber layer is 60 micrometers. Other parameters, processes and steps are the same as those of example 3.
Comparative example 10
The polymethyl methacrylate electrostatic spinning fiber layer is prepared by the following method: dissolving polymethyl methacrylate in dimethyl siloxane and uniformly stirring to obtain a polymethyl methacrylate spinning solution, wherein the concentration of the polymethyl methacrylate spinning solution is 25 wt%. Other parameters, processes and steps are the same as those of example 3.
Comparative example 11
The formation of the polymethyl methacrylate electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 25kV, the injection speed of the spinning solution is 5mL/h, the spinning distance is 20cm, the receiving speed of a winding roller is 50r/min, and the thickness of the polymethyl methacrylate electrostatic spinning fiber layer is 60 micrometers. Other parameters, processes and steps are the same as those of example 3.
Each of the samples prepared in examples 1 to 3 and comparative examples 1 to 11 was tested with reference to national standards for filtration efficiency (%), air resistance (Pa), and filtration efficiency maintenance (%), wherein the filtration efficiency maintenance (%) refers to a ratio of the filtration efficiency remaining in the sample to the filtration efficiency originally measured after filtering for 120min using the relevant sample in an environment of 30 degrees celsius and 85% humidity.
TABLE 1
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (1)

1. The gradient electrostatic spinning composite fiber material for the N95 mask is characterized by sequentially comprising the following components from inside to outside: the polyacrylonitrile electrostatic spinning fiber layer is prepared by the following method: dissolving polyacrylonitrile in a DMF solvent and uniformly stirring to obtain a polyacrylonitrile spinning solution, wherein the concentration of the polyacrylonitrile spinning solution is 20-25 wt%; the polyacrylonitrile spinning solution is used for electrostatic spinning to form a polyacrylonitrile electrostatic spinning fiber layer, and the formation of the polyacrylonitrile electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 20-25kV, the injection speed of the spinning solution is 3-5mL/h, the spinning distance is 10-15cm, the receiving speed of a winding roller is 70-90r/min, the thickness of the polyacrylonitrile electrostatic spinning fiber layer is 40-50 microns, and the first polyether-ether-ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a first polyether-ether-ketone spinning solution, wherein the concentration of the first polyether-ether-ketone spinning solution is 15-20 wt%; performing electrostatic spinning by using the first polyether-ether-ketone spinning solution to form a first polyether-ether-ketone electrostatic spinning fiber layer, wherein the forming of the first polyether-ether-ketone electrostatic spinning fiber layer through electrostatic spinning specifically comprises the following steps: the spinning voltage is 20-25kV, the injection speed of the spinning solution is 1-3mL/h, the spinning distance is 20-25cm, the receiving speed of a winding roller is 50-60r/min, the thickness of the first polyether-ether-ketone electrostatic spinning fiber layer is 30-40 micrometers, and the second polyether-ether-ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in hexafluoroisopropanol solvent and uniformly stirring to obtain a second polyether-ether-ketone spinning solution, wherein the concentration of the second polyether-ether-ketone spinning solution is 30-35 wt%; performing electrostatic spinning by using the second polyether ether ketone spinning solution to form a second polyether ether ketone electrostatic spinning fiber layer, wherein the electrostatic spinning for forming the second polyether ether ketone electrostatic spinning fiber layer specifically comprises the following steps: the spinning voltage is 30-35kV, the injection speed of the spinning solution is 1-3mL/h, the spinning distance is 10-15cm, the receiving speed of a winding roller is 100-120r/min, the thickness of the second polyether ether ketone electrostatic spinning fiber layer is 70-80 microns, and the third polyether ether ketone electrostatic spinning fiber layer is prepared by the following method: dissolving polyether-ether-ketone in a hexafluoroisopropanol solvent and uniformly stirring to obtain a third polyether-ether-ketone spinning solution, wherein the concentration of the third polyether-ether-ketone spinning solution is 21-26 wt%; performing electrostatic spinning by using the third polyether ether ketone spinning solution to form a third polyether ether ketone electrostatic spinning fiber layer, wherein the electrostatic spinning for forming the third polyether ether ketone electrostatic spinning fiber layer specifically comprises the following steps: the spinning voltage is 25-30kV, the injection speed of the spinning solution is 2-4mL/h, the spinning distance is 15-20cm, the receiving speed of a winding roller is 80-90r/min, the thickness of the third polyether ether ketone electrostatic spinning fiber layer is 40-50 microns, and the polymethyl methacrylate electrostatic spinning fiber layer is prepared by the following method: dissolving polymethyl methacrylate in dimethyl siloxane and uniformly stirring to obtain a polymethyl methacrylate spinning solution, wherein the concentration of the polymethyl methacrylate spinning solution is 35-40 wt%; performing electrostatic spinning by using the polymethyl methacrylate spinning solution to form a polymethyl methacrylate electrostatic spinning fiber layer; the polymethyl methacrylate electrostatic spinning fiber layer formed by electrostatic spinning specifically comprises the following components: the spinning voltage is 15-20kV, the injection speed of the spinning solution is 2-4mL/h, the spinning distance is 10-15cm, the receiving speed of a winding roller is 70-90r/min, and the thickness of the polymethyl methacrylate electrostatic spinning fiber layer is 40-50 microns.
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