CN110438659A - A kind of preparation method of Waterproof Breathable nano-fiber composite film - Google Patents
A kind of preparation method of Waterproof Breathable nano-fiber composite film Download PDFInfo
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- CN110438659A CN110438659A CN201910606694.6A CN201910606694A CN110438659A CN 110438659 A CN110438659 A CN 110438659A CN 201910606694 A CN201910606694 A CN 201910606694A CN 110438659 A CN110438659 A CN 110438659A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-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
- D04H1/42—Non-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
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- Mechanical Engineering (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Nonwoven Fabrics (AREA)
- Laminated Bodies (AREA)
Abstract
The present invention relates to a kind of preparation methods of Waterproof Breathable nano-fiber composite film, belong to textile material technical field.The present invention is using polyacrylonitrile as primary raw material, and add Kynoar and polyurethane, prepare a kind of Waterproof Breathable nano-fiber composite film, there is high porosity with the waterproof humidity-permeant film of polyacrylonitrile nanofiber preparation, fibre diameter, the characteristics of small-bore, effectively improve the Waterproof Breathable effect of tunica fibrosa, polyacrylonitrile and Kynoar and polyurethane are tentatively obtained into hydrophobic microporous barrier by solution blending spinning, and the waterproof humidity-permeant film with certain welding structure is obtained in conjunction with heat treatment, effectively prevent the infiltration of liquid water, polyurethane is a kind of block polymer, carrier is provided in hydrophilic radical isopolarity group present on macromolecular chain segment for steam transfer, the hydrophobic performance that hydrophobic grouping on segment also makes polyurethane certain simultaneously, polyurethane, which is added, can assign nano-fiber composite film excellent comprehensive performance.
Description
Technical field
The present invention relates to a kind of preparation methods of Waterproof Breathable nano-fiber composite film, belong to textile material technical field.
Background technique
Fire-entry suit is the functional clothing for protecting one kind of line rescue personnel's personal safety special.It is to prevent respectively that it, which is acted on,
On the inside of heat (advection heat, conduction heat, radiant heat and hot steam etc.) intrusion clothes of kind form, human body is protected not come to harm.
Domestic typical case's fire-fighting class thermal protection clothes are multilayered structure, are followed successively by thermal insulation layer, moisture barrier and fire-retardant outer layer from inside to outside.Its
In, moisture barrier is combined by waterproof humidity-permeant film and bottom fabric layer, and effect is to prevent external high temperature fire demand water from penetrating into clothes
Internal layer scalds human body, and human body sweat vapour can be allowed to exclude in time again, guarantees its snugness of fit.Therefore the waterproof and moisture-permeable function of film
It is the key factor for influencing fireman's personal safety and dressing hot wet migration.
So-called Waterproof Breathable, referring to can prevent liquid water molecules from passing through, while the property for keeping water vapour freely to penetrate.Tool
The film or film class laminated fabric for having waterproofing and moisture-penetration performances are referred to as that fabric can be breathed again.According to moisture permeation mechanism, can incite somebody to action
Moisture permeable membrane is divided into two classes: microporous barrier and non-porous hydrophilic film.
Waterproofness refers to the performance that film or film surface material prevent the liquid water of certain pressure or kinetic energy from penetrating.Microporous barrier
Waterproof Breathable mechanism is the aperture using film itself between water droplet and moisture, and while obstructing extraneous water droplet, water steams
Vapour can be diffused into the external world by tortuous duct.Judge from macrophysics angle, by material surface pore size control certain
Range (0.2 ~ 20 μm).
There are apparent difference, the moisture-inhibiting principles of non-porous hydrophilic film with micropore Waterproof & Moisture Permeable Film for the moisture-inhibiting process of non-porous film
It is using hydrophilic segment or hydrophilic radical special inside film, the sweat vapour that human body is generated is from the high one side of humidity by inhaling
Wet-diffusion-moisture releasing process is transported to the low one side of humidity, to reach moisture-inhibiting purpose.
For water proof and moisture permeable material, should also have good water repellency, otherwise water vapour soaks film surface, film surface shape
At moisture film, the water vapour that can seriously hinder circulates outward, to make to generate sultry and tacky discomfort in clothes.
According to practical situations, waterproof humidity-permeant film can be generally divided into monofilm and composite membrane two major classes.Wherein, single layer
Film includes the hydrophilic film of single layer microporous film and single layer densification.
There are a large amount of diameters to be generally less than the 2 μm tiny micropore continuously penetrated through for micropore film surface, to ensure the anti-of microporous barrier
Water water vapour permeability.Micropore class waterproof humidity-permeant film has preferable waterproof, moisture-inhibiting, permeability and preferable feel.But it processes
The process is more complicated, there are certain requirements to coating agent and equipment.In addition, easily adsorbing dust in use, micropore is caused
Blocking is stain, and waterproofing and moisture-penetration performances is caused to decline.And micropore, when by external force, pore size becomes larger, film easily quilt
It destroys, shortens the service life of fabric.Meanwhile microporous barrier is windproof also poor.
The basic resin of fine and close hydrophilic film is by one group of soft chain segment and hard segment along dividing chain alternately arranged copolymer greatly
Composition, hard segment and soft chain segment are alternately arranged along macromolecular chain.The soft chain segment part that hydrophilic component is constituted, can adsorb aqueous vapor
Macromolecular, and transmit outward.Chemical structure and crosslinking degree determine the water vapour permeability of hydrophilic film, in general, film thickness
Smaller, film penetrability is better.Micropore is not present in non-porous hydrophilic film, and liquid water cannot pass through, therefore possess higher resistance to hydrostatic pressure,
With excellent wind-proof performance.And non-porous film has wider chemically-resistant, solvent nature, due to the frivolous softness of film, so that
The feel of laminated fabric is relatively close to initial single-ply cloth.But compared with microporous fabric, the penetrability of product is opposite
It is poor.In addition, by the moisture permeation mechanism of non-porous hydrophilic film it is not difficult to find that film lead it is wet before first happens is that hydrophilic radical pair
Process is accumulated in the absorption of hygroscopic water, thus wetting swelling easily occurs for film, is also easy to produce clammy sense, and when wet laminated fabric phase mutual friction is
Ear-piercing noise can be generated.
Microporous barrier cuts both ways with non-porous hydrophilic film, in practical applications, usually combines the two to form composite membrane.
Composite membrane refers to using microporous barrier as supporting layer, covers certain thickness hydrophilic non-porous film alternatively separating layer on its surface, this
The composite membrane that sample is constituted not only with moisture-permeability waterproof but also can play the isolated advantage of its selection.Made of being laminated such composite membrane
Composite material, which has, makes water droplet (or drop) that cannot penetrate into fabric, and the sweat gas that human body distributes can be spread by fabric and is transmitted to outside
Boundary, and can stop or be isolated toxic biochemical chemical substance, it is allowed to that the intracorporal unique effect of people cannot be invaded.Due to laminated film
Layers of material possess some special properties so that composite membrane is more extensive in application.Common laminated film is gone in packaging
It is widely used in the other industries such as industry and workers and peasants doctor, many functionality composite membranes are widely used in permeation filtration neck
Domain, proton exchange field, textile garment field etc..
Summary of the invention
The technical problems to be solved by the invention: for the problem that existing composite membrane water vapour permeability is poor, one kind is provided
The preparation method of Waterproof Breathable nano-fiber composite film.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) polyacrylonitrile, Kynoar, polyurethane are added in n,N-Dimethylformamide, in 30~40 DEG C of water-bath item
20~30min is stirred with 300~320r/min revolving speed under part, heat preservation obtains polymer solution；
(2) dimethyl silicone polymer, modified manometer silicon dioxide are added in polymer solution, in 30~40 DEG C of water bath condition
Under with 800~1000r/min revolving speed stir 1~2h, obtain polymer suspension；
(3) polymer suspension is placed in ultrasonic dispersing machine, 40~60min of ultrasonic disperse under room temperature obtains spinning solution；
(4) spinning solution is placed in the pipette of electrostatic spinning machine, is to receive with aluminium foil disc using stainless steel syringe needle as spray-hole
Disk carries out electrostatic spinning, obtains thin polymer film；
(5) thin polymer film is placed in in 60~80 DEG C of air dry oven dry 1~2h, room temperature cooling obtains Waterproof Breathable and receives
Rice composite fiber membrane.
The polyacrylonitrile, Kynoar, polyurethane, dimethyl silicone polymer, modified manometer silicon dioxide, N, N-
The parts by weight of dimethylformamide are 40~60 parts of polyacrylonitrile, 16~24 parts of Kynoar, 12~18 parts of polyurethane, 2~3
Part dimethyl silicone polymer, 4~6 parts of modified manometer silicon dioxides, 160~240 parts of n,N-Dimethylformamide.
The power of ultrasonic disperse described in step (3) is 400~500W.
The internal diameter of stainless steel syringe needle described in step (4) is 0.4~0.6mm, and the condition of electrostatic spinning is temperature 20~30
DEG C, relative humidity 40%~60%, 10~20kV of spinning voltage, spinning flow velocity be 0.6~1.0mL/h.
The average thickness of Waterproof Breathable nano-fiber composite film described in step (5) is 20~24 μm.
The specific preparation step of modified manometer silicon dioxide described in step (2) are as follows:
(1) deionized water is added to absolute ethanol, 6~8h is stirred with 100~120r/min revolving speed under room temperature, it is molten to obtain ethyl alcohol
Liquid；
(2) dimethyldichlorosilane, stearic acid are added in ethanol solution, under 30~40 DEG C of water bath condition with 180~
200r/min revolving speed stirs 12~16min, and heat preservation obtains modified solution；
(3) nano silica is added in modified solution, is turned under 30~40 DEG C of water bath condition with 800~1000r/min
Speed 30~40min of stirring, obtains suspension；
(4) suspension is placed in ultrasonic dispersing machine, 20~30min of ultrasonic vibration under room temperature obtains dispersion liquid；
(5) dispersion liquid is placed in a centrifuge, 15~20min is centrifugated with 4000~4500r/min revolving speed under room temperature, is removed
Layer solid, is washed 3~5 times, then be washed with deionized 1~3 time with dehydrated alcohol, is placed in 50~60 DEG C of baking oven dry 1
~2h, obtains modified manometer silicon dioxide.
The nano silica, dimethyldichlorosilane, stearic acid, dehydrated alcohol, deionized water parts by weight be
30~40 parts of nano silicas, 12~16 parts of dimethyldichlorosilanes, 6~8 parts of stearic acid, 60~80 parts of dehydrated alcohols, 30
~40 parts of deionized waters.
The power of ultrasonic vibration described in step (4) is 300~400W.
The average grain diameter of modified manometer silicon dioxide described in step (5) is 30~40nm.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention and adds Kynoar and polyurethane using polyacrylonitrile as primary raw material, prepares a kind of Waterproof Breathable and receives
Rice composite fiber membrane, polyacrylonitrile nanofiber has lesser fibre diameter and higher porosity, with polyacrylonitrile nano
The waterproof humidity-permeant film of fiber preparation has the characteristics that high porosity, fibre diameter, small-bore, and tunica fibrosa have interconnection more
Pore structure can spread a large amount of water vapour and prevent Liquid Penetrant, to effectively improve the Waterproof Breathable effect of tunica fibrosa
Polyacrylonitrile and Kynoar and polyurethane are tentatively obtained hydrophobic microporous barrier by solution blending spinning, and tied by fruit
It closes heat treatment and obtains the waterproof humidity-permeant film with certain welding structure, the addition of Kynoar can make fiber composite
Film surface is rich in fluorocarbon chain section and shows hydrophobic wetting characteristics, effectively prevents the infiltration of liquid water, and polyurethane is a kind of
Block polymer provides carrier in hydrophilic radical isopolarity group present on macromolecular chain segment for steam transfer, simultaneously
The hydrophobic performance that hydrophobic grouping on segment also makes polyurethane certain, it is excellent that addition polyurethane can assign nano-fiber composite film
Comprehensive performance；
(2) present invention prepares a kind of Waterproof Breathable Nanowire by addition modified manometer silicon dioxide and dimethyl silicone polymer
Composite membrane is tieed up, modified manometer silicon dioxide and dimethyl silicone polymer contain silicon oxygen bond, distance between Si-O key, Si-O-Si
Between strong angle is big, bond energy is big, and the silicon oxygen segment in dimethyl silicone polymer is shielded by methyl, so dimethyl silicone polymer
Segment it is soft, since silicon oxygen interchain interaction power is small, molal volume is big, so the surface tension of dimethyl silicone polymer
Small, the special molecular structure of polysiloxanes makes it have good water repellency, film forming and highly-breathable, can effectively improve
The waterproof performance and water vapour permeability of material；
(3) present invention uses method of electrostatic spinning, prepares a kind of Waterproof Breathable nano-fiber composite film, and electrostatic spinning technique is electrification
Polymer solution or fusant form the drop of suspension under the synergistic effect of self gravity, own viscosity and surface tension,
Charged drop, by the stretching action of electric field force, is injected into thread, solidifies during stretching in electrostatic field, is finally receiving
End obtains fibre and gathers, and conjunction object jet stream is fine by, by high-speed stretch, being finally deposited on and receiving on substrate under the action of electrostatic field
Tunica fibrosa made of dimension stacks has tridimensional network, can effectively improve the mechanical property of polymer nanocomposite membrane and steady
It is qualitative.
Specific embodiment
According to parts by weight, 30~40 parts of nano silicas, 12~16 parts of dimethyldichlorosilanes, 6~8 are weighed respectively
Part stearic acid, 60~80 parts of dehydrated alcohols, 30~40 parts of deionized waters, deionized water is added to absolute ethanol, under room temperature with
100~120r/min revolving speed stirs 6~8h, obtains ethanol solution, and dimethyldichlorosilane, stearic acid are added in ethanol solution,
12~16min is stirred with 180~200r/min revolving speed under 30~40 DEG C of water bath condition, heat preservation obtains modified solution, by nanometer
Silica be added modified solution in, under 30~40 DEG C of water bath condition with 800~1000r/min revolving speed stirring 30~
40min obtains suspension, and suspension is placed in ultrasonic dispersing machine, under room temperature with the power ultrasonic vibration 20 of 300~400W~
30min obtains dispersion liquid, and dispersion liquid is placed in a centrifuge, under room temperature with 4000~4500r/min revolving speed centrifuge separation 15~
20min takes lower layer's solid, is washed 3~5 times with dehydrated alcohol, then is washed with deionized 1~3 time, is placed in 50~60 DEG C of baking
Dry 1~2h, obtains the modified manometer silicon dioxide of 30~40nm of average grain diameter in case；Again according to parts by weight, 40 are weighed respectively
~60 parts of polyacrylonitrile, 16~24 parts of Kynoar, 12~18 parts of polyurethane, 2~3 parts of dimethyl silicone polymers, 4~6 parts
Polyacrylonitrile, Kynoar, polyurethane are added for modified manometer silicon dioxide, 160~240 parts of n,N-Dimethylformamide
In n,N-Dimethylformamide, 20~30min is stirred with 300~320r/min revolving speed under 30~40 DEG C of water bath condition, is protected
Temperature obtains polymer solution, dimethyl silicone polymer, modified manometer silicon dioxide is added in polymer solution, at 30~40 DEG C
Water bath condition under with 800~1000r/min revolving speed stir 1~2h, obtain polymer suspension, polymer suspension be placed in super
In sound wave dispersion machine, with power 40~60min of ultrasonic disperse of 400~500W under room temperature, spinning solution is obtained, spinning solution is placed in quiet
It is to receive disk with aluminium foil disc using the stainless steel syringe needle of 0.4~0.6mm of internal diameter as spray-hole in the pipette of Electrospun machine,
Under conditions of 20~30 DEG C of temperature, relative humidity 40%~60%, 10~20kV of spinning voltage, with the flow velocity of 0.6~1.0mL/h
Electrostatic spinning is carried out, thin polymer film is obtained, thin polymer film is placed in in 60~80 DEG C of air dry oven dry 1~2h, often
Temperature is cooling, obtains 20~24 μm of average thickness of Waterproof Breathable nano-fiber composite film.
Embodiment 1
According to parts by weight, 30 parts of nano silicas, 12 parts of dimethyldichlorosilanes, 6 parts of stearic acid, 60 parts of nothings are weighed respectively
Water-ethanol, 30 parts of deionized waters, deionized water is added to absolute ethanol, and is stirred 6h under room temperature with 100r/min revolving speed, is obtained second
Alcoholic solution dimethyldichlorosilane, stearic acid is added in ethanol solution, with 180r/min revolving speed under 30 DEG C of water bath condition
Stir 12min, heat preservation, obtain modified solution, by nano silica be added modified solution in, under 30 DEG C of water bath condition with
800r/min revolving speed stirs 30min, obtains suspension, suspension is placed in ultrasonic dispersing machine, with the power of 300W under room temperature
Ultrasonic vibration 20min, obtains dispersion liquid, and dispersion liquid is placed in a centrifuge, with the centrifuge separation of 4000r/min revolving speed under room temperature
15min takes lower layer's solid, is washed 3 times with dehydrated alcohol, then is washed with deionized 1 time, is placed in 50 DEG C of baking oven dry
1h obtains the modified manometer silicon dioxide of average grain diameter 30nm；Again according to parts by weight, 40 parts of polyacrylonitrile, 16 parts are weighed respectively
Kynoar, 12 parts of polyurethane, 2 parts of dimethyl silicone polymers, 4 parts of modified manometer silicon dioxides, 160 parts of N, N- dimethyl methyl
Amide, by polyacrylonitrile, Kynoar, polyurethane be added n,N-Dimethylformamide in, under 30 DEG C of water bath condition with
300r/min revolving speed stirs 20min, and heat preservation obtains polymer solution, and dimethyl silicone polymer, modified manometer silicon dioxide are added
In polymer solution, 1h is stirred with 800r/min revolving speed under 30 DEG C of water bath condition, polymer suspension is obtained, polymer is hanged
Supernatant liquid is placed in ultrasonic dispersing machine, with the power ultrasonic disperse 40min of 400W under room temperature, obtains spinning solution, spinning solution is placed in
It is to receive disk, In with aluminium foil disc using the stainless steel syringe needle of internal diameter 0.4mm as spray-hole in the pipette of electrostatic spinning machine
Under conditions of 20 DEG C of temperature, relative humidity 40%, spinning voltage 10kV, electrostatic spinning is carried out with the flow velocity of 0.6mL/h, must be polymerize
Thin polymer film, is placed in 60 DEG C of air dry oven dry 1h by object film, and room temperature cooling obtains 20 μm of average thickness of waterproof
Moisture-inhibiting nano-fiber composite film.
Embodiment 2
According to parts by weight, 35 parts of nano silicas, 14 parts of dimethyldichlorosilanes, 7 parts of stearic acid, 70 parts of nothings are weighed respectively
Water-ethanol, 35 parts of deionized waters, deionized water is added to absolute ethanol, and is stirred 7h under room temperature with 110r/min revolving speed, is obtained second
Alcoholic solution dimethyldichlorosilane, stearic acid is added in ethanol solution, with 190r/min revolving speed under 35 DEG C of water bath condition
Stir 14min, heat preservation, obtain modified solution, by nano silica be added modified solution in, under 35 DEG C of water bath condition with
900r/min revolving speed stirs 35min, obtains suspension, suspension is placed in ultrasonic dispersing machine, with the power of 350W under room temperature
Ultrasonic vibration 25min, obtains dispersion liquid, and dispersion liquid is placed in a centrifuge, with the centrifuge separation of 4250r/min revolving speed under room temperature
18min takes lower layer's solid, is washed 4 times with dehydrated alcohol, then is washed with deionized 2 times, is placed in 55 DEG C of baking oven dry
1h obtains the modified manometer silicon dioxide of average grain diameter 35nm；Again according to parts by weight, 50 parts of polyacrylonitrile, 20 parts are weighed respectively
Kynoar, 15 parts of polyurethane, 2 parts of dimethyl silicone polymers, 5 parts of modified manometer silicon dioxides, 200 parts of N, N- dimethyl methyl
Amide, by polyacrylonitrile, Kynoar, polyurethane be added n,N-Dimethylformamide in, under 35 DEG C of water bath condition with
310r/min revolving speed stirs 25min, and heat preservation obtains polymer solution, and dimethyl silicone polymer, modified manometer silicon dioxide are added
In polymer solution, 1h is stirred with 900r/min revolving speed under 35 DEG C of water bath condition, polymer suspension is obtained, polymer is hanged
Supernatant liquid is placed in ultrasonic dispersing machine, with the power ultrasonic disperse 50min of 450W under room temperature, obtains spinning solution, spinning solution is placed in
It is to receive disk, In with aluminium foil disc using the stainless steel syringe needle of internal diameter 0.5mm as spray-hole in the pipette of electrostatic spinning machine
Under conditions of 25 DEG C of temperature, relative humidity 50%, spinning voltage 15kV, electrostatic spinning is carried out with the flow velocity of 0.8mL/h, must be polymerize
Thin polymer film, is placed in 70 DEG C of air dry oven dry 1h by object film, and room temperature cooling obtains 22 μm of average thickness of waterproof
Moisture-inhibiting nano-fiber composite film.
Embodiment 3
According to parts by weight, 40 parts of nano silicas, 16 parts of dimethyldichlorosilanes, 8 parts of stearic acid, 80 parts of nothings are weighed respectively
Water-ethanol, 40 parts of deionized waters, deionized water is added to absolute ethanol, and is stirred 8h under room temperature with 120r/min revolving speed, is obtained second
Alcoholic solution dimethyldichlorosilane, stearic acid is added in ethanol solution, with 200r/min revolving speed under 40 DEG C of water bath condition
Stir 16min, heat preservation, obtain modified solution, by nano silica be added modified solution in, under 40 DEG C of water bath condition with
1000r/min revolving speed stirs 40min, obtains suspension, suspension is placed in ultrasonic dispersing machine, with the power of 400W under room temperature
Ultrasonic vibration 30min, obtains dispersion liquid, and dispersion liquid is placed in a centrifuge, with the centrifuge separation of 4500r/min revolving speed under room temperature
20min takes lower layer's solid, is washed 5 times with dehydrated alcohol, then is washed with deionized 3 times, is placed in 60 DEG C of baking oven dry
2h obtains the modified manometer silicon dioxide of average grain diameter 40nm；Again according to parts by weight, 60 parts of polyacrylonitrile, 24 parts are weighed respectively
Kynoar, 18 parts of polyurethane, 3 parts of dimethyl silicone polymers, 6 parts of modified manometer silicon dioxides, 240 parts of N, N- dimethyl methyl
Amide, by polyacrylonitrile, Kynoar, polyurethane be added n,N-Dimethylformamide in, under 40 DEG C of water bath condition with
320r/min revolving speed stirs 30min, and heat preservation obtains polymer solution, and dimethyl silicone polymer, modified manometer silicon dioxide are added
In polymer solution, 2h is stirred with 1000r/min revolving speed under 40 DEG C of water bath condition, polymer suspension is obtained, by polymer
Suspension is placed in ultrasonic dispersing machine, with the power ultrasonic disperse 60min of 500W under room temperature, obtains spinning solution, spinning solution is set
It is to receive disk with aluminium foil disc using the stainless steel syringe needle of internal diameter 0.6mm as spray-hole in the pipette of electrostatic spinning machine,
Under conditions of 30 DEG C of temperature, relative humidity 60%, spinning voltage 20kV, electrostatic spinning is carried out with the flow velocity of 1.0mL/h, is obtained poly-
Object film is closed, thin polymer film is placed in in 80 DEG C of air dry oven dry 2h, room temperature cooling obtains 24 μm of average thickness anti-
Water moisture-inhibiting nano-fiber composite film.
Reference examples: the Waterproof Breathable nano-fiber composite film of Dongguan company production.
The Waterproof Breathable nano-fiber composite film that embodiment and reference examples are prepared is detected, specific detection is such as
Under:
Waterproofing and moisture-penetration performances test: referring to GB/T4744-19887 " textile fabric water permeability resistance measures hydrostatic test ", to 5 pieces
Composite membrane carries out resistance to hydrostatic pressure (the digital seepage of water tester of YG825E type) test, selects supercharge method, and the rate of rise is
1.0KPa/min is averaged the waterproof performance for indicating composite membrane.With the computermatic fabric moisture transmission instrument of YG601- type, reference standard
GB/T12704-91 " fabric moisture transmission quantity measuring method moisture-inhibiting agar diffusion method/method A moisture absorption method ", tests the water vapour permeability of composite membrane.
Tensile property test: referring to GB/T1040.1-2006 " measurement of plastic tensile performance ", sample is cut into 10mm
Wide strip utilizes the tensile property of Instron5582 test composite membrane, effective tensile elongation 25mm, tensile speed 5mm/
min。
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples |
| Resistance to hydrostatic pressure/Pa | 1504.9 | 1502.1 | 1513.6 | 6240.3 |
| Vapor transfer rate/g/m2·24h | 6233.5 | 6235..1 | 6239.6 | 3515.9 |
| Tensile strength/MPa | 6.5 | 6.6 | 6.7 | 2.1 |
As shown in Table 1, Waterproof Breathable nano-fiber composite film prepared by the present invention has good waterproofing and moisture-penetration performances and mechanics
Performance.
Claims (9)
1. a kind of preparation method of Waterproof Breathable nano-fiber composite film, which is characterized in that specific preparation step are as follows:
(1) polyacrylonitrile, Kynoar, polyurethane are added in n,N-Dimethylformamide, in 30~40 DEG C of water-bath item
20~30min is stirred with 300~320r/min revolving speed under part, heat preservation obtains polymer solution；
(2) dimethyl silicone polymer, modified manometer silicon dioxide are added in polymer solution, in 30~40 DEG C of water bath condition
Under with 800~1000r/min revolving speed stir 1~2h, obtain polymer suspension；
(3) polymer suspension is placed in ultrasonic dispersing machine, 40~60min of ultrasonic disperse under room temperature obtains spinning solution；
(4) spinning solution is placed in the pipette of electrostatic spinning machine, is to receive with aluminium foil disc using stainless steel syringe needle as spray-hole
Disk carries out electrostatic spinning, obtains thin polymer film；
(5) thin polymer film is placed in in 60~80 DEG C of air dry oven dry 1~2h, room temperature cooling obtains Waterproof Breathable and receives
Rice composite fiber membrane.
2. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 1, which is characterized in that described
Polyacrylonitrile, Kynoar, polyurethane, dimethyl silicone polymer, modified manometer silicon dioxide, n,N-Dimethylformamide
Parts by weight be 40~60 parts of polyacrylonitrile, 16~24 parts of Kynoar, 12~18 parts of polyurethane, 2~3 parts of poly dimethyl silicon
Oxygen alkane, 4~6 parts of modified manometer silicon dioxides, 160~240 parts of n,N-Dimethylformamide.
3. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 1, which is characterized in that step
(3) power of the ultrasonic disperse described in is 400~500W.
4. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 1, which is characterized in that step
(4) internal diameter of the stainless steel syringe needle described in is 0.4~0.6mm, and the condition of electrostatic spinning is 20 ~ 30 DEG C of temperature, relative humidity 40%
~60%, 10~20kV of spinning voltage, spinning flow velocity are 0.6~1.0mL/h.
5. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 1, which is characterized in that step
(5) average thickness of the Waterproof Breathable nano-fiber composite film described in is 20~24 μm.
6. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 1, which is characterized in that step
(2) the specific preparation step of the modified manometer silicon dioxide described in are as follows:
(1) deionized water is added to absolute ethanol, 6~8h is stirred with 100~120r/min revolving speed under room temperature, it is molten to obtain ethyl alcohol
Liquid；
(2) dimethyldichlorosilane, stearic acid are added in ethanol solution, under 30~40 DEG C of water bath condition with 180~
200r/min revolving speed stirs 12~16min, and heat preservation obtains modified solution；
(3) nano silica is added in modified solution, is turned under 30~40 DEG C of water bath condition with 800~1000r/min
Speed 30~40min of stirring, obtains suspension；
(4) suspension is placed in ultrasonic dispersing machine, 20~30min of ultrasonic vibration under room temperature obtains dispersion liquid；
(5) dispersion liquid is placed in a centrifuge, 15~20min is centrifugated with 4000~4500r/min revolving speed under room temperature, is removed
Layer solid, is washed 3~5 times, then be washed with deionized 1~3 time with dehydrated alcohol, is placed in 50~60 DEG C of baking oven dry 1
~2h, obtains modified manometer silicon dioxide.
7. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 6, which is characterized in that described
Nano silica, dimethyldichlorosilane, stearic acid, dehydrated alcohol, deionized water parts by weight be 30~40 parts of nanometers
Silica, 12~16 parts of dimethyldichlorosilanes, 6~8 parts of stearic acid, 60~80 parts of dehydrated alcohols, 30~40 parts of deionizations
Water.
8. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 6, which is characterized in that step
(4) power of the ultrasonic vibration described in is 300~400W.
9. a kind of preparation method of Waterproof Breathable nano-fiber composite film according to claim 6, which is characterized in that step
(5) average grain diameter of the modified manometer silicon dioxide described in is 30~40nm.
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