CN107326653A - Nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof - Google Patents
Nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof Download PDFInfo
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- CN107326653A CN107326653A CN201710357563.XA CN201710357563A CN107326653A CN 107326653 A CN107326653 A CN 107326653A CN 201710357563 A CN201710357563 A CN 201710357563A CN 107326653 A CN107326653 A CN 107326653A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/38—Polyurethanes
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- D—TEXTILES; PAPER
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The present invention relates to nanofiber waterproof ventilated membrane of a kind of ultra-high throughput and preparation method thereof, belong to textile technology materials synthesis field.The nanofiber waterproof ventilated membrane of the ultra-high throughput is made up of following two components：The nanometer silicon dioxide particle and polymer nanofibre film of bifunctional group modification.The nano particle that the nano fibrous membrane is modified using bifunctional group is as interfibrous adhesion agent, the water proofing property of the rub resistance that can not only strengthen membrane material but also the roughness increase tunica fibrosa that can increase nanofiber surface.The Waterproof Breathable function membrane aperture of ultra-high throughput prepared by the present invention is small, porosity is high, and has enhanced adhesion structure, has the characteristics of water pressure resistance is high, moisture-inhibiting flux is high, intensity is high, moisture-inhibiting flux >=18000g/m when for Waterproof Breathable field2/ d, water pressure resistance >=100kPa, with extensive actual application prospect.
Description
Technical field
The present invention relates to a kind of waterproof ventilated membrane, and in particular to a kind of nanofiber waterproof ventilated membrane of ultra-high throughput and its
Preparation method.
Background technology
Waterproof moisture permeating fabric (Waterproof＆Moisture Permeable Fabric) generally also makes waterproof and breathable knit
Thing, foreign countries commonly referred to as can breathe fabric (Waterproof but Breathable Fabric), be one kind can rain-proof,
The fabric can perspire again, breathed freely.It is that the mankind are the infringement for resisting the Nature, is occurred in the case of improving constantly self-protection
's.In wearing process, water can not be impregnated with fabric under a certain pressure, and the sweat that human body is distributed can be in the form of water vapour
The external world is transmitted to by fabric, the condensation accumulation not between human body surface and fabric keeps wearer dry and comfortable, warm.So,
Foreign countries are referred to as " can breathe fabric ".When this fabric can not only meet people's activity in the adverse circumstances such as severe cold, sleet, strong wind
Dress need, people's daily life demand is also applied for, with vast potential for future development.
Waterproof moisture permeating fabric is mainly realized using the greatest differences of water vapour molecule and hydrone, try on fabric
Certain " hole " is formed, makes the size in aperture between water droplet and water vapour molecule, then fabric can be made only to allow vapor point
Son passes through, and prevents the transmission of water droplet.The preparation approach of waterproof moisture permeating fabric has following three kinds：1) highly dense knitted through what water repellent was handled
Thing；2) laminated fabric；3) coated fabric.Due to high density fabric complex manufacturing, with high costs and waterproofing and moisture-penetration performances less
It is preferable.Another kind of is exactly coated fabric, although it is this kind of can respiratory fabric technique it is simple, with low cost, waterproof and moisture permeability
Can not be good.Existing market mainstream technology is ePTFE (expanded ptfe) microporous barrier of U.S. Gore-Tex (GORE-TEX)
With the laminar composite of fabric, waterproof moisture permeating fabric prepared by the technology has preferable waterproofing and moisture-penetration performances, but by its system
The special biaxial tension equipment of standby needs, complex process, Product processing difficulty is big, cost is high, valuable product, in very great Cheng
Its popularization and application is limited on degree.
The relevant report of waterproof and breathable fiber is also related in the prior art：
Patent CN102632648A proposes at room temperature, polyurethane to be added in solvent, hydrophobic nano is added
Grain, obtains the homogeneous spinning solution of property；Spinning solution is subjected to ultrasonication, the spinning solution after ultrasonication is subjected to electrostatic
Spinning, is obtained with electrostatic spinning nano fiber film on the reception device；Adhesive is transferred to point format by transferring roller
Adhesive point-like glue-line is formed on electrostatic spinning nano fiber film, then fabric is sticked, fiber fabric layer, Ran Houjin is formed
Row hot rolling, is made High-efficiency waterproof moisture-permeable shell fabric, and nanofiber prepared by electrostatic spinning is used for preparing waterproof moisture permeating fabric.
Patent CN201410148615.9 discloses a kind of Waterproof Breathable composite membrane and preparation method thereof, and the Waterproof Breathable is answered
Closing film includes hydrophobic membrane and hydrophilic film, with polyester-type thermoplastic film (TPEE films) to receive substrate, utilizes Static Spinning nanometer technology
Hydrophobic type polymer dope will be drawn into nanoscale/Sub-micro Fibers, and be deposited on non-porous film, formed " hydrophilic film+
Microporous barrier " composite membrane.
Patent CN105568556A discloses nano fibrous membrane that is a kind of super-hydrophobic or super hydrophilic and possessing anti-microbial property
Preparation method, the preparation process of described nano fibrous membrane that is super-hydrophobic or super hydrophilic and possessing anti-microbial property is as follows：Step (1)
Prepare polymer solution；Step (2) electrostatic spinning；Step (3) prepares quaternary ammonium salt solution；Step (4) prepares quaternary ammonium salt and nanometer
The suspension mixed solution of particle；The suspension mixed solution modification porous nano-fibre film of step (5) quaternary ammonium salt and nano particle；Step
(6)：The porous nano-fibre film of the suspension mixed solution modified of quaternary ammonium salt and nano particle made from step (5) is placed in 60
DEG C vacuum drying oven in dry 1-3h, be made nano fibrous membrane finished product that is super-hydrophobic or super hydrophilic and possessing anti-microbial property.This is special
Profit is only with super-hydrophobic or super hydrophilic nano-particle modified nano fibrous membrane, and nano grain surface only exists hydrophilic or thin
The group of water, it is impossible to meet the effect of loomage water proof and moisture permeable.
Nano fibrous membrane prepared by electrostatic spinning is used because fibre diameter is nanoscale, porosity is high, with good
The performance of Waterproof Breathable, but the method that prior art is proposed is generally basede on hydrophobic type polymer, such polymer dope is molten
Agent is organic solvent, and spinning process can form dusty gas, and the nanofiber surface of direct fabrics formation smooth does not have
There is the coarse structure of similar lotus leaf surface, cause this nano fibrous membrane waterproof ability directly prepared not enough.And Nanowire
Dimension film toughness and can rub that performance is bad, the intermolecular forces of fiber can be increased by hot pressing plus glue-line, reinforcing fiber film it is tough
Property, but the structure of original fiber can be also destroyed, reduce the voidage of original tunica fibrosa.Therefore the present invention is deposited for prior art
Waterproofing and moisture-penetration performances are not good, preparation flow is complicated, complex process, intolerant to the method that technique drawback proposes solution such as rubbing.
The content of the invention
Have that waterproofing and moisture-penetration performances are not good, preparation flow is complicated to solve waterproof ventilated membrane in the prior art, complex process,
The problems such as intolerant to rubbing, the present invention provides a kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof.
In order to solve the above technical problems, present invention offer technical scheme is as follows：
On the one hand, the present invention provides a kind of nanofiber waterproof ventilated membrane of ultra-high throughput, by following percentage by weight
Component is made：
The nanometer silicon dioxide particle 1%-10% of bifunctional group modification
Polymer nanofibre film surplus.
Further, the nanofiber waterproof ventilated membrane of the ultra-high throughput, is made up of following components in percentage by weight：
The nanometer silicon dioxide particle 2%-5% of bifunctional group modification
Polymer nanofibre film surplus.
The bifunctional group is scion grafting group and hydrophobic grouping；The scion grafting group includes carboxyl, amino, sulfydryl, aldehyde
Base or epoxy radicals；The hydrophobic grouping includes polyoxypropylene base, long-chain perfluoroalkyl, polysiloxane group or long chain hydrocarbon groups.
Further, in the step 1, the scion grafting group is by silane coupler dihydro -3- [3- (trimethoxy silicon
Base) propyl group] furans -2,5- diketone, 3- (2,3 epoxypropoxy) triethoxysilane, gamma-aminopropyl-triethoxy-silane or
What 3- mercaptopropyltriethoxysilanes were produced；
The hydrophobic grouping is by hexadecyl trimethoxy silane, dodecyltrimethoxysilane, ten trifluoro octyl groups
Trimethoxy silane, VTES or ne-butyltriethoxysilaneand.
Specified otherwise is needed, above-mentioned silane coupler is that the present invention includes the several examples come, as long as can
The silane coupler for producing scion grafting group carboxyl, amino, sulfydryl, aldehyde radical or epoxy radicals etc. can be used in the present invention；Can
The silane coupler for producing the hydrophobic groupings such as polyoxypropylene base, long-chain perfluoroalkyl, polysiloxane group or long chain hydrocarbon groups can
For in the present invention.
Nanometer silicon dioxide particle surface modification two kinds of functional groups, the functional group that scion grafting group can be with fiber surface
Chemically react, particulate matter and the fiber contacted with each other occur after scion grafting simultaneously, can be increased with the active force between reinforcing fiber
The toughness of strong tunica fibrosa；Hydrophobic grouping has strong hydrophobicity, and the coarse structure of class lotus leaf surface is formd in fiber surface, increases
The strong water proofing property of waterproof humidity-permeant film, so ensure former nano fibrous membrane it is fluffy in the state of, both add fiber surface
Roughness, cementation between fiber is added again, the rub resistance of fiber is enhanced.And this method greatly breaks through
The existing material limitation for preparing waterproof humidity-permeant film, is no longer limited by the hydrophobicitys such as polyurethanes (PU), polytetrafluoroethylene (PTFE)
High molecular polymer, some hydrophilic environmental protective polymers may also be used for preparing Waterproof Breathable membrane material.
Further, a diameter of 5nm-100nm of the nanometer silicon dioxide particle of the bifunctional group modification.
Further, the polymer nanofibre film is by polyurethane, organosilicon-propylene vinegar copolymer, polypropylene
Acid esters, organosilicon, polystyrene, polyvinyl acetate, PLA-caprolactone, polyacrylonitrile, PLA-polyethylene glycol oxide, poly- ammonia
Ester-propylene vinegar, polyvinyl alcohol, styrene-propene vinegar copolymer, chitosan, vinyl acetate-propylene vinegar copolymer, vinegar
One or more in sour fiber, polytetrafluoroethylene (PTFE), fibroin fiber, polyamide are made.
Further, the polymer fiber film thickness is 1-50 μm.
On the other hand, the present invention also provides a kind of preparation side of the nanofiber waterproof ventilated membrane of above-mentioned ultra-high throughput
Method, including：
Step 1：Receiving for surface bifunctional group modification is prepared by the method for alternately adding different silane coupler scion graftings
Rice silica dioxide granule；
Step 2：Prepared polymer solution, nano fibrous membrane is prepared by electrostatic spinning process；
Step 3：The chemical scion grafting of nanometer silicon dioxide particle of bifunctional group modification prepared by step 1 is in nanofiber
On.
Further, in the step 3, described nano fibrous membrane before nanometer silicon dioxide particle scion grafting with doing surface
The nanometer silicon dioxide particle that nano fibrous membrane surface functional group can be modified with bifunctional group after modification, processing occurs
Scion grafting is reacted.
Further, in the step 3, the place of the chemical scion grafting of nanometer silicon dioxide particle of the bifunctional group modification
Reason method is one or more kinds of combinations in dip-coating, brushing, spraying, then passes through heating, illumination, radiation, microwave or ultrasound
One or more kinds of combinations in processing promote nano silicon to be fixed on fiber surface.
The invention provides nanofiber waterproof ventilated membrane of a kind of ultra-high throughput and preparation method thereof, with following beneficial
Effect：
1) the tunica fibrosa surface void that causes present invention, avoiding methods such as addition point jelly, hot pressing is destroyed, reduce
Problem, maintains the more loose state of nano fibrous membrane, improves tunica fibrosa permeability；
2) nanometer silicon dioxide particle of bifunctional group modification is prepared for, what long-chain or fluorine-containing hydrophobic grouping were modified receives
Rice grain thing had both added the roughness of fiber surface, and the hydrophobicity of fiber itself is added again, tunica fibrosa is drastically increased
The water proofing property on surface；
3) scion grafting group is that crosslinked group is crosslinked together by the fiber contacted with each other in tunica fibrosa, is secured between fiber
Structure, improve toughness, the rub resistance of tunica fibrosa；
4) present invention is prepared for the nano particle of bifunctional group, can chemical scion grafting on hydrophilic fibre film surface, expand
The raw material range of choice of Waterproof Breathable membrane material has been opened up, pollution of the organic solvent to environment has been reduced, with good environmental protection
Meaning；
5) the waterproof and breathable membrane aperture of ultra-high throughput that prepared by the present invention is small, porosity is high, and has an enhanced adhesion structure,
There is the characteristics of water pressure resistance is high, moisture-inhibiting flux is high, intensity is high, moisture-inhibiting flux >=18000g/m when for Waterproof Breathable field2/
D, water pressure resistance >=100kPa, with extensive actual application prospect.
Brief description of the drawings
Fig. 1 is silica/polyvinyl alcohol nano spinning film of the bifunctional group modification of the embodiment of the present invention 1
SEM photograph.
Embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
Such scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are to be used to illustrate
The present invention and be not limited to limit the scope of the present invention.The implementation condition used in embodiment can be done according to the condition of specific producer
Further adjustment, unreceipted implementation condition is usually the condition in normal experiment.
Material, reagent used etc., are commercially obtained in following embodiments.
The present invention provides a kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof, specific material consumption and
Experimentation is referring to following embodiments.
Embodiment 1：
A kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof, including：
Step 1：The nano silicon toluene dispersion liquid 100g of 0.5% mass concentration is prepared, then the two of preparation 10%
The toluene solution 5g of hydrogen -3- [3- (trimethoxy silicon substrate) propyl group] furans -2,5- diketone, 10% hexadecyl trimethoxy silicon
The toluene solution 5g of alkane, is alternately added in nano silicon toluene dispersion liquid, after the completion of addition, stands overnight several times,
0.5g water is added, dihydro -3- [3- (trimethoxy silicon substrate) propyl group] furans -2,5- diketone, which is hydrolyzed to form, forms double after two carboxyls
The nano silicon toluene dispersion liquid of functional group modification；
Step 2：The spinning solution of polyvinyl alcohol is prepared, solvent is water, and mass concentration is 12%, carry out electrostatic spinning, spun
Flight lead is made after polyvinyl alcohol nanofiber membrane from 15cm, spinning voltage 35kv, passes through 1% gamma-aminopropyl-triethoxy silicon
After the processing of alkane ethanol solution, amino modified polyvinyl alcohol nanofiber membrane is obtained after drying；
Step 3：Amino modified polyvinyl alcohol nanofiber membrane is immersed in bifunctional group modification prepared by step 1
In nano silicon toluene dispersion liquid, add EDC (1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides) and
NHS (n-hydroxysuccinimide), reacts at room temperature 12h, and tunica fibrosa is taken out to the nanofiber waterproof for being dried to obtain ultra-high throughput
Ventilated membrane.
Dioxide-containing silica is 10% in the waterproof ventilated membrane of the ultra-high throughput of acquisition, and the water pressure resistance of waterproof ventilated membrane is
145kPa, moisture-inhibiting flux is 20000g/m2/ d, rubbing test instrument is rubbed after 2000 times, vapor transfer rate reduction by 0.3%.
Embodiment 2：
A kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof, including：
Step 1：Prepare the nano silicon alcohol dispersion liquid 100g of 0.5% mass concentration, then prepare 10% γ-
Ethanol solution 5g, the ethanol solution 5g of 10% ten trifluoro octyl group trimethoxy silanes of aminopropyl triethoxysilane, divide many
Secondary alternating is added in nano silicon alcohol dispersion liquid, the rear nano silicon ethanol point for forming bifunctional group modification
Dispersion liquid；
Step 2：The spinning solution of deacetylated 90% chitosan is prepared, solvent is glacial acetic acid, and mass concentration is 9%,
Electrostatic spinning is carried out, spinning obtains porous chitosan nano fibrous membrane apart from 18cm, spinning voltage 70kv；
Step 3：The nano silicon alcohol dispersion liquid of bifunctional group modification prepared by step 1 is sprayed on chitosan
Nano fibrous membrane surface, after drying, makes chitosan surface amino groups and silicon dioxide meter in the steam that tunica fibrosa is put into glutaraldehyde
Face amino crosslinks reaction, obtains the nanofiber waterproof ventilated membrane of ultra-high throughput.
Dioxide-containing silica is 1% in the waterproof ventilated membrane of the ultra-high throughput of acquisition, and waterproof ventilated membrane water pressure resistance is
121kPa, moisture-inhibiting flux is 18000g/m2/ d, rubbing test instrument is rubbed after 2000 times, vapor transfer rate reduction by 1%.
Embodiment 3:
A kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof, including：
Step 1：Prepare the nano silicon alcohol dispersion liquid 100g of 0.5% mass concentration, then prepare 10% γ-
The ethanol solution 5g of aminopropyl triethoxysilane, the ethanol solution 5g of 10% VTES, are handed over several times
For being added in nano silicon alcohol dispersion liquid, the rear nano silicon ethanol for forming bifunctional group modification disperses
Liquid；
Step 2：The spinning solution of polyacrylonitrile is prepared, solvent is DMF, and mass concentration is 12%, is entered
Polyacrylonitrile nanofiber film is made apart from 16cm, spinning voltage 60kv in row electrostatic spinning, spinning, after pass through 10% hydroxide
Sodium solution is handled, and 15% HCl treatment is added after cleaning, and carboxy-modified gathering with insertion pore structure is obtained after drying
Acrylonitrile nano fibrous membrane；
Step 3：Carboxy-modified polyacrylonitrile nanofiber film is immersed in the nanometer titanium dioxide of bifunctional group modification
In silicon alcohol dispersion liquid, 35 DEG C of reaction 24h take out tunica fibrosa the nanofiber that ultra-high throughput is obtained after Infrared irradiation is dried
Waterproof ventilated membrane.
Dioxide-containing silica is 6.8% in the waterproof ventilated membrane of the ultra-high throughput of acquisition, and waterproof ventilated membrane water pressure resistance is
136kPa, moisture-inhibiting flux is 19500g/m2/ d, rubbing test instrument is rubbed after 2000 times, vapor transfer rate reduction by 0.5%.
Embodiment 4:
A kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof, including：
Step 1：The nano silicon alcohol dispersion liquid 100g of 0.5% mass concentration is prepared, 10% 3- is then prepared
The ethanol solution 5g of mercaptopropyltriethoxysilane, the ethanol solution 5g of 10% ne-butyltriethoxysilaneand, are handed over several times
For being added in nano silicon alcohol dispersion liquid, the rear nano silicon ethanol for forming bifunctional group modification disperses
Liquid；
Step 2：The spinning solution of polyurethane-acrylate vinegar is prepared, solvent is acetone, and mass concentration is 12%, carried out quiet
Electrospun, spinning is handled apart from 16cm, spinning voltage 60kv by 1% gamma-aminopropyl-triethoxy-silane ethanol solution
Afterwards, amino modified polyurethane-acrylate vinegar nano fibrous membrane is obtained after drying；
Step 3：Amino modified polyurethane-acrylate vinegar nano fibrous membrane is immersed in the nanometer of bifunctional group modification
In silica alcohol dispersion liquid, 35 DEG C of reaction 24h, the nanofiber waterproof that tunica fibrosa taking-up is dried to obtain into ultra-high throughput is saturating
Air film.
Dioxide-containing silica is 5% in the waterproof ventilated membrane of the ultra-high throughput of acquisition, and waterproof ventilated membrane water pressure resistance is
131kPa, moisture-inhibiting flux is 19070g/m2/ d, rubbing test instrument is rubbed after 2000 times, vapor transfer rate reduction by 0.4%.
Embodiment 5:
A kind of nanofiber waterproof ventilated membrane of ultra-high throughput and preparation method thereof, including：
Step 1：Prepare the nano silicon alcohol dispersion liquid 100g of 0.5% mass concentration, then prepare 10% γ-
The ethanol solution 5g of aminopropyl triethoxysilane, the ethanol solution 5g of 10% dodecyltrimethoxysilane, several times
Alternating is added in nano silicon alcohol dispersion liquid, and the rear nano silicon ethanol for forming bifunctional group modification disperses
Liquid；
Step 2：The spinning solution of styrene-propene vinegar copolymer is prepared, solvent is acetone, and mass concentration is 12%,
Electrostatic spinning is carried out, styrene-propene vinegar copolymer nanofiber film is made apart from 16cm, spinning voltage 60kv in spinning, after
After 1% gamma-aminopropyl-triethoxy-silane ethanol solution processing, amino modified polyvinyl alcohol nano is obtained after drying
Tunica fibrosa；
Step 3：Carboxy-modified polyurethane-acrylate vinegar nano fibrous membrane is immersed in the nanometer of bifunctional group modification
In silica alcohol dispersion liquid, 35 DEG C of reaction 24h, the nanofiber that tunica fibrosa taking-up heat drying is obtained into ultra-high throughput is prevented
Water ventilated membrane.
Dioxide-containing silica is 2% in the waterproof ventilated membrane of the ultra-high throughput of acquisition, and waterproof ventilated membrane water pressure resistance is
128kPa, moisture-inhibiting flux is 18750g/m2/ d, rubbing test instrument is rubbed after 2000 times, vapor transfer rate reduction by 0.7%.
For the performance for the nanofiber waterproof ventilated membrane for further illustrating ultra-high throughput prepared by the present invention, the present invention is with reality
Structure comparative example is as follows exemplified by applying example 3.
Comparative example 1：
A kind of nano fibrous membrane and preparation method thereof, including：
Step 1：Prepare the nano silicon alcohol dispersion liquid 100g of 0.5% mass concentration, then prepare 10% γ-
Aminopropyl triethoxysilane ethanol solution 5g, 10% VTES ethanol solution 5g, three is well mixed,
Form modified silica dioxide granule；
Step 2：The DMF solution that mass concentration is 12% polyacrylonitrile, stirring are added into step 1
Spinning solution is formed uniformly, modified polyacrylonitrile nano fibrous membrane is made apart from 16cm, spinning voltage 60kv in spinning.
The water pressure resistance of the modified polyacrylonitrile nano fibrous membrane of acquisition is 92kPa, and moisture-inhibiting flux is 8700g/m2/ d, is rubbed
Test instrument is rubbed after 2000 times, vapor transfer rate reduction by 28%.
Comparative example 2：
A kind of nano fibrous membrane and preparation method thereof, including：
Step 1：Prepare the nano silicon alcohol dispersion liquid 100g of 0.5% mass concentration, then prepare 10% γ-
Aminopropyl triethoxysilane ethanol solution 5g, 10% VTES ethanol solution 5g, alternately add several times
It is added in nano silicon alcohol dispersion liquid, the rear nano silicon alcohol dispersion liquid for forming bifunctional group modification；
Step 2：The DMF solution that mass concentration is 12% polyacrylonitrile, stirring are added into step 1
Spinning solution is formed uniformly, modified polyacrylonitrile nano fibrous membrane is made apart from 16cm, spinning voltage 60kv in spinning.
The water pressure resistance of the modified polyacrylonitrile nano fibrous membrane of acquisition is 95kPa, and moisture-inhibiting flux is 9700g/m2/ d, is rubbed
Test instrument is rubbed after 2000 times, vapor transfer rate reduction by 13%.
By above-described embodiment 1-5 and comparative example 1-2, the present invention is by alternately adding different silane coupler scion graftings
Method prepare the nanometer silicon dioxide particle of surface bifunctional group modification, and disposable to add whole silane couplers (right
Ratio 1) compare, its water pressure resistance, moisture-inhibiting flux and rub performance and greatly improve, this is probably due to even by alternately addition silane
Join the mode of agent so that the first silane coupler is another silane coupled when silica surface modification is not up to saturation
Agent can continue to modify silica in its space, after multiplicating, it is ensured that different bases are completely covered in silica surface
Group, is easy to the follow-up reaction adjacent fiber between, secures the structure between fiber, improve the toughness of tunica fibrosa, resistance to rub
Stranding with the hands property；The roughness of the both fiber surface of more hydrophobic grouping increase simultaneously, adds the hydrophobicity of fiber itself, greatly again
Improve the water proofing property on tunica fibrosa surface.
By the way that compared with comparative example 2, the silica dioxide granule that the bifunctional group of preparation is modified passes through dip-coating, brush
The form for applying or spraying, is modified on tunica fibrosa surface, the properties of the nanofiber waterproof ventilated membrane of obtained ultra-high throughput
It is excellent.This is probably due on the one hand the silica dioxide granule be modified not being added in polymer solution, it is to avoid polymerize
Influence of the solvent to silica dioxide granule in thing solution；On the other hand it is that the present invention is follow-up to be not required to carry out electrostatic spinning process, no
The problem of having that the tunica fibrosa surface void that the methods such as hot pressing cause is destroyed, reduce, maintains more dredging for nano fibrous membrane
The state of pine, improves tunica fibrosa permeability.
The experiment lifted only is the preferably example of the present invention, the protection domain being not intended to limit the present invention.It should refer to
Go out, for those skilled in the art, on the premise of principle of the present invention is not departed from, can also make
Some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. the nanofiber waterproof ventilated membrane of a kind of ultra-high throughput, it is characterised in that be made up of following components in percentage by weight：
The nanometer silicon dioxide particle 1%-10% of bifunctional group modification
Polymer nanofibre film surplus；
The nanometer silicon dioxide particle of the bifunctional group modification is modified by scion grafting group and hydrophobic grouping to be formed；The scion grafting
Group includes carboxyl, amino, sulfydryl, aldehyde radical or epoxy radicals；The hydrophobic grouping include polyoxypropylene base, long-chain perfluoroalkyl,
Polysiloxane group or long chain hydrocarbon groups.
2. the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 1, it is characterised in that by following weight hundred
The component of ratio is divided to be made：
The nanometer silicon dioxide particle 2%-5% of bifunctional group modification
Polymer nanofibre film surplus.
3. the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 1 or 2, it is characterised in that the scion grafting
Group is by silane coupler dihydro -3- [3- (trimethoxy silicon substrate) propyl group] furans -2,5- diketone, 3- (2,3 the third oxygen of epoxy third
Base) triethoxysilane, gamma-aminopropyl-triethoxy-silane or the generation of 3- mercaptopropyltriethoxysilanes.
4. the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 1 or 2, it is characterised in that described hydrophobic
Group is by hexadecyl trimethoxy silane, dodecyltrimethoxysilane, ten trifluoro octyl group trimethoxy silanes, vinyl
Triethoxysilane or ne-butyltriethoxysilaneand are produced.
5. the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 1 or 2, it is characterised in that described pair of work(
A diameter of 5nm-100nm of the nanometer silicon dioxide particle of energy base group modification.
6. the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 1 or 2, it is characterised in that the polymerization
Thing nano fibrous membrane is by polyurethane, organosilicon-propylene vinegar copolymer, polyacrylate, organosilicon, polystyrene, poly-vinegar
Sour ethene, PLA-caprolactone, polyacrylonitrile, PLA-polyethylene glycol oxide, polyurethane-acrylate vinegar, polyvinyl alcohol, benzene second
Alkene-propylene vinegar copolymer, chitosan, vinyl acetate-propylene vinegar copolymer, acetate fiber, polytetrafluoroethylene (PTFE), fibroin
One or more in fiber, polyamide are made.
7. the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 1 or 2, it is characterised in that the polymerization
Fibres film thickness is 1-50 μm.
8. the preparation method of the nanofiber waterproof ventilated membrane of any described ultra-high throughput of claim 1 to 7, its feature exists
In, including：
Step 1：The method that the silane coupler scion grafting of scion grafting group and hydrophobic grouping can be produced by alternately addition prepares surface
The nanometer silicon dioxide particle of bifunctional group modification；
Step 2：Prepared polymer solution, prepares nanofiber by electrostatic spinning process, then prepares nano fibrous membrane；
Step 3：The chemical scion grafting of nanometer silicon dioxide particle of bifunctional group modification prepared by step 1 is on nanofiber.
9. the preparation method of the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 8, it is characterised in that institute
State in step 3, described nano fibrous membrane does surface before the nanometer silicon dioxide particle scion grafting modified with bifunctional group and changed
Property processing, after processing nano fibrous membrane surface functional group can with bifunctional group modify nanometer silicon dioxide particle occur branch
It is reversed to answer.
10. the preparation method of the nanofiber waterproof ventilated membrane of ultra-high throughput according to claim 8, it is characterised in that
In the step 3, the treating method of the chemical scion grafting of nanometer silicon dioxide particle of the bifunctional group modification is dip-coating, brushed
Apply, one or more kinds of combinations in spraying, then by heating, illumination, radiation, microwave or it is ultrasonically treated in one kind or
Multiple combinations promote nano silicon to be fixed on fiber surface.
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