CN110258021A - A kind of high waterproof height is breathed freely nano fibrous membrane and preparation method thereof - Google Patents
A kind of high waterproof height is breathed freely nano fibrous membrane and preparation method thereof Download PDFInfo
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- CN110258021A CN110258021A CN201910597733.0A CN201910597733A CN110258021A CN 110258021 A CN110258021 A CN 110258021A CN 201910597733 A CN201910597733 A CN 201910597733A CN 110258021 A CN110258021 A CN 110258021A
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- electrospinning film
- pvb
- spinning
- fpu
- pvdf
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- 239000012528 membrane Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000001523 electrospinning Methods 0.000 claims abstract description 195
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 92
- 239000002033 PVDF binder Substances 0.000 claims abstract description 71
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 71
- 239000004814 polyurethane Substances 0.000 claims abstract description 44
- 239000000835 fiber Substances 0.000 claims abstract description 20
- 239000002121 nanofiber Substances 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 229920002635 polyurethane Polymers 0.000 claims abstract description 9
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000009987 spinning Methods 0.000 claims description 92
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 20
- 238000010041 electrostatic spinning Methods 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000003760 magnetic stirring Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005030 aluminium foil Substances 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims 1
- 150000002085 enols Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 4
- 239000004744 fabric Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 7
- 230000035699 permeability Effects 0.000 description 7
- 230000002706 hydrostatic effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000006798 recombination Effects 0.000 description 6
- 238000005215 recombination Methods 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- 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
- D04H1/4282—Addition polymers
- D04H1/4318—Fluorine series
-
- 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
- D04H1/4326—Condensation or reaction polymers
-
- 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
- D04H1/4326—Condensation or reaction polymers
- D04H1/4358—Polyurethanes
-
- 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
- D04H1/4374—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 using different kinds of webs, e.g. by layering webs
-
- 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
-
- 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
-
- 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
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/38—Polyurethanes
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/35—Abrasion, pilling or fibrillation resistance
Abstract
The invention discloses ventilative nano fibrous membrane of a kind of high waterproof height and preparation method thereof, the ventilative nano fibrous membrane of the high waterproof height includes PVB electrospinning film, PVDF electrospinning film and FPU electrospinning film；PVB electrospinning film, PVDF electrospinning film and FPU electrospinning film are laminated compound from inside to outside；PVB electrospinning film is to be interwoven by polyvinyl butyral nanofiber；The average diameter of polyvinyl butyral nanofiber is 150-400nm；PVDF electrospinning film is to be formed by polyvinylidene fluoride nanometer fiber interweaving；The average diameter of polyvinylidene fluoride nanometer fiber is 400-600nm；FPU electrospinning film is to be interwoven through the modified polyurethane nanofiber of silicon fluoride；The diameter of polyurethane nanofiber is 200-300nm.Present invention process advantages of simple, manufacturing cost is low, and the high waterproof height of preparation is breathed freely, and nanofiber film-strength is high, and waterproof performance is good, and one-way ventilating performance is good.
Description
Technical field
The present invention relates to nano fibrous membrane field more particularly to a kind of ventilative nano fibrous membrane of high waterproof height and its preparation sides
Method.
Background technique
Proofed breathable fabric refers in use, and water cannot be impregnated with fabric under a certain pressure, and the liquid distributed
Especially vapor can pass through fabric.Fabric with waterproof and breathable function is widely used in daily life, such as
Tent, sleeping bag, water-proof jacket, shoes, down jackets etc., and be increasingly taken seriously in some special dimensions, such as militarily use
In the production of military uniform, protective garment, and protective materials as precision instrument etc..With the function phase of common fabric keep warm
Than waterproof ventilative material should have the various functions such as waterproof, moisture-inhibiting, ventilative, insulation, radix saposhnikoviae, warming, and some of them function
Realization be it is conflicting, should waterproof, again moisture-inhibiting, ventilative mutually restrict.
Currently, existing proofed breathable fabric mainly has in the market: high density fabric, coated fabric and laminated fabric.But it is high
Though close fabric water vapour permeability is good, resistance to hydrostatic pressure is poor；Coated fabric waterproof performance is excellent, but there is that flexibility is poor, gas permeability
The defect of energy difference；Though laminated fabric waterproof and breathable performance relative good, preparation process is complicated, at high cost, is lacked due to respective
It falls into and limits its scope of application.Electrostatic spinning nano fiber film is a kind of novel waterproof ventilative material.Electrostatic spinning principle master
If first applying the high-pressure electrostatic of thousands of volts to polymer drop or melt, subsequent charged drop shape under electric field force effect
Become and form Tayer cone in spinning nozzle, the lasting increase of electric field force is so that drop finally can overcome its surface tension from cone
Jet stream is sprayed, jet stream is further stretched during the motion, refines, while solvent volatilizees so that jet stream solidification, forms nanometer
The superfine fibre of grade is fallen on the receiver in the form of rambling non-woven cloth, forms nano fibrous membrane.Static Spinning is suitble to
It for the research of waterproof and breathable performance, but is still in infancy, compared with traditional waterproof and breathable textile, still has one
It is a little insufficient, therefore the novel nano tunica fibrosa that a kind of high waterproof height of demand is ventilative.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of ventilative nano fibrous membrane of high waterproof height and its preparation sides
Method carries out coordinated by three layers of different nano fibrous membrane, on the basis for improving intensity aiming at the shortcomings in the prior art
On, optimize its waterproof performance and promote one-way wet-guide permeability, solves existing nano fibrous membrane intensity difference, waterproof and breathable
The undesirable problem of performance.
In order to achieve the above objectives, technical scheme is as follows: a kind of ventilative nano fibrous membrane of high waterproof height, including
PVB electrospinning film, PVDF electrospinning film and FPU electrospinning film；The PVB electrospinning film, PVDF electrospinning film and FPU electrospinning film layer from inside to outside
It folds compound；The PVB electrospinning film is to be interwoven by polyvinyl butyral nanofiber；The polyvinyl butyral nanometer
The average diameter of fiber is 150-400nm；The PVDF electrospinning film is to be formed by polyvinylidene fluoride nanometer fiber interweaving；It is described poly-
The average diameter of vinylidene nanofiber is 400-600nm；The FPU electrospinning film is the polyurethane nano modified through silicon fluoride
Fiber interweaving forms；The diameter of the polyurethane nanofiber is 200-300nm.
As a preferred solution of the present invention, the PVB electrospinning film with a thickness of 0.010-0.025mm.
As a preferred solution of the present invention, the thickness ratio of the PVB electrospinning film and FPU electrospinning film is 1:(1.2-
1.6)。
As a preferred solution of the present invention, silica nanometer coating, energy are coated in the FPU electrospinning film surface
Enough wear-resisting properties for further improving FPU electrospinning film surface, improve the hydrophobic performance of FPU electrospinning film.
The preparation method of the ventilative nano fibrous membrane of above-mentioned high waterproof height, comprising the following steps:
Step 1, PVB electrospinning film is prepared；The PVB powder end for weighing certain mass, is added dehydrated alcohol, is configured to mass fraction
It for the PVB spinning solution of 6-8%, is sufficiently stirred by magnetic stirring apparatus, makes the sufficiently dissolution of PVB powder end；Then pass through electrostatic
Device for spinning carries out spinning and prepares PVB electrospinning film, and PVB spinning solution is injected in needle tubing and carries out electrostatic spinning, using aluminium foil as substrate,
Spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 12-25kV, and receiving distance is 13-16cm, spinning
Speed is 0.5-1mL/h, and the thickness control of PVB electrospinning film is in 0.010-0.025mm；
Step 2, in the compound PVDF electrospinning film of PVB electrospinning film surface；Weigh a certain amount of PVDF powder, be dissolved into DMF and
The in the mixed solvent that the volume ratio of acetone is 6/4 is heated in 40 DEG C of water-baths and is sufficiently stirred by magnetic stirring apparatus, made
PVDF powder sufficiently dissolves, and prepares the PVDF spinning solution that mass fraction is 13-16%；By electrostatic spinning apparatus to PVB electrospinning
Film surface carries out continuation spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, and spinning voltage 15-18kV connects
Receiving distance is 15-20cm, and the thickness of spinning speed 0.5-1mL/h, PVDF electrospinning film is maintained at 0.010-0.040 μm；
Step 3, in the compound FPU electrospinning film of PVDF electrospinning film surface；It weighs a certain amount of PU particle and is added to and be dissolved with
It in the DMF solvent of NaCl, is sufficiently stirred by magnetic stirring apparatus, dissolves PU particle sufficiently, preparing mass fraction is 15-
18% PU spinning solution, in PU spinning solution, the mass fraction of NaCl is 0.01%；Continued by electrostatic spinning apparatus to PVDF
Electrospinning film surface carries out spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, and spinning voltage 13-16kV connects
Receiving distance is 15-20cm, spinning speed 0.5-1mL/h, prepares PU electrospinning film；Using plasma instrument to PU electrospinning film table
Face is activated, and under helium environment, is activated power control in 100W, pressure control handles time 1-3min in 20Pa；
Then the methanol solution for being 1wt% in PU electrospinning film surface coating FAS concentration, every 30min coating is primary, coats 20-30 altogether
It is secondary, then vacuum drying is carried out, drying temperature is 60-75 DEG C, drying time 16-20h, forms FPU in PVDF electrospinning film surface
Composite cellulosic membrane is made in electrospinning film；
Step 4, composite cellulosic membrane is heat-treated；By 130-140 DEG C of hot wind to the two sides of composite cellulosic membrane into
Row heat treatment, heating time 5-15min.
As the optimization to above-mentioned preparation method, above-mentioned preparation method further includes step 5, and FPU electrospinning film surface is preheated
To 40 DEG C, the acetone soln that nano SiO 2 particle concentration is 0.1-0.2wt% is uniformly scratched to FPU electrospinning film surface,
110 DEG C at a temperature of, vacuum drying 10 minutes, repeatedly blade coating drying 3 times.
Wherein, PVB electrospinning film is polyvinyl butyral electrospinning film, and PVDF electrospinning film is Kynoar electrospinning film, FPU
Electrospinning film is fluorochemical urethane electrospinning film.
Through the above technical solutions, the beneficial effect of technical solution of the present invention is: simple production process of the present invention is reasonable, system
It makes at low cost, can be suitable for industrialized mass production, the high waterproof height of preparation nanofiber film properties of breathing freely are stablized, yield rate
Height improves nano fibrous membrane in the applied defect in waterproof and breathable field, is conducive to promote and apply.High waterproof height of the invention is ventilative
Nano fibrous membrane improves the problem of existing single layer nano fibrous membrane intensity difference, and PVDF electrospinning film and FPU electrospinning film are compound, energy
Tearing toughness is enough effectively improved, and PVB electrospinning film can be improved the flexibility of FPU electrospinning film, by sandwich composite construction,
Breaking strength is in 5MPa or more, and elongation is in 35-45%；Face where FPU electrospinning film of the present invention has good waterproof performance, resistance to
Hydrostatic pressing value reaches 100KPa, and face has good permeability, penetrability 10.1kgm where PVB electrospinning film-2d-1.The present invention
FPU electrospinning film where face be waterproof surface, FPU electrospinning membrane fiber structure is uniform, fine and closely woven, and the porous of uniform pore diameter is formed after intertexture
The average pore size of structure, FPU electrospinning film is small, while FPU electrospinning film hydrophobic performance is good, carries out hydrophobically modified, shape by silicon fluoride
At lotus leaf effect, FPU electrospinning film is made to have high-strength waterproof performance；And face where PVB electrospinning film is ventilative face, the present invention is logical
" adsorption -diffusion " effect and " capillary-diffusion " effect are crossed, ensure that good permeability, since PVB electrospinning film is with hydrophilic
Property, and PVDF electrospinning film and FPU electrospinning film hydrophobicity are good, aqueous vapor is adsorbed by PVB electrospinning film, is then spread from the high side of humidity
One-way wet-guide is realized in the side low to humidity；It is greater than FPU with interfibrous average pore size between the fiber of PVDF electrospinning film simultaneously
Electrospinning film, aqueous vapor are moved to side where FPU electrospinning film due to pressure difference, are then diffused on the outside of FPU electrospinning film, and realization is unidirectionally led
It is penetrable ventilated.In addition, PVB electrospinning film flexibility is good, sense of touch is comfortable, is suitable for dress.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the structural diagram of the present invention.
Number and corresponding component title represented by letter in figure:
1.PVB electrospinning film 2.PVDF electrospinning film 3.FPU electrospinning film.
Specific embodiment
Below in conjunction with the attached drawing of the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of ventilative nano fibrous membrane of high waterproof height, using three layers of compound sandwich structure, including from inside to outside successively
Compound PVB electrospinning film 1, PVDF electrospinning film 2 and FPU electrospinning film 3 is laminated.PVB electrospinning film 1 is by polyvinyl butyral nanometer
Fiber interweaving forms.PVDF electrospinning film 2 is to be formed by polyvinylidene fluoride nanometer fiber interweaving.FPU electrospinning film 3 is to change through silicon fluoride
The polyurethane nanofiber of property is interwoven.
The preparation method of the ventilative nano fibrous membrane of the high waterproof height, comprising the following steps:
Step 1, PVB electrospinning film 1 is prepared；The PVB powder end for weighing certain mass, is added dehydrated alcohol, is configured to quality point
Number is the PVB spinning solution of 6-8%, is sufficiently stirred by magnetic stirring apparatus, and the sufficiently dissolution of PVB powder end is made；Then by quiet
Electric spinning device carries out spinning and prepares PVB electrospinning film 1, and PVB spinning solution is injected in needle tubing and carries out electrostatic spinning, using aluminium foil as base
Material, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 12kV, and receiving distance is 13cm, spinning speed
Degree is 0.5mL/h, and the thickness control of PVB electrospinning film 1 is in 0.010mm.
Step 2, in 1 surface recombination PVDF electrospinning film 2 of PVB electrospinning film；A certain amount of PVDF powder is weighed, DMF is dissolved into
The in the mixed solvent that volume ratio with acetone is 6/4, heats in 40 DEG C of water-baths and is sufficiently stirred by magnetic stirring apparatus,
It dissolves PVDF powder sufficiently, prepares the PVDF spinning solution that mass fraction is 13-16%；By electrostatic spinning apparatus to PVB electricity
It spins 1 surface of film and carries out continuation spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, and spinning voltage 15kV connects
Receiving distance is 15cm, and the thickness of spinning speed 0.5mL/h, PVDF electrospinning film 2 is maintained at 0.010 μm.
Step 3, in 2 surface recombination FPU electrospinning film 3 of PVDF electrospinning film；It weighs a certain amount of PU particle and is added to and be dissolved with
It in the DMF solvent of NaCl, is sufficiently stirred by magnetic stirring apparatus, dissolves PU particle sufficiently, preparing mass fraction is 15-
18% PU spinning solution, in PU spinning solution, the mass fraction of NaCl is 0.01%；Continued by electrostatic spinning apparatus to PVDF
2 surface of electrospinning film carries out spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 13kV, is received
Distance is 15cm, spinning speed 0.5mL/h, prepares PU electrospinning film；PU electrospinning film surface is carried out using plasma instrument
Activation is activated power control in 100W, pressure control handles time 1-3min in 20Pa under helium environment；Then exist
PU electrospinning film surface coats the methanol solution that FAS concentration is 1wt%, and every 30min coating is primary, coats 20-30 times altogether, then into
Row vacuum drying, drying temperature are 60-75 DEG C, drying time 16-20h, form FPU electrospinning film on 2 surface of PVDF electrospinning film
3, composite cellulosic membrane is made.
Step 4, composite cellulosic membrane is heat-treated；By 130-140 DEG C of hot wind to the two sides of composite cellulosic membrane into
Row heat treatment, heating time 5-15min.
High waterproof height obtained breathes freely nano fibrous membrane breaking strength in 5.58MPa or more, and elongation is 42.66%；This
It invents 3 place face resistance to hydrostatic pressure value of FPU electrospinning film and reaches 108KPa, 1 place face penetrability of PVB electrospinning film is 11.6kgm-2d-1。
Embodiment 2
A kind of ventilative nano fibrous membrane of high waterproof height, using three layers of compound sandwich structure, including from inside to outside successively
Compound PVB electrospinning film 1, PVDF electrospinning film 2 and FPU electrospinning film 3 is laminated.PVB electrospinning film 1 is by polyvinyl butyral nanometer
Fiber interweaving forms.PVDF electrospinning film 2 is to be formed by polyvinylidene fluoride nanometer fiber interweaving.FPU electrospinning film 3 is to change through silicon fluoride
The polyurethane nanofiber of property is interwoven.
The preparation method of the ventilative nano fibrous membrane of the high waterproof height, comprising the following steps:
Step 1, PVB electrospinning film 1 is prepared；The PVB powder end for weighing certain mass, is added dehydrated alcohol, is configured to quality point
Number is the PVB spinning solution of 6-8%, is sufficiently stirred by magnetic stirring apparatus, and the sufficiently dissolution of PVB powder end is made；Then by quiet
Electric spinning device carries out spinning and prepares PVB electrospinning film 1, and PVB spinning solution is injected in needle tubing and carries out electrostatic spinning, using aluminium foil as base
Material, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 25kV, and receiving distance is 16cm, spinning speed
Degree is 1mL/h, and the thickness control of PVB electrospinning film 1 is in 0.025mm.
Step 2, in 1 surface recombination PVDF electrospinning film 2 of PVB electrospinning film；A certain amount of PVDF powder is weighed, DMF is dissolved into
The in the mixed solvent that volume ratio with acetone is 6/4, heats in 40 DEG C of water-baths and is sufficiently stirred by magnetic stirring apparatus,
It dissolves PVDF powder sufficiently, prepares the PVDF spinning solution that mass fraction is 13-16%；By electrostatic spinning apparatus to PVB electricity
It spins 1 surface of film and carries out continuation spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, and spinning voltage 18kV connects
Receiving distance is 25cm, and the thickness of spinning speed 1mL/h, PVDF electrospinning film 2 is maintained at 0.040 μm.
Step 3, in 2 surface recombination FPU electrospinning film 3 of PVDF electrospinning film；It weighs a certain amount of PU particle and is added to and be dissolved with
It in the DMF solvent of NaCl, is sufficiently stirred by magnetic stirring apparatus, dissolves PU particle sufficiently, preparing mass fraction is 15-
18% PU spinning solution, in PU spinning solution, the mass fraction of NaCl is 0.01%；Continued by electrostatic spinning apparatus to PVDF
2 surface of electrospinning film carries out spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 16kV, is received
Distance is 20cm, spinning speed 1mL/h, prepares PU electrospinning film；It is lived using plasma instrument to PU electrospinning film surface
Change, under helium environment, is activated power control in 100W, pressure control handles time 1-3min in 20Pa；Then in PU
Electrospinning film surface coats the methanol solution that FAS concentration is 1wt%, and every 30min coating is primary, coats 20-30 times altogether, then carry out
Vacuum drying, drying temperature are 60-75 DEG C, drying time 16-20h, form FPU electrospinning film 3 on 2 surface of PVDF electrospinning film,
Composite cellulosic membrane is made.
Step 4, composite cellulosic membrane is heat-treated；By 130-140 DEG C of hot wind to the two sides of composite cellulosic membrane into
Row heat treatment, heating time 5-15min.
High waterproof height obtained breathes freely nano fibrous membrane breaking strength as 8.96MPa or more, and elongation is 40.35%；This
It invents 3 place face resistance to hydrostatic pressure value of FPU electrospinning film and reaches 126KPa, 1 place face penetrability of PVB electrospinning film is 10.2kgm-2d-1。
Embodiment 3
A kind of ventilative nano fibrous membrane of high waterproof height, using three layers of compound sandwich structure, including from inside to outside successively
Compound PVB electrospinning film 1, PVDF electrospinning film 2 and FPU electrospinning film 3 is laminated.PVB electrospinning film 1 is by polyvinyl butyral nanometer
Fiber interweaving forms.PVDF electrospinning film 2 is to be formed by polyvinylidene fluoride nanometer fiber interweaving.FPU electrospinning film 3 is to change through silicon fluoride
The polyurethane nanofiber of property is interwoven.In order to make the better coordinated of three, PVB electrospinning film 1 with a thickness of 0.010-
0.025mm.The thickness ratio of PVB electrospinning film 1 and FPU electrospinning film 3 is 1:(1.2-1.6).Improve 3 table of FPU electrospinning film to improve
The wear-resisting property in face improves the hydrophobic performance of FPU electrospinning film 3, is coated with silica nanometer coating on 3 surface of FPU electrospinning film.
The preparation method of the ventilative nano fibrous membrane of the high waterproof height, comprising the following steps:
Step 1, PVB electrospinning film 1 is prepared；The PVB powder end for weighing certain mass, is added dehydrated alcohol, is configured to quality point
The PVB spinning solution that number is 7%, is sufficiently stirred by magnetic stirring apparatus, makes the sufficiently dissolution of PVB powder end；Then pass through electrostatic
Device for spinning carries out spinning and prepares PVB electrospinning film 1, and PVB spinning solution is injected in needle tubing and carries out electrostatic spinning, using aluminium foil as base
Material, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 15kV, and receiving distance is 15cm, spinning speed
Degree is 0.6mL/h, and the thickness control of PVB electrospinning film 1 is in 0.015mm.
Step 2, in 1 surface recombination PVDF electrospinning film 2 of PVB electrospinning film；A certain amount of PVDF powder is weighed, DMF is dissolved into
The in the mixed solvent that volume ratio with acetone is 6/4, heats in 40 DEG C of water-baths and is sufficiently stirred by magnetic stirring apparatus,
It dissolves PVDF powder sufficiently, prepares the PVDF spinning solution that mass fraction is 15%；By electrostatic spinning apparatus to PVB electrospinning film
1 surface carries out continuation spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity be 40 ± 5%, spinning voltage 17kV, receive away from
0.010-0.040 μm is maintained at from the thickness for 16cm, spinning speed 0.8mL/h, PVDF electrospinning film 2.
Step 3, in 2 surface recombination FPU electrospinning film 3 of PVDF electrospinning film；It weighs a certain amount of PU particle and is added to and be dissolved with
It in the DMF solvent of NaCl, is sufficiently stirred by magnetic stirring apparatus, dissolves PU particle sufficiently, preparing mass fraction is
16% PU spinning solution, in PU spinning solution, the mass fraction of NaCl is 0.01%；Continued by electrostatic spinning apparatus to PVDF
2 surface of electrospinning film carries out spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 17kV, is received
Distance is 16cm, spinning speed 0.8mL/h, prepares PU electrospinning film；PU electrospinning film surface is carried out using plasma instrument
Activation is activated power control in 100W, pressure control handles time 1-3min in 20Pa under helium environment；Then exist
PU electrospinning film surface coats the methanol solution that FAS concentration is 1wt%, and every 30min coating is primary, coats 20-30 times altogether, then into
Row vacuum drying, drying temperature are 60-75 DEG C, drying time 16-20h, form FPU electrospinning film on 2 surface of PVDF electrospinning film
3, composite cellulosic membrane is made.
Step 4, composite cellulosic membrane is heat-treated；By 130-140 DEG C of hot wind to the two sides of composite cellulosic membrane into
Row heat treatment, heating time 5-15min.
Step 5,3 surface of FPU electrospinning film is preheating to 40 DEG C, is 0.1-0.2wt% by nano SiO 2 particle concentration
Acetone soln uniformly scratch to 3 surface of FPU electrospinning film, 110 DEG C at a temperature of, vacuum drying 10 minutes, scrape coated baking repeatedly
It is 3 times dry.
High waterproof height obtained breathes freely nano fibrous membrane breaking strength as 8.54MPa or more, and elongation is 42.15%；This
It invents 3 place face resistance to hydrostatic pressure value of FPU electrospinning film and reaches 132KPa, 1 place face penetrability of PVB electrospinning film is 10.8kgm-2d-1。
By above-mentioned specific embodiment, the beneficial effects of the present invention are: simple production process of the present invention is reasonable, manufacturing cost
It is low, industrialized mass production can be suitable for, the high waterproof height of preparation is breathed freely, and nanofiber film properties are stable, and high yield rate changes
It has been apt to nano fibrous membrane in the applied defect in waterproof and breathable field, has been conducive to promote and apply.The ventilative nanometer of high waterproof height of the invention
Tunica fibrosa improves the problem of existing single layer nano fibrous membrane intensity difference, and PVDF electrospinning film 2 and FPU electrospinning film 3 are compound, can
Tearing toughness is effectively improved, and PVB electrospinning film 1 can be improved the flexibility of FPU electrospinning film 3, by sandwich composite construction,
Breaking strength is in 5MPa or more, and elongation is in 35-45%；3 place face of FPU electrospinning film of the present invention has good waterproof performance,
Resistance to hydrostatic pressure value reaches 100KPa, and 1 place face of PVB electrospinning film has good permeability, penetrability 10.1kgm-2d-1.This
The 3 place face of FPU electrospinning film of invention is waterproof surface, and FPU electrospinning 3 fibre structures of film are uniform, fine and closely woven, and uniform pore diameter is formed after intertexture
Porous structure, the average pore size of FPU electrospinning film 3 is small, while 3 hydrophobic performance of FPU electrospinning film is good, is carried out by silicon fluoride hydrophobic
It is modified, lotus leaf effect is formed, FPU electrospinning film 3 is made to have high-strength waterproof performance；And 1 place face of PVB electrospinning film is ventilative
Face, the present invention ensure that good permeability by " adsorption -diffusion " effect and " capillary-diffusion " effect, due to PVB electricity
Spinning film 1 has hydrophily, and PVDF electrospinning film 2 and 3 hydrophobicity of FPU electrospinning film are good, and aqueous vapor is adsorbed by PVB electrospinning film 1, then from
The high side of humidity is diffused into the low side of humidity, realizes one-way wet-guide；Simultaneously between the fiber of PVDF electrospinning film 2 between fiber
Average pore size be greater than FPU electrospinning film 3, aqueous vapor move due to pressure difference to 3 place side of FPU electrospinning film, and it is electric to be then diffused into FPU
3 outside of film is spun, realizes that one-way wet-guide is ventilative.In addition, 1 flexibility of PVB electrospinning film is good, sense of touch is comfortable, is suitable for dress.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (6)
- The nano fibrous membrane 1. a kind of high waterproof height is breathed freely, which is characterized in that including PVB electrospinning film, PVDF electrospinning film and FPU electrospinning Film；The PVB electrospinning film, PVDF electrospinning film and FPU electrospinning film are laminated compound from inside to outside；The PVB electrospinning film is by poly- second Enol butyral nanofiber is interwoven；The average diameter of the polyvinyl butyral nanofiber is 150-400nm；Institute Stating PVDF electrospinning film is to be formed by polyvinylidene fluoride nanometer fiber interweaving；The average diameter of the polyvinylidene fluoride nanometer fiber is 400-600nm；The FPU electrospinning film is to be interwoven through the modified polyurethane nanofiber of silicon fluoride；The polyurethane nano The diameter of fiber is 200-300nm.
- The nano fibrous membrane 2. high waterproof height according to claim 1 is breathed freely, which is characterized in that the thickness of the PVB electrospinning film Degree is 0.010-0.025mm.
- The nano fibrous membrane 3. high waterproof height according to claim 1 is breathed freely, which is characterized in that the PVB electrospinning film and FPU The thickness ratio of electrospinning film is 1:(1.2-1.6).
- The nano fibrous membrane 4. high waterproof height according to claim 3 is breathed freely, which is characterized in that in the FPU electrospinning film table Face is coated with silica nanometer coating.
- The preparation method of nano fibrous membrane 5. a kind of high waterproof height is breathed freely, which comprises the following steps:Step 1, PVB electrospinning film is prepared；The PVB powder end for weighing certain mass, is added dehydrated alcohol, and being configured to mass fraction is 6- 8% PVB spinning solution, is sufficiently stirred by magnetic stirring apparatus, makes the sufficiently dissolution of PVB powder end；Then pass through electrostatic spinning Device carries out spinning and prepares PVB electrospinning film, and PVB spinning solution is injected in needle tubing and carries out electrostatic spinning, using aluminium foil as substrate, spinning Condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 12-25kV, and receiving distance is 13-16cm, spinning speed For 0.5-1mL/h, the thickness control of PVB electrospinning film is in 0.010-0.025mm；Step 2, in the compound PVDF electrospinning film of PVB electrospinning film surface；A certain amount of PVDF powder is weighed, DMF and acetone are dissolved into Volume ratio be 6/4 in the mixed solvent, in 40 DEG C of water-baths heat and be sufficiently stirred by magnetic stirring apparatus, make PVDF Powder sufficiently dissolves, and prepares the PVDF spinning solution that mass fraction is 13-16%；By electrostatic spinning apparatus to PVB electrospinning film table Face carries out continuation spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity be 40 ± 5%, spinning voltage 15-18kV, receive away from 0.010-0.040 μm is maintained at from the thickness for 15-20cm, spinning speed 0.5-1mL/h, PVDF electrospinning film；Step 3, in the compound FPU electrospinning film of PVDF electrospinning film surface；A certain amount of PU particle is weighed to be added to dissolved with NaCl's It in DMF solvent, is sufficiently stirred by magnetic stirring apparatus, dissolves PU particle sufficiently, preparing mass fraction is 15-18%'s PU spinning solution, in PU spinning solution, the mass fraction of NaCl is 0.01%；Continued by electrostatic spinning apparatus to PVDF electrospinning film Surface carries out spinning, spinning condition: temperature is 25 ± 3 DEG C；Humidity is 40 ± 5%, spinning voltage 13-16kV, receives distance For 15-20cm, spinning speed 0.5-1mL/h, PU electrospinning film is prepared；PU electrospinning film surface is carried out using plasma instrument Activation is activated power control in 100W, pressure control handles time 1-3min in 20Pa under helium environment；Then exist PU electrospinning film surface coats the methanol solution that FAS concentration is 1wt%, and every 30min coating is primary, coats 20-30 times altogether, then into Row vacuum drying, drying temperature are 60-75 DEG C, drying time 16-20h, form FPU electrospinning film in PVDF electrospinning film surface, Composite cellulosic membrane is made；Step 4, composite cellulosic membrane is heat-treated；Heat is carried out by two sides of 130-140 DEG C of the hot wind to composite cellulosic membrane Processing, heating time 5-15min.
- The preparation method of nano fibrous membrane 6. high waterproof height according to claim 5 is breathed freely, which is characterized in that further include step Rapid 5, FPU electrospinning film surface is preheating to 40 DEG C, nano SiO 2 particle concentration is equal for the acetone soln of 0.1-0.2wt% It is even blade coating arrive FPU electrospinning film surface, 110 DEG C at a temperature of, vacuum drying 10 minutes, repeatedly blade coating drying 3 times, FPU electricity It spins film surface and forms silica nanometer coating.
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| CN115122731A (en) * | 2022-07-06 | 2022-09-30 | 江苏梦吉妮科技集团有限公司 | Skin-friendly waterproof moisture-permeable nanofiber fabric and preparation method thereof |
| CN115122731B (en) * | 2022-07-06 | 2023-06-16 | 江苏梦吉妮科技集团有限公司 | Skin-friendly waterproof moisture-permeable nanofiber fabric and preparation method thereof |
| CN115161879A (en) * | 2022-07-12 | 2022-10-11 | 广东职业技术学院 | Method for preparing polyvinyl butyral micro-nano fiber through rotor centrifugal spinning and application |
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