CN105887333B - Three dimensional tortuous nano fibrous membrane and its electrospinning process - Google Patents

Three dimensional tortuous nano fibrous membrane and its electrospinning process Download PDF

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Publication number
CN105887333B
CN105887333B CN201610406884.XA CN201610406884A CN105887333B CN 105887333 B CN105887333 B CN 105887333B CN 201610406884 A CN201610406884 A CN 201610406884A CN 105887333 B CN105887333 B CN 105887333B
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spinning
dimensional tortuous
tortuous
syringe needle
dimensional
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CN105887333A (en
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丁彬
李玉瑶
赵兴雷
王珊
印霞
俞建勇
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Shanxi Huarui Nano New Material Technology Co ltd
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Donghua University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • 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
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • 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
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • 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
    • 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
    • D04H1/76—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 otherwise than in a plane, e.g. in a tubular way
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/39—Electrospinning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/24—Mechanical properties, e.g. strength

Abstract

The present invention relates to a kind of three dimensional tortuous nano fibrous membrane and its electrospinning process, during electrostatic spinning spining technology is circulated by using tortuous template reception technique, syringe needle 3 D stereo alignment technology and gradient electric field, the three dimensional tortuous nano-fiber composite film with the fluffy stepped construction of adhesion is obtained, three dimensional tortuous nano-fiber composite film loft layer bulk density is 0.006 0.084g/cm3, tack coat bulk density is 0.01 0.1g/cm3, fiber film-strength is 5 100MPa, and to filter efficiency >=80% of 0.006 10 μm of particles of particle diameter, resistance pressure drop is in below 25Pa.Preparation technology of the present invention is simple, and cost is cheap, and the composite filter material filter efficiency of preparation is high, and resistance pressure drop is small, has broad prospect of application in individual protection field and indoor air purification field.

Description

Three dimensional tortuous nano fibrous membrane and its electrospinning process
Technical field
The invention belongs to filtering material preparing technical field, is related to a kind of three dimensional tortuous nano fibrous membrane and its electrostatic spinning side Method, more particularly to a kind of three dimensional tortuous nanofiber filtration material and its electrospinning process, specifically one kind passes through The three dimensional tortuous Nanowire that template reception technique, syringe needle 3 D stereo alignment technology and gradient electric field circulation spining technology are combined Dimensional filter material and its electrospinning process.
Background technology
The haze pollution problem serious threat that China's most area persistently occurs in recent years the health of people, Haze environment dropping window is taken a breath turns into paradox with indoor cleaning, and therefore, exploitation haze window screening filtering material, which turns into, solves this The effective way of one contradiction.Existing haze window screening filtering material is difficult to meet high efficiency, the filtration needs of low pressure resistance, nothing simultaneously Method realizes effective protection to haze.Electrostatic spinning nano fiber is due to fibre diameter is small, aperture is small, porosity is high, structure The features such as adjustability is strong, it, which is combined the composite filter material prepared with base material, has the advantages that filtration efficiency, low-drag, The ideal material for preparing high-performance window screening is thus become, there is huge application value.It is disclosed to prepare Static Spinning nanometer The technology of fiber window screening filtering material has：A kind of haze nanometer window screening preparation method (CN201410272399.9), printing opacity, thoroughly Gas, Coulomb repulsion PM2.5 air-filtering membranes and preparation method (CN201510307864.2), a kind of nano fibrous membrane window screening (CN201520278851.2) a kind of, nanometer anti-fog haze screen window (CN201520338542.X), haze screen window (CN201520696501.8) a kind of, the anti-haze screen door structure of the adjustable self assembly DIY antibacterials of new size (CN201520785799.X), the strainability research (paper) of Static Spinning polylactic acid nano fiber composite filtering material, acetic acid nanometer The preparation of fiber/PP spun-bonded non-woven air filtration composites and performance study (paper), the compound mistakes of melt Static Spinning PET The preparation of filter material material and performance study (paper), the research (paper) of meltblown/spunbonded composite non-weaving cloth filtering material, Static Spinning The structural behaviour of fiber/non-woven fabric composite filter material is all directly to spray electrostatic spinning nano fiber with simulation (Master's thesis) It is coated onto to receive and prepares nanofiber composite filter material, prepared nanofiber composite filter material generally existing mistake on base material The problem of efficiency is relatively low, resistance pressure drop is big is filtered, therefore the window screening filtering material of novel high-performance need to be developed.
The content of the invention
It is an object of the invention to provide three dimensional tortuous nano fibrous membrane and its electrospinning process, efficiently solves existing skill Filtering material filter efficiency prepared by art is relatively low, the problem of resistance pressure drop is big.
The electrospinning process of the three dimensional tortuous nano fibrous membrane of the present invention, Static Spinning is carried out by polymer spinning solution Silk, it is characterized in that：Using three dimensional tortuous receiving plane；The corresponding one group of spinning syringe needle of each fluctuating of the three dimensional tortuous receiving plane, The profile that the needle point of the spinning syringe needle is formed is consistent with the three dimensional tortuous receiving plane；Every group of spinning syringe needle comprise at least it is left, Neutralize right three rows, the peak of each fluctuating of three dimensional tortuous receiving plane, left bank and right row described in the spinning syringe needle face of middle row Spinning syringe needle correspond to respectively the three dimensional tortuous receiving plane fluctuating centre position, the spinning syringe needle of left bank is perpendicular to described The left side plan of the fluctuating of three dimensional tortuous receiving plane or parallel to the three dimensional tortuous receiving plane fluctuating left side curved surface Normal direction, the spinning syringe needle of right row is perpendicular to the right side plan of the fluctuating of the three dimensional tortuous receiving plane or parallel to institute State the normal direction in the centre position of the curved surface on the right side of the fluctuating of three dimensional tortuous receiving plane.
As preferable technical scheme：
The electrospinning process of three dimensional tortuous nano fibrous membrane as described above, the technique of the electrostatic spinning are：
The concentration of polymer spinning solution is 10-40wt%；
Spinning order pressed according to spinning syringe needle in, it is left and right or in, it is right, it is left circulation spinning in turn, period 1-60；
The spinning syringe needle spinning parameter of middle row：Voltage 15-100kV, receive distance 10-150cm, rate of flooding 0.1- 10mL/h, 15-35 DEG C of temperature, humidity 5-90%, spinning time 5-300s；
The spinning parameter of left bank and the spinning syringe needle of right row is：Voltage 10-90kV, distance 10-150cm is received, irrigated Speed 0.1-10mL/h, 15-35 DEG C of temperature, humidity 5-90%, spinning time 5-300s；
And meet：The spinning syringe needle voltage ＞ left banks of middle row or the spinning syringe needle voltage of right row；
Or further：
After one layer of nano fibrous membrane being spun by aforementioned electrostatic spinning technique, then by aforementioned electrostatic spinning technique route and same width The voltage that degree reduces 10-15% spins one layer of fluffy nano fibrous membrane, and so alternately, spinning obtains the three dimensional tortuous of stepped construction Nano-fiber composite film；
Spun nano fibrous membrane 40-200 DEG C of drying 10-180min in vacuum drying oven.
The electrospinning process of three dimensional tortuous nano fibrous membrane as described above, the three dimensional tortuous receiving plane refer to：Connect The receiving plane for receiving substrate is three dimensional tortuous shape, and either the receiving plane of reception base material is three dimensional tortuous shape or is plane The receiving plane for receiving base material is compounded with removable type three dimensional tortuous shape template.
The electrospinning process of three dimensional tortuous nano fibrous membrane as described above, the removable type three dimensional tortuous shape mould Plate is hot melt material or water-soluble high-molecular material.
The electrospinning process of three dimensional tortuous nano fibrous membrane as described above, reception base material or planar receiver base material Aperture is 0.01-3mm, thickness 0.1-2mm, grammes per square metre 30-100g/m2, receiving plane is the meander-like base of three dimensional tortuous shape Material rolls over high h=5-40mm, 5-45 ° of knuckle.
The electrospinning process of three dimensional tortuous nano fibrous membrane as described above, each song of the three dimensional tortuous receiving plane It is triangle, trapezoidal or waveform to roll over unit meandering manner；Triangle rolls over high h=5-40mm, rolls over wide w=hcot α, knuckle α =5-45 °；The high h=5-40mm of trapezoidal folding, rolls over wide w=hcot α+b, and it is 2-20mm to roll over away from b, α=5-45 ° of knuckle；Waveform High h=5-40mm is rolled over, rolls over wide w=5-40mm, α=5-45 ° of knuckle；Each tortuous unit is one group, and number is organized in electrospinning unit and is 3-20, the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 1-50.
The electrospinning process of three dimensional tortuous nano fibrous membrane as described above, in the polymer spinning solution, polymerization Thing is FEP fluorinated ethylene propylene copolymer, perfluoroethylene-propylene, polypropylene, soluble poly tetrafluoroethene, Kynoar, polyvinyl alcohol Butyral, polystyrene, polyester, polyvinyl acetate, nylon 6, polyvinyl alcohol, polymethyl methacrylate, polyaniline, polyoxygenated Ethene, polyvinylpyrrolidone, polyacrylonitrile, polycaprolactone, PET, polytetrafluoroethylene (PTFE), polyethylene glycol, Polyurethane, polysulfones, polyether sulfone, Kynoar-hexafluoropropene, Kynoar-tetrafluoroethylene-perfluoro methyl vinyl ether or One or more of Kynoar-CTFE；
Solvent is formic acid, tetrahydrofuran, water, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, acetone, chloroform, first Phenol, dimethyl sulfoxide (DMSO), methanol, ethanol, propyl alcohol, isopropanol, butanol, isobutanol, toluene, 1-METHYLPYRROLIDONE, MEK or One or more of methyl ethyl ketone.
A kind of three dimensional tortuous nano fibrous membrane, it is characterized in that：Bulk density is 0.006-0.1g/cm3, roll over high h=5- 40mm, α=5-45 ° of knuckle, meander-shaped are triangle, trapezoidal or waveform；Fiber film-strength is 0.1-10MPa, to particle diameter The filter efficiency of 0.006-10 μm of particle is 10-50%, and resistance pressure drop is in below 15Pa.
Invention further provides a kind of three dimensional tortuous nano-fiber composite film, the three dimensional tortuous nano-fiber composite film, It is in macroscopically the nano fibrous membrane of three dimensional tortuous shape, is intervally arranged in a thickness direction in fluffy-bonding, the three dimensional tortuous shape Nano fibrous membrane loft layer bulk density is 0.006-0.084g/cm3, the three dimensional tortuous shape nano fibrous membrane tack coat accumulation Density is 0.01-0.1g/cm3；Tunica fibrosa rolls over high h=5-40mm, α=5-45 ° of knuckle, meander-shaped is triangle, it is trapezoidal or Waveform；Fiber film-strength is 5-100MPa, and to filter efficiency >=80% of 0.006-10 μm of particle of particle diameter, resistance pressure drop exists Below 25Pa.
The present invention can also carry out polymer solution and UV curing agent composite spinning, and complex method can be that polymer is molten Liquid/UV curing agent blending carries out spinning, or both perfusion syringe needle ratio progress are compound by adjustment.In electrostatic spinning module list Ultra violet lamp is installed in member and receives substrate, the fiber that UV curing agent sprays directly is solidified, produces interfibrous adhesion structure, Strengthen the structural stability of layers of nanofibers, improve the binding strength between nanofiber., can by the in-situ solidifying of UV curing agent The stripper-resistance of layers of nanofibers is improved, greatly prolongs the service life of nanofiber filtration material.
Beneficial effect：
1. preparation method technique provided by the invention is simple, it is applicable to a series of extensive polymer-based nano fibers and answers Close the preparation of filtering material.The curved structure of layers of nanofibers can increase the filter area of material, improve filter efficiency, drop simultaneously Lower resistance pressure drop, so that nanofiber composite filter material has filter efficiency height, the performance that resistance pressure drop is low, translucency is good concurrently Feature.
2., can be by controlling the arrangement model of syringe needle to make in addition, this preparation method has good fibre structure controllability It is adapted with receiving surface structure, so as to realize the variation of nanofiber filtration material structure.
3. using layers of nanofibers macrobend shape reduce resistance pressure drop on the basis of, by adjust spinning away from From, change electric field level, produce the inside fluff bulk structure of layers of nanofibers, further reduce resistance pressure drop.Meanwhile utilize Interfibrous adhesion structure, strengthen the structural stability of layers of nanofibers.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Fixed scope.
Embodiment 1
A kind of method of electrostatic spinning of three dimensional tortuous nano fibrous membrane, specific spinning technique are as follows：
1) FEP fluorinated ethylene propylene copolymer is dissolved in formic acid, forms the spinning solution that concentration is 25wt%；
2) it is bent from the reception substrate that receiving plane is three dimensional tortuous shape, each tortuous unit of its three dimensional tortuous receiving plane Folding mode is triangle, and triangle rolls over high h=5mm, rolls over wide w=57mm, knuckle α=5 °, and each tortuous unit is one group, spinning It is 3 that number is organized in unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 1；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 15kV, receiving distance is 150cm, rate of flooding 0.1mL/h, 15 DEG C of temperature, humidity 5%, spinning time 5s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 10kV, it is 150cm to receive distance, rate of flooding 0.1mL/h, 15 DEG C of temperature, humidity 5%, the spinning time 5s, the perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, jet emission direction is hung down Directly in left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open the filling that control right lateral aspect syringe needle goes out liquid Note switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to right zig zag plane；
4) circulation step 3) 1 time, three dimensional tortuous nano fibrous membrane is removed in 40 DEG C of drying 180min of vacuum drying oven；
Test shows, obtained three dimensional tortuous nano fibrous membrane, bulk density 0.006g/cm3, high h=5mm is rolled over, is rolled over Angle α=5 °, meander-shaped are triangle；Fiber film-strength is 0.1MPa, and the filter efficiency to 0.006 μm of particle of particle diameter is 10%, resistance pressure drop 15Pa.
Embodiment 2
A kind of method of electrostatic spinning of three dimensional tortuous nano fibrous membrane, specific spinning technique are as follows：
1) perfluoroethylene-propylene is dissolved in tetrahydrofuran, forms the spinning solution that concentration is 20wt%；
2) it is 0.01mm, thickness 0.5mm, grammes per square metre 30g/m from aperture2, receiving plane is connecing for three dimensional tortuous shape Base material is received, each tortuous unit meandering manner of its three dimensional tortuous receiving plane is triangle, and triangle rolls over high h=40mm, rolls over wide w For 40mm, knuckle α=45 °, each tortuous unit is one group, and it is 5 that number is organized in electrospinning unit, the syringe needle on each group with it is left, in, Right three rows are a line, every group of line number 5；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 30kV, receiving distance is 80cm, rate of flooding 2mL/h, 20 DEG C of temperature, humidity 15%, spinning time 20s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 20kV, it is 80cm to receive distance, rate of flooding 2mL/h, 20 DEG C of temperature, humidity 15%, spinning time 20s, The perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction vertical In left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open the perfusion that control right lateral aspect syringe needle goes out liquid Switch, the conductive wire on syringe needle is adjusted, makes jet emission direction perpendicular to right zig zag plane；
4) circulation step 3) 15 times, three dimensional tortuous nano fibrous membrane is removed in 50 DEG C of drying 170min of vacuum drying oven；
Test shows, obtained three dimensional tortuous nano fibrous membrane, bulk density 0.02g/cm3, high h=40mm is rolled over, is rolled over Angle α=45 °, meander-shaped are triangle；Fiber film-strength is 3MPa, and the filter efficiency to 4 μm of particles of particle diameter is 20%, resistance Pressure drop is 12Pa.
Embodiment 3
A kind of method of electrostatic spinning of three dimensional tortuous nano fibrous membrane, specific spinning technique are as follows：
1) it is 1 by mass ratio:1 FEP fluorinated ethylene propylene copolymer and the mixture of perfluoroethylene-propylene are dissolved in N, N- dimethyl In formamide, the spinning solution that concentration is 20wt% is formed；
2) it is 1mm, thickness 0.8mm, grammes per square metre 60g/m from aperture2, receiving plane is compounded with removable type three dimensional tortuous The planar receiver base material of shape gelatin template, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are trapezoidal, ladder Shape rolls over high h=5mm, and it is 59mm to roll over wide w, and it is 2mm to roll over away from b, and knuckle α=5 °, each tortuous unit is one group, group in electrospinning unit Number is 10, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 15；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 50kV, receiving distance is 67cm, rate of flooding 5mL/h, 25 DEG C of temperature, humidity 45%, spinning time 100s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 45kV, it is 67cm to receive distance, rate of flooding 5mL/h, 25 DEG C of temperature, humidity 45%, the spinning time 100s, the perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open control right lateral aspect syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to right zig zag plane；
4) circulation step 3) 25 times, three dimensional tortuous nano fibrous membrane is removed in 60 DEG C of drying 130min of vacuum drying oven；
Test shows, obtained three dimensional tortuous nano fibrous membrane, bulk density 0.04g/cm3, roll over high h=5mm, knuckle α=5 °, meander-shaped are trapezoidal；Fiber film-strength is 6MPa, and the filter efficiency to 6 μm of particles of particle diameter is 30%, resistance pressure drop For 11Pa.
Embodiment 4
A kind of method of electrostatic spinning of three dimensional tortuous nano fibrous membrane, specific spinning technique are as follows：
1) polyurethane is dissolved in DMA, forms the spinning solution that concentration is 22wt%；
2) it is 1.5mm, thickness 1mm, grammes per square metre 75g/m from aperture2, receiving plane is compounded with removable type three dimensional tortuous The planar receiver base material of shape starch template, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are trapezoidal, ladder Shape rolls over high h=40mm, and it is 60mm to roll over wide w, and it is 20mm to roll over away from b, and knuckle α=45 °, each tortuous unit is one group, electrospinning unit Middle group of number is 15, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 30；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 65kV, receiving distance is 18cm, rate of flooding 6mL/h, 20 DEG C of temperature, humidity 60%, spinning time 150s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 55kV, it is 18cm to receive distance, rate of flooding 6mL/h, 20 DEG C of temperature, humidity 60%, the spinning time 150s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；
4) circulation step 3) 40 times, remove three dimensional tortuous nano fibrous membrane, washing is removed after planar receiver base material true Empty 80 DEG C of drying 120min of baking oven；
Test shows, obtained three dimensional tortuous nano fibrous membrane, bulk density 0.06g/cm3, high h=40mm is rolled over, is rolled over Angle α=45 °, meander-shaped are trapezoidal；Fiber film-strength is 7MPa, and the filter efficiency to 7 μm of particles of particle diameter is 35%, resistance pressure It is reduced to 10Pa.
Embodiment 5
A kind of method of electrostatic spinning of three dimensional tortuous nano fibrous membrane, specific spinning technique are as follows：
1) it is soluble poly tetrafluoroethene is soluble in water, form the spinning solution that concentration is 25wt%；
2) it is bent from the reception substrate that receiving plane is three dimensional tortuous shape, each tortuous unit of its three dimensional tortuous receiving plane Folding mode is waveform, and waveform rolls over high h=5mm, rolls over wide w=5mm, knuckle α=5 °, and each tortuous unit is one group, spinning It is 18 that number is organized in unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 40；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 90kV, receiving distance is 23cm, rate of flooding 8mL/h, 30 DEG C of temperature, humidity 80%, spinning time 250s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 80kV, it is 23cm to receive distance, rate of flooding 8mL/h, 30 DEG C of temperature, humidity 80%, the spinning time 250s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；
4) circulation step 3) 50 times, three dimensional tortuous nano fibrous membrane is removed in 100 DEG C of drying 140min of vacuum drying oven；
Test shows, obtained three dimensional tortuous nano fibrous membrane, bulk density 0.08g/cm3, roll over high h=5mm, knuckle α=5 °, meander-shaped are waveform；Fiber film-strength is 8MPa, and the filter efficiency to 8 μm of particles of particle diameter is 40%, resistance pressure It is reduced to 9Pa.
Embodiment 6
A kind of method of electrostatic spinning of three dimensional tortuous nano fibrous membrane, specific spinning technique are as follows：
1) Kynoar is dissolved in acetone, forms the spinning solution that concentration is 18wt%；
2) it is 3mm, thickness 2mm, grammes per square metre 100g/m from aperture2, receiving plane is the reception base of three dimensional tortuous shape Material, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are waveform, and waveform rolls over high h=40mm, rolls over wide w= 40mm, knuckle α=45 °, each tortuous unit are one group, and it is 20 that number is organized in electrospinning unit, the syringe needle on each group with it is left, in, Right three rows are a line, every group of line number 50；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 100kV, receiving distance is 10cm, rate of flooding 10mL/h, 35 DEG C of temperature, humidity 90%, spinning time 300s；It is then shut off middle perfusion switch, regulation Technological parameter is：Voltage 90kV, it is 10cm to receive distance, rate of flooding 10mL/h, 35 DEG C of temperature, humidity 90%, the spinning time 300s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；
4) circulation step 3) 60 times, three dimensional tortuous nano fibrous membrane is removed in 90 DEG C of drying 100min of vacuum drying oven；
Test shows, obtained three dimensional tortuous nano fibrous membrane, bulk density 0.1g/cm3, roll over high h=40mm, knuckle α=45 °, meander-shaped are waveform；Fiber film-strength is 10MPa, and the filter efficiency to 10 μm of particles of particle diameter is 50%, resistance Pressure drop is 8Pa.
Embodiment 7
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polyvinyl butyral resin is dissolved in chloroform, forms the spinning solution that concentration is 23wt%；
2) it is bent from the reception substrate that receiving plane is three dimensional tortuous shape, each tortuous unit of its three dimensional tortuous receiving plane Folding mode is triangle, and triangle rolls over high h=5mm, and it is 57mm to roll over wide w, and knuckle α=5 °, each tortuous unit is one group, spinning It is 3 that number is organized in unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 1；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 15kV, receiving distance is 65cm, rate of flooding 0.1mL/h, 15 DEG C of temperature, humidity 5%, spinning time 5s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 10kV, it is 65cm to receive distance, rate of flooding 0.1mL/h, 15 DEG C of temperature, humidity 5%, spinning time 5s, The perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction vertical In left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open the perfusion that control right lateral aspect syringe needle goes out liquid Switch, the conductive wire on syringe needle is adjusted, makes jet emission direction perpendicular to right zig zag plane；So far, adhesion structure nanometer Fibrous layer spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 10% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 1 time, three dimensional tortuous nano-fiber composite film is removed in 110 DEG C of drying of vacuum drying oven 120min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.006g/cm3, tack coat bulk density is 0.01g/cm3；Tunica fibrosa rolls over high h=5mm, and knuckle α=5 °, meander-shaped is triangle；Fiber film-strength is 5MPa, to particle diameter The filter efficiency of 0.006 μm of particle is 80%, resistance pressure drop 25Pa.
Embodiment 8
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polystyrene is dissolved in mass ratio for 1:In 1 acetone and the mixed solution of chloroform, it is 22wt% to form concentration Spinning solution；
2) it is 0.5mm, thickness 0.1mm, grammes per square metre 45g/m from aperture2, receiving plane is the reception of three dimensional tortuous shape Base material, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are triangle, and triangle rolls over high h=40mm, rolls over wide w= 40mm, knuckle α=45 °, each tortuous unit are one group, and it is 5 that number is organized in electrospinning unit, and the syringe needle on each group is with left, center, right Three rows are a line, every group of line number 5；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 30kV, receiving distance is 40cm, rate of flooding 2mL/h, 20 DEG C of temperature, humidity 15%, spinning time 20s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 20kV, it is 40cm to receive distance, rate of flooding 2mL/h, 20 DEG C of temperature, humidity 15%, spinning time 20s, The perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction vertical In left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open the perfusion that control right lateral aspect syringe needle goes out liquid Switch, the conductive wire on syringe needle is adjusted, makes jet emission direction perpendicular to right zig zag plane；So far, adhesion structure nanometer Fibrous layer spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 11% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 18 times, three dimensional tortuous nano-fiber composite film is removed in 120 DEG C of drying of vacuum drying oven 110min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.01g/cm3, tack coat bulk density is 0.03g/cm3；Tunica fibrosa rolls over high h=40mm, and knuckle α=45 °, meander-shaped is triangle；Fiber film-strength is 20MPa, right The filter efficiency of 2 μm of particles of particle diameter is 81%, resistance pressure drop 24Pa.
Embodiment 9
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polyester is dissolved in cresols, forms the spinning solution that concentration is 28wt%；
2) it is 1mm, thickness 0.8mm, grammes per square metre 60g/m from aperture2, receiving plane is compounded with removable type three dimensional tortuous The planar receiver base material of shape gelatin template, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are trapezoidal, ladder Shape rolls over high h=5mm, and it is 59mm to roll over wide w, and it is 2mm to roll over away from b, and knuckle α=5 °, each tortuous unit is one group, group in electrospinning unit Number is 10, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 15；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 50kV, receiving distance is 67cm, rate of flooding 5mL/h, 25 DEG C of temperature, humidity 45%, spinning time 100s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 45kV, it is 67cm to receive distance, rate of flooding 5mL/h, 25 DEG C of temperature, humidity 45%, the spinning time 100s, the perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open control right lateral aspect syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to right zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 11% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 25 times, three dimensional tortuous nano-fiber composite film is removed in 130 DEG C of drying of vacuum drying oven 100min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.04g/cm3, tack coat bulk density is 0.04g/cm3；The high h=5mm of tunica fibrosa folding, knuckle α=5 °, meander-shaped are trapezoidal；Fiber film-strength is 40MPa, to 4 μm of particle diameter The filter efficiency of particle is 82%, resistance pressure drop 23Pa.
Embodiment 10
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polyvinyl acetate is dissolved in dimethyl sulfoxide (DMSO), forms the spinning solution that concentration is 15wt%；
2) it is 1.5mm, thickness 1mm, grammes per square metre 75g/m from aperture2, receiving plane is compounded with removable type three dimensional tortuous The planar receiver base material of shape carboxymethyl cellulose template, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are Trapezoidal, the trapezoidal high h=40mm of folding, it is 60mm to roll over wide w, and it is 20mm to roll over away from b, and knuckle α=45 °, each tortuous unit is one group, is spun It is 15 that number is organized in silk unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 30；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 65kV, receiving distance is 24cm, rate of flooding 6mL/h, 20 DEG C of temperature, humidity 60%, spinning time 150s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 55kV, it is 24cm to receive distance, rate of flooding 6mL/h, 20 DEG C of temperature, humidity 60%, the spinning time 150s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 13% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 40 times, three dimensional tortuous nano-fiber composite film is removed, washing removes planar receiver base In 135 DEG C of drying 90min of vacuum drying oven after material；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.02g/cm3, tack coat bulk density is 0.06g/cm3；Tunica fibrosa rolls over high h=40mm, knuckle α=45 °, and meander-shaped is trapezoidal；Fiber film-strength is 60MPa, to grain The filter efficiency of the 6 μm of particles in footpath is 83%, resistance pressure drop 22Pa.
Embodiment 11
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) nylon 6 is dissolved in methanol, forms the spinning solution that concentration is 10wt%；
2) it is bent from the reception substrate that receiving plane is three dimensional tortuous shape, each tortuous unit of its three dimensional tortuous receiving plane Folding mode is waveform, and waveform rolls over high h=5mm, rolls over wide w=5mm, knuckle α=5 °, and each tortuous unit is one group, spinning It is 18 that number is organized in unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 40；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 90kV, receiving distance is 57cm, rate of flooding 8mL/h, 30 DEG C of temperature, humidity 80%, spinning time 250s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 80kV, it is 57cm to receive distance, rate of flooding 8mL/h, 30 DEG C of temperature, humidity 80%, the spinning time 250s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 14% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 50 times, three dimensional tortuous nano-fiber composite film is removed in 140 DEG C of drying of vacuum drying oven 80min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.07g/cm3, tack coat bulk density is 0.08g/cm3；Tunica fibrosa rolls over high h=5mm, and knuckle α=5 °, meander-shaped is waveform；Fiber film-strength is 80MPa, to grain The filter efficiency of the 8 μm of particles in footpath is 84%, resistance pressure drop 21Pa.
Embodiment 12
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polyvinyl alcohol is dissolved in ethanol, forms the spinning solution that concentration is 35wt%；
2) it is 2mm, thickness 2mm, grammes per square metre 100g/m from aperture2, receiving plane is the reception base of three dimensional tortuous shape Material, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are waveform, and waveform rolls over high h=40mm, rolls over wide w= 40mm, knuckle α=45 °, each tortuous unit are one group, and it is 20 that number is organized in electrospinning unit, the syringe needle on each group with it is left, in, Right three rows are a line, every group of line number 50；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 100kV, receiving distance is 40cm, rate of flooding 10mL/h, 35 DEG C of temperature, humidity 90%, spinning time 300s；It is then shut off middle perfusion switch, regulation Technological parameter is：Voltage 90kV, it is 40cm to receive distance, rate of flooding 10mL/h, 35 DEG C of temperature, humidity 90%, the spinning time 300s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 15% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 60 times, three dimensional tortuous nano-fiber composite film is removed in 150 DEG C of drying of vacuum drying oven 70min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.084g/cm3, tack coat bulk density is 0.1g/cm3；Tunica fibrosa rolls over high h=40mm, and knuckle α=45 °, meander-shaped is waveform；Fiber film-strength is 100MPa, right The filter efficiency of 10 μm of particles of particle diameter is 85%, resistance pressure drop 20Pa.
Embodiment 13
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) it is 1 by mass ratio:1:The mixture of 1 polystyrene, polyester and nylon 6 is dissolved in propyl alcohol, and forming concentration is 21wt% spinning solution；
2) it is bent from the reception substrate that receiving plane is three dimensional tortuous shape, each tortuous unit of its three dimensional tortuous receiving plane Folding mode is triangle, and triangle rolls over high h=5mm, and it is 57mm to roll over wide w, and knuckle α=5 °, each tortuous unit is one group, spinning It is 3 that number is organized in unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 1；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 15kV, receiving distance is 130cm, rate of flooding 0.1mL/h, 15 DEG C of temperature, humidity 5%, spinning time 5s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 10kV, it is 130cm to receive distance, rate of flooding 0.1mL/h, 15 DEG C of temperature, humidity 5%, the spinning time 5s, the perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, jet emission direction is hung down Directly in left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open the filling that control right lateral aspect syringe needle goes out liquid Note switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to right zig zag plane；So far, adhesion structure is received Rice fibrous layer spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 10% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 1 time, three dimensional tortuous nano-fiber composite film is removed in 160 DEG C of drying of vacuum drying oven 60min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.03g/cm3, tack coat bulk density is 0.05g/cm3；Tunica fibrosa rolls over high h=5mm, and knuckle α=5 °, meander-shaped is triangle；Fiber film-strength is 40MPa, to grain The filter efficiency of the 10 μm of particles in footpath is 85%, resistance pressure drop 15Pa.
Embodiment 14
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polymethyl methacrylate is dissolved in mass ratio for 1:1:In the mixed solution of 1 methanol, ethanol and propyl alcohol, shape Into the spinning solution that concentration is 24wt%；
2) it is 0.5mm, thickness 0.5mm, grammes per square metre 45g/m from aperture2, receiving plane is the reception of three dimensional tortuous shape Base material, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are triangle, and triangle rolls over high h=40mm, and rolling over wide w is 40mm, knuckle α=45 °, each tortuous unit are one group, and it is 5 that number is organized in electrospinning unit, and the syringe needle on each group is with left, center, right Three rows are a line, every group of line number 5；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 30kV, receiving distance is 40cm, rate of flooding 2mL/h, 20 DEG C of temperature, humidity 15%, spinning time 20s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 20kV, it is 40cm to receive distance, rate of flooding 2mL/h, 20 DEG C of temperature, humidity 15%, spinning time 20s, The perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction vertical In left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open the perfusion that control right lateral aspect syringe needle goes out liquid Switch, the conductive wire on syringe needle is adjusted, makes jet emission direction perpendicular to right zig zag plane；So far, adhesion structure nanometer Fibrous layer spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 11% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 18 times, three dimensional tortuous nano-fiber composite film is removed in 170 DEG C of drying of vacuum drying oven 50min；
Test shows obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.053g/cm3, tack coat bulk density is 0.079g/cm3；Tunica fibrosa rolls over high h=40mm, and knuckle α=45 °, meander-shaped is triangle；Fiber film-strength is 60MPa, right The filter efficiency of 10 μm of particles of particle diameter is 88%, resistance pressure drop 20Pa.
Embodiment 15
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) polyaniline is dissolved in isopropanol, forms the spinning solution that concentration is 30wt%；
2) it is 1mm, thickness 0.8mm, grammes per square metre 60g/m from aperture2, receiving plane is compounded with removable type three dimensional tortuous The planar receiver base material of shape agar-agar, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are trapezoidal, trapezoidal folding High h=5mm, it is 59mm to roll over wide w, and it is 2mm to roll over away from b, and knuckle α=5 °, each tortuous unit is one group, and number is organized in electrospinning unit and is 10, the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 15；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 50kV, receiving distance is 67cm, rate of flooding 5mL/h, 25 DEG C of temperature, humidity 45%, spinning time 100s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 45kV, it is 67cm to receive distance, rate of flooding 5mL/h, 25 DEG C of temperature, humidity 45%, the spinning time 100s, the perfusion switch that orientation syringe needle in control left side goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to left zig zag plane；Keep technological parameter constant, close left side perfusion switch, open control right lateral aspect syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to right zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 11% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 25 times, three dimensional tortuous nano-fiber composite film is removed in 180 DEG C of drying of vacuum drying oven 40min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.014g/cm3, tack coat bulk density is 0.029g/cm3；Tunica fibrosa rolls over high h=5mm, knuckle α=5 °, and meander-shaped is trapezoidal；Fiber film-strength is 60MPa, to particle diameter The filter efficiency of 10 μm of particles is 80%, resistance pressure drop 10Pa.
Embodiment 16
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) Kynoar-tetrafluoroethylene-perfluoro methyl vinyl ether is dissolved in butanol, it is 20wt%'s to form concentration Spinning solution；
2) it is 1.5mm, thickness 1mm, grammes per square metre 75g/m from aperture2, receiving plane is compounded with removable type three dimensional tortuous The planar receiver base material of shape gelatin template, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are trapezoidal, ladder Shape rolls over high h=40mm, and it is 60mm to roll over wide w, and it is 20mm to roll over away from b, and knuckle α=45 °, each tortuous unit is one group, electrospinning unit Middle group of number is 15, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 30；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 65kV, receiving distance is 18cm, rate of flooding 6mL/h, 20 DEG C of temperature, humidity 60%, spinning time 150s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 55kV, it is 18cm to receive distance, rate of flooding 6mL/h, 20 DEG C of temperature, humidity 60%, the spinning time 150s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 13% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 40 times, the compound fenestrated membrane yarn of three dimensional tortuous nanofiber is removed in 190 DEG C of bakings of vacuum drying oven Dry 30min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.053g/cm3, tack coat bulk density is 0.079g/cm3；Tunica fibrosa rolls over high h=40mm, knuckle α=45 °, and meander-shaped is trapezoidal；Fiber film-strength is 70MPa, to grain The filter efficiency of the 5 μm of particles in footpath is 82%, resistance pressure drop 20Pa.
Embodiment 17
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) it is 1 by mass ratio:1:1:1 polyethylene glycol, polyurethane, the mixture of polysulfones and polyether sulfone are dissolved in isobutanol In, form the spinning solution that concentration is 40wt%；
2) it is bent from the reception substrate that receiving plane is three dimensional tortuous shape, each tortuous unit of its three dimensional tortuous receiving plane Folding mode is waveform, and waveform rolls over high h=5mm, rolls over wide w=5mm, knuckle α=5 °, and each tortuous unit is one group, spinning It is 18 that number is organized in unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 40；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 90kV, receiving distance is 46cm, rate of flooding 8mL/h, 30 DEG C of temperature, humidity 80%, spinning time 250s；Middle perfusion switch is then shut off, adjusts work Skill parameter is：Voltage 80kV, it is 46cm to receive distance, rate of flooding 8mL/h, 30 DEG C of temperature, humidity 80%, the spinning time 250s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 14% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 50 times, three dimensional tortuous nano-fiber composite film is removed in 195 DEG C of drying of vacuum drying oven 20min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.042g/cm3, tack coat bulk density is 0.083g/cm3；Tunica fibrosa rolls over high h=5mm, and knuckle α=5 °, meander-shaped is waveform；Fiber film-strength is 15MPa, to grain The filter efficiency of the 10 μm of particles in footpath is 80%, resistance pressure drop 11Pa.
Embodiment 18
A kind of method of electrostatic spinning of three dimensional tortuous nano-fiber composite film, specific spinning technique are as follows：
1) it is 1 by mass ratio:2:The mixture of 1 polyaniline, polyacrylonitrile and polycaprolactone is dissolved in mass ratio for 1:1: 1:1 butanol, toluene, MEK and cresols mixed solution in, form the spinning solution that concentration is 24wt%；
2) it is 3mm, thickness 2mm, grammes per square metre 100g/m from aperture2, receiving plane is the reception base of three dimensional tortuous shape Material, each tortuous unit meandering manner of its three dimensional tortuous receiving plane are waveform, and waveform rolls over high h=40mm, rolls over wide w= 40mm, knuckle α=45 °, each tortuous unit are one group, and it is 20 that number is organized in electrospinning unit, the syringe needle on each group with it is left, in, Right three rows are a line, every group of line number 50；
3) the perfusion switch that control intermediate orientation syringe needle goes out liquid is opened, polymer solution is waved by stretching-solvent of electric field Hair forms nanofiber electrostatic spray to three dimensional tortuous receiving plane, and spinning technology parameter is：Voltage 100kV, receiving distance is 20cm, rate of flooding 10mL/h, 35 DEG C of temperature, humidity 90%, spinning time 300s；It is then shut off middle perfusion switch, regulation Technological parameter is：Voltage 90kV, it is 20cm to receive distance, rate of flooding 10mL/h, 35 DEG C of temperature, humidity 90%, the spinning time 300s, the perfusion switch that control right lateral aspect syringe needle goes out liquid is opened, the conductive wire on syringe needle is adjusted, makes jet emission direction Perpendicular to right zig zag plane；Keep technological parameter constant, close right side perfusion switch, open control left side orientation syringe needle and go out liquid Perfusion switch, adjusts the conductive wire on syringe needle, makes jet emission direction perpendicular to left zig zag plane；So far, adhesion structure Layers of nanofibers spinning is completed；
4) after spinning one layer of nano fibrous membrane by above-mentioned electrostatic spinning process, then by above-mentioned electrostatic spinning process route and same The voltage of amplitude reduction 15% spins one layer of fluffy nano fibrous membrane, and so far, fluff structure layers of nanofibers spinning is completed；
5) circulation step 3) and 4) 60 times, three dimensional tortuous nano-fiber composite film is removed in 200 DEG C of drying of vacuum drying oven 10min；
Test shows, obtained three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, It is intervally arranged in a thickness direction in fluffy-bonding, loft layer bulk density is 0.062g/cm3, tack coat bulk density is 0.01g/cm3；Tunica fibrosa rolls over high h=40mm, and knuckle α=45 °, meander-shaped is waveform；Fiber film-strength is 50MPa, right The filter efficiency of 5 μm of particles of particle diameter is 86%, resistance pressure drop 20Pa.
Embodiment 19-30 spinning technique is substantially identical with embodiment 1-18, the technological parameter to change such as polymer Concentration of species, solvent species and polymer etc., and the performance of the product prepared are as shown in the table.

Claims (9)

1. the electrospinning process of three dimensional tortuous nano fibrous membrane, polymer spinning solution is subjected to electrostatic spinning, it is characterized in that： Using three dimensional tortuous receiving plane；The corresponding one group of spinning syringe needle of each fluctuating of the three dimensional tortuous receiving plane, the spinning syringe needle Needle point form profile it is consistent with the three dimensional tortuous receiving plane；Every group of spinning syringe needle comprises at least left, right three rows of neutralization, in The spinning syringe needle difference of the peak of each fluctuating of three dimensional tortuous receiving plane described in the spinning syringe needle face of row, left bank and right row The centre position of the fluctuating of the corresponding three dimensional tortuous receiving plane, the spinning syringe needle of left bank is perpendicular to the three dimensional tortuous receiving plane Fluctuating right side plan or parallel to the three dimensional tortuous receiving plane fluctuating right side normal to a surface direction, right row Spinning syringe needle perpendicular to the fluctuating of the three dimensional tortuous receiving plane left side plan or parallel to the three dimensional tortuous receive The normal direction in the centre position of the curved surface in the left side of the fluctuating in face.
2. the electrospinning process of three dimensional tortuous nano fibrous membrane according to claim 1, it is characterised in that the electrostatic The technique of spinning is：
Spinning order pressed according to spinning syringe needle in, it is left and right or in, it is right, it is left circulation spinning in turn, period 1-60；
The spinning syringe needle spinning parameter of middle row：Voltage 15-100kV, distance 10-150cm, rate of flooding 0.1-10mL/h are received, 15-35 DEG C of temperature, humidity 5-90%, spinning time 5-300s；
The spinning parameter of left bank and the spinning syringe needle of right row is：Voltage 10-90kV, receive distance 10-150cm, rate of flooding 0.1-10mL/h, 15-35 DEG C of temperature, humidity 5-90%, spinning time 5-300s；
And meet：The spinning syringe needle voltage ＞ left banks of middle row or the spinning syringe needle voltage of right row；
Or further：
After one layer of nano fibrous membrane being spun by aforementioned electrostatic spinning technique, then by aforementioned electrostatic spinning technique route and with amplitude drop Low 10-15% voltage spins one layer of fluffy nano fibrous membrane, and so alternately, spinning obtains the three dimensional tortuous nanometer of stepped construction Composite fiber membrane.
3. the electrospinning process of three dimensional tortuous nano fibrous membrane according to claim 1, it is characterised in that the three-dimensional Tortuous receiving plane refers to：The receiving plane for receiving substrate is three dimensional tortuous shape, or the receiving plane of reception base material is three dimensional tortuous Shape, or it is compounded with removable type three dimensional tortuous shape template for the receiving plane of planar receiver base material.
4. the electrospinning process of three dimensional tortuous nano fibrous membrane according to claim 3, it is characterised in that described to go Except type three dimensional tortuous shape template is hot melt material or water-soluble high-molecular material.
5. the electrospinning process of three dimensional tortuous nano fibrous membrane according to claim 3, it is characterised in that receive base material Or the aperture of planar receiver base material is 0.01-3mm, thickness 0.1-2mm, grammes per square metre 30-100g/m2；Receiving plane is three-dimensional The meander-like base material of meander-shaped rolls over high h=5-40mm, α=5-45 ° of knuckle.
6. the electrospinning process of three dimensional tortuous nano fibrous membrane according to claim 1, it is characterised in that the three-dimensional Each tortuous unit meandering manner of tortuous receiving plane is triangle, trapezoidal or waveform；Triangle rolls over high h=5-40mm, folding Wide w=hcot α, α=5-45 ° of knuckle；The trapezoidal high h=5-40mm of folding, rolls over wide w=hcot α+b, and it is 2-20mm to roll over away from b, folding α=5-45 ° of angle；Waveform rolls over high h=5-40mm, rolls over wide w=5-40mm, α=5-45 ° of knuckle；Each tortuous unit is one group, It is 3-20 that number is organized in electrospinning unit, and the syringe needle on each group is using the row of left, center, right three as a line, every group of line number 1-50.
7. the electrospinning process of three dimensional tortuous nano fibrous membrane according to claim 1, it is characterised in that the polymerization In thing spinning solution, polymer is FEP fluorinated ethylene propylene copolymer, perfluoroethylene-propylene, polypropylene, soluble poly tetrafluoroethene, poly- Vinylidene, polyvinyl butyral resin, polystyrene, polyester, polyvinyl acetate, nylon 6, polyvinyl alcohol, polymethylacrylic acid Methyl esters, polyaniline, polyethylene glycol oxide, polyvinylpyrrolidone, polyacrylonitrile, polycaprolactone, polytetrafluoroethylene (PTFE), polyethylene glycol, Polyurethane, polysulfones, polyether sulfone, Kynoar-hexafluoropropene, Kynoar-tetrafluoroethylene-perfluoro methyl vinyl ether or One or more of Kynoar-CTFE；
Solvent be formic acid, tetrahydrofuran, water, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, acetone, chloroform, cresols, Dimethyl sulfoxide (DMSO), methanol, ethanol, propyl alcohol, isopropanol, butanol, isobutanol, toluene, 1-METHYLPYRROLIDONE, MEK or methyl One or more of ethyl ketone.
8. a kind of three dimensional tortuous nano fibrous membrane made from the method according to claim any one of 1-7, it is characterized in that：Heap Product density is 0.006-0.1g/cm3, high h=5-40mm, α=5-45 ° of knuckle are rolled over, meander-shaped is triangle, trapezoidal or wave Shape；Fiber film-strength is 0.1-10MPa, and the filter efficiency to 0.006-10 μm of particle of particle diameter is 10-50%, and resistance pressure drop exists Below 15Pa.
9. a kind of three dimensional tortuous nano-fiber composite film, its feature made from the method according to claim any one of 1-7 It is：The three dimensional tortuous nano-fiber composite film, macroscopically in the nano fibrous membrane of three dimensional tortuous shape, in a thickness direction in fluffy Pine-bonding is intervally arranged, and the three dimensional tortuous shape nano fibrous membrane loft layer bulk density is 0.006-0.084g/cm3, it is described Three dimensional tortuous shape nano fibrous membrane tack coat bulk density is 0.01-0.1g/cm3；Tunica fibrosa folding high h=5-40mm, knuckle α= 5-45 °, meander-shaped is triangle, trapezoidal or waveform；Fiber film-strength is 5-100MPa, to 0.006-10 μm of particle of particle diameter Filter efficiency >=80%, resistance pressure drop is in below 25Pa.
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