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CN108452690A - The preparation method of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane - Google Patents

The preparation method of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane Download PDF

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CN108452690A
CN108452690A CN201810156617.0A CN201810156617A CN108452690A CN 108452690 A CN108452690 A CN 108452690A CN 201810156617 A CN201810156617 A CN 201810156617A CN 108452690 A CN108452690 A CN 108452690A
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solution
layers
nanofibers
mass percent
spinning
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符思敏
费辉
王龙
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
    • B01D71/68—Polysulfones; Polyethersulfones
    • 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
    • B01D67/0079—Manufacture of membranes comprising organic and inorganic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • B01D71/34—Polyvinylidene fluoride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • B01D71/36—Polytetrafluoroethene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/44—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of groups B01D71/26-B01D71/42
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/48—Polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
    • B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
    • 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
    • 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
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a kind of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane and preparation methods.Multilayered structure Electrospun nano-fibers composite membrane, is combined by base material, layers of nanofibers and protection materials, wherein layers of nanofibers is made of three layers of nanofiber.The present invention discloses the preparation methods of multilayered structure Electrospun nano-fibers composite membrane, spinning formula of liquid and spinning technique are improved, overcome the shortcomings of the prior art and product, pass through the method for wire-type of electrode electrostatic spinning, simply, efficiently preparation filter efficiency is high, resistance pressure drop is low, satisfactory mechanical property air filtration product, has larger application and industrialization value.

Description

The preparation method of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane
Invention field
The present invention relates to functional nano fibrous material field more particularly to a kind of efficient low-resistance multilayered structure electrostatic spinnings The preparation method of nano-fiber composite film.
Background technology
With the development of science and technology air filter is using very extensive, such as microelectronics, optomagnetic technology, bioengineering, electronics The new high-tech industries such as instrument, precision instrument, aerospace, food industry, cosmetics industry, pharmaceuticals industry, certainly with enterprise The audit increasingly strict to clean place of the needs of body, government, the implementation of medicine company new edition GMP, food-safe attention, these The clean engineering demand of industry can further expand, and keep toilet market more diversified, while unclean air is to people Health cause huge threat, therefore, either industry or it is civilian on, be required for having efficiently, low-resistance etc. The air filter of advantage.Traditional air filting material, such as glass fibre, meltblown fibers, spun-bonded fibre, production technology at Ripe, the advantages that strainability is excellent, occuping market leading position.But traditional fibre material causes performance in the presence of scarce because being relatively large in diameter It falls into, material grammes per square metre promotion filter efficiency is handled or increased often through electret, correspondingly resistance pressure drop is made to remain high, used Energy consumption is significantly increased and brings security risk in the process, while limiting the application of its under specific condition (such as high temperature and humidity). Preparing diameter by electrostatic spinning technique, nanofiber has obtained a large amount of research smaller, but fails have preferable practicality always Property, that there are bulk densities is high, mechanical property is poor, and material molding effect is bad that (such as filter efficiency is relatively low, layers of nanofibers is easy Damage) the shortcomings of.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of efficient low-resistance multilayered structure electrostatic spinning nano The preparation method of composite fiber membrane is promoting nanometer by introducing multi-walled carbon nanotube and different classes of high molecular polymer While Fibrous membrane filtration performance, enhance its mechanical property.And using the method for wire-type of electrode electrostatic spinning, prepare multilayered structure Base material, layers of nanofibers and protection materials are combined into a kind of novel filtering material by Electrospun nano-fibers composite membrane, Simply, efficiently, and the product filter efficiency that is prepared is high, resistance pressure drop is low, satisfactory mechanical property, have larger application and Industrialization value.
A kind of preparation method of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane, preparation process are as follows：
1) dry high molecular polymer 1 is added in solvent A, in 80 DEG C of uniform stirrings under confined conditions, keeps it fully molten Solution, solution are in colourless transparent liquid, obtain 1 solution of high molecular polymer that mass percent concentration is 10%~25%；
2) it by the dispersion liquid of dry high molecular polymer 1 and the modified MWCNTs in surface, is added sequentially in solvent B, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, obtain MWCNTs mass percent concentrations be 0.05%~0.3%, it is high 2 solution of MWCNTs/ high molecular polymers that 2 mass percent concentration of Molecularly Imprinted Polymer is 5%~10%；
3) using 1 solution of high molecular polymer obtained in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, One layer of nanofiber is spun on coiled base material, the grammes per square metre of layers of nanofibers is 10~100g/m2, obtain nano fiber basis material A；
4) using 2 solution of MWCNTs/ high molecular polymers obtained in step 2) as spinning solution B, pass through wire-type of electrode electrostatic spinning Method, respin one layer of nanofiber on nano fiber basis material A on the basis of step 3), the grammes per square metre of layers of nanofibers is 10 ~100g/m2, obtain nano fiber basis material B；
5) using 1 solution of high molecular polymer obtained in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, One layer of nanofiber is respinned on nano fiber basis material B on the basis of step 4), the grammes per square metre of layers of nanofibers is 10~100g/ m2, obtain nano fiber basis material C；
6) the nano fiber basis material C that step 5) obtains is bonded with protection materials, and applies 1.5~2.0MPa pressure and carries out hot place Reason, to which efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane be made.
Solvent A in the method is in N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone One kind.
Solvent B in the method is one kind in formic acid, acetonitrile, malononitrile, ethylene carbonate.
High molecular polymer 1 described in step 1) be nylon 6 (PA6), nylon66 fiber (PA66), Kynoar (PVDF), Polyvinyl fluoride (PVF), polytetrafluoroethylene (PTFE) (PTFE), polytrifluorochloroethylene (PCTFE), fluoroethylene-propylene copolymer (FEP), second The mixture of one or both of alkene-TFE copolymer (ETFE).
High molecular polymer 2 described in step 2) is polyacrylonitrile (PAN), polymethyl methacrylate (PMMA), polyphenyl One kind in sulfone (PPSU), polyetherimide (PEI).
The method of the wire-type of electrode electrostatic spinning, spinning process are as follows：The solution configured is placed in solution storage trough It is interior, solution is coated in by opposing stationary wire electrode surface by the module of reciprocating movement, is subsequently placed in high voltage electric field, by The continuous drawing-off splitting of jet stream one by one of the droplet formation of electrostatic force traction, the fiber accumulations eventually formed are in mobile substrate surface Nanofiber mats are obtained, technological parameter is：Base material running rate is 0.2~2.0m/min, and the roller bearing speed of rotation is 6~10rpm, 30~50cm of distance is received, voltage is 50~100KV, and the grammes per square metre of layers of nanofibers is 10~100g/m2。
Step 3) the base material is synthetic fibers filter cotton, non-woven fabrics filter cotton, glass fiber filter cotton, coconut husk charcoal folder carbon One kind in cloth, PET material, to filter efficiency≤15% of 0.3 micron particles object of grain size, resistance pressure drop≤5Pa.
Protection materials described in step 6) are non-woven fabrics, grammes per square metre 5g/m2, the filtering of 0.3 micron particles object of grain size is imitated Rate is 0, resistance pressure drop 0Pa.
The efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane is layer stereo composite construction, including base Material, layers of nanofibers and the protected material bed of material, the layers of nanofibers are made of three layers of nanofiber, and grammes per square metre is respectively 10~ 100g/m2, nano-fiber composite film is to filter efficiency >=99.900% of 0.3 micron particles object of grain size, resistance pressure drop≤50Pa, And tensile strength >=7.3MPa, toughness >=1.70MJ/m3, Young's modulus >=125.0MPa.
Beneficial effects of the present invention：
Novel nano fibrous material is developed, not only can be mutually equal to commercial filtration medium in the market costly, very It is more than these materials to performance, and is exploitation other application field (such as battery diaphragm, biological organization material, acoustic material Deng) nano-fiber material provide new approaches.
Description of the drawings
Fig. 1 is wire-type of electrode electrostatic spinning schematic diagram；
Fig. 2 is the scanning electron microscope spectrogram of the layers of nanofibers of embodiment 2；
Fig. 3 is the scanning electron microscope spectrogram of the layers of nanofibers of embodiment 10.
Specific implementation mode
Invention is further elaborated below in conjunction with drawings and examples.
A kind of preparation process of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane is as follows：
1) dry high molecular polymer 1 is added in solvent A, in 80 DEG C of uniform stirrings under confined conditions, keeps it fully molten Solution, solution are in colourless transparent liquid, obtain 1 solution of high molecular polymer that mass percent concentration is 10%~25%；
2) it by the dispersion liquid of dry high molecular polymer 1 and the modified MWCNTs in surface, is added sequentially in solvent B, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, obtain MWCNTs mass percent concentrations be 0.05%~0.3%, it is high 2 solution of MWCNTs/ high molecular polymers that 2 mass percent concentration of Molecularly Imprinted Polymer is 5%~10%；
3) using 1 solution of high molecular polymer obtained in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, One layer of nanofiber is spun on coiled base material, the grammes per square metre of layers of nanofibers is 10~100g/m2, obtain nano fiber basis material A；
4) using 2 solution of MWCNTs/ high molecular polymers obtained in step 2) as spinning solution B, pass through wire-type of electrode electrostatic spinning Method, respin one layer of nanofiber on nano fiber basis material A on the basis of step 3), the grammes per square metre of layers of nanofibers is 10 ~100g/m2, obtain nano fiber basis material B；
5) using 1 solution of high molecular polymer obtained in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, One layer of nanofiber is respinned on nano fiber basis material B on the basis of step 4), the grammes per square metre of layers of nanofibers is 10~100g/ m2, obtain nano fiber basis material C；
6) the nano fiber basis material C that step 5) obtains is bonded with protection materials, and applies 1.5~2.0MPa pressure and carries out hot place Reason, to which efficient low-resistance layer stereo structure Electrospun nano-fibers composite membrane be made.
Solvent A in the method is in N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone One kind.Solvent B in the method is one kind in formic acid, acetonitrile, malononitrile, ethylene carbonate.It is high described in step 1) Molecularly Imprinted Polymer 1 is nylon 6 (PA6), nylon -66 (PA66), Kynoar (PVDF), polyvinyl fluoride (PVF), polytetrafluoroethyl-ne Alkene (PTFE), polytrifluorochloroethylene (PCTFE), fluoroethylene-propylene copolymer (FEP), ethylene-tetrafluoroethylene copolymer (ETFE) One or both of mixture.High molecular polymer 2 described in step 2) is polyacrylonitrile (PAN), polymethylacrylic acid One kind in methyl esters (PMMA), polyphenylsulfone (PPSU), polyetherimide (PEI).The method of the wire-type of electrode electrostatic spinning, Spinning process is as follows：The solution configured is placed in solution storage trough, is coated in solution relatively by the module of reciprocating movement Static wire electrode surface, is subsequently placed in high voltage electric field, and jet stream is constantly led the droplet formation drawn by electrostatic force one by one Splitting is stretched, the fiber accumulations eventually formed obtain nanofiber mats in mobile substrate surface, and technological parameter is：Base material running speed Rate is 0.2~2.0m/min, and the roller bearing speed of rotation is 6~10rpm, receives 30~50cm of distance, and voltage is 50~100KV, is received The grammes per square metre of rice fibrous layer is 10~100g/m2, Fig. 1 is wire-type of electrode electrostatic spinning schematic diagram.Step 3) the base material is synthesis One kind in fiber filter cotton, non-woven fabrics filter cotton, glass fiber filter cotton, coconut husk charcoal folder carbon cloth, PET material, to grain size 0.3 Filter efficiency≤15% of micron particles object, resistance pressure drop≤5Pa.Protection materials described in step 6) are non-woven fabrics, and grammes per square metre is 5g/m2, the filter efficiency to 0.3 micron particles object of grain size is 0, resistance pressure drop 0Pa.The efficient low-resistance multilayered structure electrostatic Spinning nano-fiber composite film is layer stereo composite construction, including base material, layers of nanofibers and the protected material bed of material, the nanometer Fibrous layer is made of three layers of nanofiber, and grammes per square metre is respectively 10~100g/m2, nano-fiber composite film is to grain size 0.3 micron Filter efficiency >=99.900% of grain object, resistance pressure drop≤50Pa and tensile strength >=7.3MPa, toughness >=1.70MJ/m3、 Young's modulus >=125.0MPa.
(the mass ratio 1 of embodiment 1:4 nylon 6, Kynoar are configured to the spinning solution A of mass percent concentration 10%, The grammes per square metre of finally obtained PET material composite membrane, layers of nanofibers is respectively 10g/m2、50g/m2、20g/m2)
1) it is 1 by mass ratio:After 4 nylon 6, Kynoar drying, it is added sequentially in n,N-Dimethylformamide, at 80 DEG C Uniform stirring under confined conditions makes it fully dissolve, and solution is in colourless transparent liquid, and it is 10% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 5% for 0.05%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 10g/m2, base material running rate is 2.0m/min, roller bearing rotation Rotational speed rate is 6rpm, receives distance 50cm, voltage 75KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 1.2m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 70KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 10g/m2, base material running rate is 2.0m/min, roller bearing rotation speed Rate is 6rpm, receives distance 50cm, voltage 75KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 2.0MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.900% to the filter efficiency of 0.3 micron particles object of grain size, and resistance pressure drop is 25Pa and tensile strength be 7.3MPa, toughness 1.70MJ/m3, Young's modulus 125.0MPa.
(the mass ratio 1 of embodiment 2:2 nylon 6, Kynoar are configured to the spinning solution A of mass percent concentration 15%, The grammes per square metre of finally obtained PET material composite membrane, layers of nanofibers is respectively 20g/m2、50g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon 6, Kynoar drying, it is added sequentially in n,N-Dimethylformamide, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, and solution is in colourless transparent liquid, and it is 15% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 5% for 0.05%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation Rotational speed rate is 8rpm, receives distance 45cm, voltage 78KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 1.2m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 70KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 8rpm, receives distance 45cm, voltage 78KV, Fig. 2 are the scanning electron microscope spectrograms of the layers of nanofibers of embodiment 2；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 2.0MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.900% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 35Pa and tensile strength be 7.4MPa, toughness 1.75MJ/m3, Young's modulus 128.0MPa.
(the mass ratio 1 of embodiment 3:3 nylon 6, Kynoar are configured to the spinning solution A of mass percent concentration 20%, MWCNTs mass percent concentrations are 0.15%, polyacrylonitrile mass percent concentration is 10% spinning solution B, it is finally obtained The grammes per square metre of PET material composite membrane, layers of nanofibers is respectively 20g/m2、50g/m2、20g/m2)
1) it is 1 by mass ratio:After 3 nylon 6, Kynoar drying, it is added sequentially in n,N-dimethylacetamide, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, and solution is in colourless transparent liquid, and it is 20% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.15%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.4m/min, roller bearing rotation Rotational speed rate is 9rpm, receives distance 40cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 1.2m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 80KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.7m/min, roller bearing rotation speed Rate is 9rpm, receives distance 40cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 2.0MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.940% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 32Pa and tensile strength be 7.6MPa, toughness 1.79MJ/m3, Young's modulus 130.0MPa.
(the mass ratio 2 of embodiment 4:3 nylon 6, Kynoar are configured to the spinning solution A of mass percent concentration 25%, MWCNTs mass percent concentrations are 0.15%, polyacrylonitrile mass percent concentration is 10% spinning solution B, it is finally obtained The grammes per square metre of PET material composite membrane, layers of nanofibers is respectively 20g/m2、50g/m2、20g/m2)
1) it is 2 by mass ratio:After 3 nylon 6, Kynoar drying, it is added sequentially in n,N-dimethylacetamide, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, and solution is in colourless transparent liquid, and it is 25% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.15%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.1m/min, roller bearing rotation Rotational speed rate is 10rpm, receives distance 50cm, voltage 90KV；4) using the solution in step 2) as spinning solution B, pass through line style electricity The method of pole electrostatic spinning, then one layer of nanofiber is spun on the basis of step 3), the grammes per square metre of layers of nanofibers is 50g/m2, base Material exploitation speed is 1.2m/min, and the roller bearing speed of rotation is 8rpm, receives distance 35cm, voltage 80KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.1m/min, roller bearing rotation speed Rate is 10rpm, receives distance 50cm, voltage 90KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 2.0MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.910% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 35Pa and tensile strength be 7.8MPa, toughness 1.77MJ/m3, Young's modulus 131.0MPa.
(the mass ratio 1 of embodiment 5:2 nylon 6, Kynoar are configured to the spinning solution A of mass percent concentration 15%, MWCNTs mass percent concentrations are 0.15%, polyacrylonitrile mass percent concentration is 10% spinning solution B, it is finally obtained The grammes per square metre of PET material composite membrane, layers of nanofibers is respectively 20g/m2、50g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon 6, Kynoar drying, it is added sequentially in n,N-Dimethylformamide, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, and solution is in colourless transparent liquid, and it is 15% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, obtain MWCNTs it is a concentration of 0.15%, The solution of polyacrylonitrile a concentration of 10%.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation Rotational speed rate is 8rpm, receives distance 45cm, voltage 78KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 1.0m/min, and the roller bearing speed of rotation is 7rpm receives distance 40cm, voltage 80KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 8rpm, receives distance 45cm, voltage 78KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 2.0MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.950% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 32Pa and tensile strength be 7.4MPa, toughness 1.75MJ/m3, Young's modulus 128.0MPa.
(the mass ratio 1 of embodiment 6:2 nylon 6, Kynoar are configured to the spinning solution A of mass percent concentration 15%, MWCNTs mass percent concentrations are 0.25%, polyacrylonitrile mass percent concentration is 10% spinning solution B, it is finally obtained The grammes per square metre of PET material composite membrane, layers of nanofibers is respectively 20g/m2、50g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon 6, polyvinyl fluoride drying, it is added sequentially in n,N-dimethylacetamide, at 80 DEG C Uniform stirring under confined conditions makes it fully dissolve, and solution is in colourless transparent liquid, and it is 15% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.25%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation Rotational speed rate is 7rpm, receives distance 40cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 1.2m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 75KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 7rpm, receives distance 40cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.96% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 30Pa and tensile strength be 7.7MPa, toughness 1.81MJ/m3, Young's modulus 128.0MPa.
(the mass ratio 1 of embodiment 7:2 nylon 6, polytetrafluoroethylene (PTFE) are configured to the spinning solution A of mass percent concentration 15%, MWCNTs mass percent concentrations are 0.25%, polyacrylonitrile mass percent concentration is 10% spinning solution B, it is finally obtained The grammes per square metre of PET material composite membrane, layers of nanofibers is respectively 20g/m2、60g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon 6, polytetrafluoroethylene (PTFE) drying, it is added sequentially in n,N-dimethylacetamide, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, and solution is in colourless transparent liquid, and it is 15% to obtain mass percent concentration Solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.25%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation Rotational speed rate is 9rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 60g/m2, base material running rate is 1.0m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 75KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 7rpm, receives distance 40cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.96% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 28Pa and tensile strength be 7.7MPa, toughness 1.81MJ/m3, Young's modulus 128.0MPa.
(the mass ratio 1 of embodiment 8:2 nylon66 fibers, polytrifluorochloroethylene are configured to the spinning of mass percent concentration 15% Liquid A, MWCNTs mass percent concentration is 0.25%, polyacrylonitrile mass percent concentration is 10% spinning solution B, final The grammes per square metre of the PET material composite membrane arrived, layers of nanofibers is respectively 20g/m2、60g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon66 fiber, polytrifluorochloroethylene drying, it is added sequentially in n,N-dimethylacetamide, In 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, and obtaining mass percent concentration is 15% solution.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.25%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.5m/min, roller bearing rotation Rotational speed rate is 6rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 60g/m2, base material running rate is 1.0m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 75KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.5m/min, roller bearing rotation speed Rate is 6rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.97% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 29Pa and tensile strength be 8.0MPa, toughness 1.81MJ/m3, Young's modulus 128.0MPa.
(the mass ratio 1 of embodiment 9:2 nylon66 fiber, fluoroethylene-propylene copolymer are configured to mass percent concentration 15% Spinning solution A, MWCNTs mass percent concentration be 0.25%, the spinning solution B that polyacrylonitrile mass percent concentration is 10%, The grammes per square metre of finally obtained PET material composite membrane, layers of nanofibers is respectively 20g/m2、60g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon66 fiber, the drying of fluoroethylene-propylene copolymer, it is added sequentially to n,N-dimethylacetamide In, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, and it is dense to obtain mass percent The solution that degree is 15%.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.25%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.5m/min, roller bearing rotation Rotational speed rate is 7rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 60g/m2, base material running rate is 1.0m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 75KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.5m/min, roller bearing rotation speed Rate is 7rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.96% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 38Pa and tensile strength be 8.2MPa, toughness 1.81MJ/m3, Young's modulus 133.0MPa.
(the mass ratio 1 of embodiment 10:2 nylon66 fiber, ethylene-tetrafluoroethylene copolymer are configured to mass percent concentration 15% spinning solution A, MWCNTs mass percent concentration is 0.25%, the spinning that polyacrylonitrile mass percent concentration is 10% Liquid B, the grammes per square metre of finally obtained PET material composite membrane, layers of nanofibers is respectively 20g/m2、60g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon66 fiber, ethylene-tetrafluoroethylene copolymer drying, it is added sequentially to N, N- dimethyl second In amide, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, obtains quality percentage The solution that specific concentration is 15%.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.25%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.5m/min, roller bearing rotation Rotational speed rate is 7rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 60g/m2, base material running rate is 1.0m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 75KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.5m/min, roller bearing rotation speed Rate is 7rpm, receives distance 35cm, voltage 80KV, Fig. 3 are the scanning electron microscope spectrograms of the layers of nanofibers of embodiment 10；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.94% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 34Pa and tensile strength be 8.0MPa, toughness 1.84MJ/m3, Young's modulus 130.0MPa.
(the mass ratio 1 of embodiment 11:2 nylon 6, polyvinyl fluoride are configured to the spinning solution of mass percent concentration 15% The spinning solution B that A, MWCNTs mass percent concentration are 0.3%, polymethyl methacrylate mass percent concentration is 10%, The grammes per square metre of finally obtained PET material composite membrane, layers of nanofibers is respectively 20g/m2、40g/m2、20g/m2)
1) it is 1 by mass ratio:After 2 nylon 6, polyvinyl fluoride drying, it is added sequentially in n,N-dimethylacetamide, at 80 DEG C Uniform stirring under confined conditions makes it fully dissolve, and solution is in colourless transparent liquid, and it is 15% to obtain mass percent concentration Solution.
2) after polymethyl methacrylate being dried, the modified MWCNTs's in surface for being 1% with mass percent concentration Dispersion liquid is added sequentially in acetonitrile, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, is obtained MWCNTs mass The solution that percent concentration is 0.3%, polymethyl methacrylate mass percent concentration is 10%.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled PET materials Expect to spin one layer of nanofiber on base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation Rotational speed rate is 7rpm, receives distance 40cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 40g/m2, base material running rate is 1.0m/min, and the roller bearing speed of rotation is 8rpm receives distance 35cm, voltage 90KV；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 7rpm, receives distance 40cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.92% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 28Pa and tensile strength be 7.3MPa, toughness 1.77MJ/m3, Young's modulus 126.0MPa.
(nylon 6 is configured to spinning solution A, the MWCNTs mass percent concentration of mass percent concentration 15% to embodiment 12 The spinning solution B for being 10% for 0.3%, polyphenylsulfone mass percent concentration, finally obtained synthetic fibers filter cotton composite membrane are received The grammes per square metre of rice fibrous layer is respectively 20g/m2、100g/m2、20g/m2) 1) by after the drying of nylon 6, it is added sequentially to N- methylpyrroles In alkanone, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, obtains quality percentage The solution that specific concentration is 15%.
2) after polyphenylsulfone being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, successively It is added in malononitrile, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.3%, polyphenylsulfone mass percent concentration.
3) fine in coiled synthesis by the method for wire-type of electrode electrostatic spinning using the solution in step 1) as spinning solution A One layer of nanofiber is spun on dimensional filter cotton base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, The roller bearing speed of rotation is 8rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 100g/m2, base material running rate is 0.2m/min, the roller bearing speed of rotation For 8rpm, distance 40cm, voltage 90KV are received；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 8rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.99% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 40Pa and tensile strength be 7.3MPa, toughness 1.80MJ/m3, Young's modulus 127.0MPa.
(nylon 6 is configured to spinning solution A, the MWCNTs mass percent concentration of mass percent concentration 15% to embodiment 13 The spinning solution B for being 10% for 0.3%, polyetherimide mass percent concentration, finally obtained non-woven fabrics filter cotton composite membrane, The grammes per square metre of layers of nanofibers is respectively 20g/m2、100g/m2、20g/m2) 1) by after the drying of nylon 6, it is added sequentially to N- methyl pyrroles In pyrrolidone, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, obtains quality hundred It is 15% solution to divide specific concentration.
2) after polyetherimide being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, It is added sequentially in ethylene carbonate, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass hundred Divide the solution that specific concentration is 0.3%, polyetherimide mass percent concentration is 10%.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled non-woven fabrics One layer of nanofiber is spun on filter cotton base material, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, rolling Rotating rate of shaft is 8rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 100g/m2, base material running rate is 0.4m/min, the roller bearing speed of rotation For 8rpm, distance 40cm, voltage 100KV are received；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 20g/m2, base material running rate is 1.8m/min, roller bearing rotation speed Rate is 8rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.98% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 42Pa and tensile strength be 7.4MPa, toughness 1.85MJ/m3, Young's modulus 128.0MPa.
(Kynoar is configured to spinning solution A, the MWCNTs mass percent of mass percent concentration 15% to embodiment 14 A concentration of 0.3%, the spinning solution B that polyacrylonitrile mass percent concentration is 10%, finally obtained PET material composite membrane are received The grammes per square metre of rice fibrous layer is respectively 10g/m2、100g/m2、10g/m2)
1) it after drying Kynoar, is added sequentially in N-Methyl pyrrolidone, in 80 DEG C of uniform stirrings under confined conditions, It is set fully to dissolve, solution is in colourless transparent liquid, obtains the solution that mass percent concentration is 15%.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.3%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled glass fibers One layer of nanofiber is spun on dimensional filter cotton base material, the grammes per square metre of layers of nanofibers is 10g/m2, base material running rate is 2.0m/min, The roller bearing speed of rotation is 8rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 100g/m2, base material running rate is 0.4m/min, the roller bearing speed of rotation For 8rpm, distance 40cm, voltage 100KV are received；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 10g/m2, base material running rate is 2.0m/min, roller bearing rotation speed Rate is 8rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.97% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 31Pa and tensile strength be 7.4MPa, toughness 1.85MJ/m3, Young's modulus 130.0MPa.
(Kynoar is configured to spinning solution A, the MWCNTs mass percent of mass percent concentration 15% to embodiment 15 A concentration of 0.3%, the spinning solution B that polyacrylonitrile mass percent concentration is 10%, finally obtained glass fiber filter cotton are multiple Film is closed, the grammes per square metre of layers of nanofibers is respectively 10g/m2、100g/m2、10g/m2) 1) Kynoar is dried after, sequentially add Into N-Methyl pyrrolidone, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, Obtain the solution that mass percent concentration is 15%.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, it is a concentration of 0.3%, poly- to obtain MWCNTs The solution that acrylonitrile concentration is 10%.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled glass fibers One layer of nanofiber is spun on dimensional filter cotton base material, the grammes per square metre of layers of nanofibers is 10g/m2, base material running rate is 2.0m/min, The roller bearing speed of rotation is 8rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 100g/m2, base material running rate is 0.4m/min, the roller bearing speed of rotation For 8rpm, distance 40cm, voltage 100KV are received；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 10g/m2, base material running rate is 2.0m/min, roller bearing rotation speed Rate is 8rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.97% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 31Pa and tensile strength be 7.4MPa, toughness 1.85MJ/m3, Young's modulus 130.0MPa.
(nylon 6 is configured to spinning solution A, the MWCNTs mass percent concentration of mass percent concentration 15% to embodiment 16 The spinning solution B for being 10% for 0.3%, polyacrylonitrile mass percent concentration, finally obtained glass fiber filter cotton composite membrane, The grammes per square metre of layers of nanofibers is respectively 50g/m2、100g/m2、50g/m2) 1) by after the drying of nylon 6, it is added sequentially to N- methyl pyrroles In pyrrolidone, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, obtains quality hundred It is 15% solution to divide specific concentration.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.3%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled glass fibers One layer of nanofiber is spun on dimensional filter cotton base material, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 0.6m/min, The roller bearing speed of rotation is 8rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 100g/m2, base material running rate is 0.4m/min, the roller bearing speed of rotation For 8rpm, distance 40cm, voltage 100KV are received；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 50g/m2, base material running rate is 0.6m/min, roller bearing rotation speed Rate is 8rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 1.5MPa pressure on the outside, made At efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.99% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 50Pa and tensile strength be 7.9MPa, toughness 1.86MJ/m3, Young's modulus 140.0MPa.
(nylon66 fiber is configured to spinning solution A, the MWCNTs mass percent concentration of mass percent concentration 15% to embodiment 17 The spinning solution B for being 10% for 0.3%, polyacrylonitrile mass percent concentration, finally obtained coconut husk charcoal are pressed from both sides carbon cloth composite membrane, are received The grammes per square metre of rice fibrous layer is respectively 40g/m2、100g/m2、40g/m2) 1) nylon66 fiber is dried after, be added sequentially to N- methyl pyrroles In pyrrolidone, in 80 DEG C of uniform stirrings under confined conditions, it is made fully to dissolve, solution is in colourless transparent liquid, obtains quality hundred It is 15% solution to divide specific concentration.
2) after polyacrylonitrile being dried, the dispersion liquid for the modified MWCNTs in surface for being 1% with mass percent concentration, according to It is secondary to be added in formic acid, in 80 DEG C of uniform stirrings under confined conditions, so that it is fully dissolved, obtain MWCNTs mass percent concentrations The solution for being 10% for 0.3%, polyacrylonitrile mass percent concentration.
3) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, in coiled coconut husk charcoal It presss from both sides and spins one layer of nanofiber on carbon cloth base material, the grammes per square metre of layers of nanofibers is 40g/m2, base material running rate is 0.8m/min, rolling Rotating rate of shaft is 8rpm, receives distance 35cm, voltage 80KV；
4) using the solution in step 2) as spinning solution B, by the method for wire-type of electrode electrostatic spinning, then on the basis of step 3) One layer of nanofiber is spun, the grammes per square metre of layers of nanofibers is 100g/m2, base material running rate is 0.4m/min, the roller bearing speed of rotation For 8rpm, distance 40cm, voltage 100KV are received；
5) using the solution in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, continue in the basis of step 4) On respin one layer of nanofiber, the grammes per square metre of layers of nanofibers is 40g/m2, base material running rate is 0.8m/min, roller bearing rotation speed Rate is 8rpm, receives distance 35cm, voltage 80KV；
6) material made from step 5) is bonded with protection materials, and applies be heat-treated under 2MPa pressure on the outside, be made Efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane.
Gained nano-fiber composite film is 99.98% to the filter efficiency of 0.3 micron particles object of grain size, resistance pressure drop 45Pa and tensile strength be 7.7MPa, toughness 1.83MJ/m3, Young's modulus 142.0MPa.

Claims (9)

1. a kind of preparation method of efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane, it is characterised in that its preparation Steps are as follows：
1) dry high molecular polymer 1 is added in solvent A, in 80 DEG C of uniform stirrings under confined conditions, keeps it fully molten Solution, solution are in colourless transparent liquid, obtain 1 solution of high molecular polymer that mass percent concentration is 10%~25%；
2) it by the dispersion liquid of dry high molecular polymer 1 and the modified MWCNTs in surface, is added sequentially in solvent B, 80 DEG C under confined conditions uniform stirring, makes it fully dissolve, obtain MWCNTs mass percent concentrations be 0.05%~0.3%, it is high 2 solution of MWCNTs/ high molecular polymers that 2 mass percent concentration of Molecularly Imprinted Polymer is 5%~10%；
3) using 1 solution of high molecular polymer obtained in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, One layer of nanofiber is spun on coiled base material, the grammes per square metre of layers of nanofibers is 10~100g/m2, obtain nano fiber basis material A；
4) using 2 solution of MWCNTs/ high molecular polymers obtained in step 2) as spinning solution B, pass through wire-type of electrode electrostatic spinning Method, respin one layer of nanofiber on nano fiber basis material A on the basis of step 3), the grammes per square metre of layers of nanofibers is 10 ~100g/m2, obtain nano fiber basis material B；
5) using 1 solution of high molecular polymer obtained in step 1) as spinning solution A, by the method for wire-type of electrode electrostatic spinning, One layer of nanofiber is respinned on nano fiber basis material B on the basis of step 4), the grammes per square metre of layers of nanofibers is 10~100g/ m2, obtain nano fiber basis material C；
6) the nano fiber basis material C that step 5) obtains is bonded with protection materials, and applies 1.5~2.0MPa pressure and carries out hot place Reason, to which efficient low-resistance multilayered structure Electrospun nano-fibers composite membrane be made.
2. according to the method described in claim 1, it is characterized in that, solvent A in the method be n,N-Dimethylformamide, One kind in DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone.
3. according to the method described in claim 1, it is characterized in that, solvent B in the method be formic acid, acetonitrile, malononitrile, One kind in ethylene carbonate.
4. according to the method described in claim 1, it is characterized in that, high molecular polymer 1 described in step 1) is nylon 6 (PA6), nylon -66 (PA66), Kynoar (PVDF), polyvinyl fluoride (PVF), polytetrafluoroethylene (PTFE) (PTFE), poly- trifluoro chlorine One or both of ethylene (PCTFE), fluoroethylene-propylene copolymer (FEP), ethylene-tetrafluoroethylene copolymer (ETFE) mix Close object.
5. according to the method described in claim 1, it is characterized in that, high molecular polymer 2 described in step 2) is polyacrylonitrile (PAN), one kind in polymethyl methacrylate (PMMA), polyphenylsulfone (PPSU), polyetherimide (PEI).
6. according to the method described in claim 1, it is characterized in that, the method for the wire-type of electrode electrostatic spinning, spinning Journey is as follows：The solution configured is placed in solution storage trough, by the module of reciprocating movement by solution coated in opposing stationary Wire electrode surface, is subsequently placed in high voltage electric field, and the continuous drawing-off of jet stream cleaves the droplet formation drawn by electrostatic force one by one, The fiber accumulations eventually formed obtain nanofiber mats in mobile substrate surface, and technological parameter is：Base material running rate is 0.2 ~2.0m/min, the roller bearing speed of rotation are 6~10rpm, receive 30~50cm of distance, and voltage is 50~100KV, layers of nanofibers Grammes per square metre be 10~100g/m2。
7. according to the method described in claim 1, it is characterized in that, the step 3) base material is synthetic fibers filter cotton, nonwoven One kind in cloth filter cotton, glass fiber filter cotton, coconut husk charcoal folder carbon cloth, PET material, to the mistake of 0.3 micron particles object of grain size Filter efficiency≤15%, resistance pressure drop≤5Pa.
8. according to the method described in claim 1, it is characterized in that, protection materials described in step 6) are non-woven fabrics, grammes per square metre is 5g/m2, the filter efficiency to 0.3 micron particles object of grain size is 0, resistance pressure drop 0Pa.
9. according to the method described in claim 1, it is characterized in that, the efficient low-resistance multilayered structure Electrospun nano-fibers Composite membrane is layer stereo composite construction, including base material, layers of nanofibers and the protected material bed of material, and the layers of nanofibers is by three layers Nanofiber is constituted, and grammes per square metre is respectively 10~100g/m2, filtering effect of the nano-fiber composite film to 0.3 micron particles object of grain size Rate >=99.900%, resistance pressure drop≤50Pa and tensile strength >=7.3MPa, toughness >=1.70MJ/m3, Young's modulus >= 125.0MPa。
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