CN106237717B - A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method - Google Patents

A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method Download PDF

Info

Publication number
CN106237717B
CN106237717B CN201610784058.9A CN201610784058A CN106237717B CN 106237717 B CN106237717 B CN 106237717B CN 201610784058 A CN201610784058 A CN 201610784058A CN 106237717 B CN106237717 B CN 106237717B
Authority
CN
China
Prior art keywords
electrostatic spinning
nano fiber
nanofiber
electrostatic
woven
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201610784058.9A
Other languages
Chinese (zh)
Other versions
CN106237717A (en
Inventor
覃小红
高涵超
高婧
杨雨琼
张弘楠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Donghua University
Original Assignee
Donghua University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Donghua University filed Critical Donghua University
Priority to CN201610784058.9A priority Critical patent/CN106237717B/en
Publication of CN106237717A publication Critical patent/CN106237717A/en
Application granted granted Critical
Publication of CN106237717B publication Critical patent/CN106237717B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/16Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1623Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/16Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1638Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being particulate
    • B01D39/1653Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being particulate of synthetic origin
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-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
    • D04H1/72Non-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
    • D04H1/728Non-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

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)
  • Filtering Materials (AREA)

Abstract

The present invention relates to a kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method, the filtering material is spun-bonded non-woven and the spaced sandwich of nanofiber;Using needle-free electrostatic spinning nozzle, then pass through electrostatic spinning combined technology synchronous with electrostatic spray, nanofiber/microballoon composite membrane is made, using rotating cylinder as reception device, spun-bonded non-woven is to receive substrate, obtains nanofiber/non-weaving cloth composite material, then one layer of spun-bonded non-woven of surface cover, form spun-bonded non-woven and the spaced sandwich of nanofiber, then adhesion process to get.Preparation process of the present invention is simple, controllable and reproducible, and air filting material obtained has the characteristics that efficient low-resistance, and thickness is uniform, strainability it is stable, it can be achieved that nanofiber filtration material mass production, have extraordinary application prospect in field of air filtration.

Description

A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation Method
Technical field
The invention belongs to air filting material and its preparation field, in particular to a kind of efficient low-resistance electrostatic spinning nano fiber Air filting material and mass preparation method.
Background technique
As China's process of industrialization is deeply also got worse with rapid economic development, air pollution problems inherent, especially closely PM2.5 (particle of the partial size less than the 2.5 μm) pollution that the China Nian Lai various regions persistently occur, causes the health of people It seriously threatens.Filtering is used as a kind of safeguard procedures, can effectively resist the adverse effect that pollution is brought.Currently, China Industry largely use the air filting material based on glass fibre or melt-blow nonwoven, to size in the micron-scale more than Particulate matter there is preferable filter effect, but it is poor to sub-micron even nano-scale particle filter efficiency, and existed The problems such as filtration resistance power is big, dust containing capacity is small, service life is short, therefore, urgent need develop a kind of high-efficient low-resistance air filting material.
Electrostatic spinning nano fiber has many advantages, such as that fibre diameter is small, aperture is small, large specific surface area, porosity are high, by its with Ideal air filting material can be prepared after combining in substrate.But since electrostatic spinning fiber diameter is in submicron-scale, in reality Usually with higher filtration resistance while now efficient, existing literature in spinning solution mainly by being added inorganic nano Grain prepares porous fibre, realizes efficient low-resistance to three kinds of modes of nano fibrous membrane electret.(1) inorganic receive is added in spinning solution Rice grain makes tunica fibrosa have multistage surface roughness, increases specific surface area, at the same fibre section be it is non-circular, efficient Filtration resistance (N.Wang, Y.S.Si, N.Wang, et al.Multilevel structured is reduced simultaneously polyacrylonitrile/silica nanofibrous membranes for high-performance air filtration[J].Separation and Purification Technology,2014,126:44-51.).But it is inorganic Nano particle additive amount is limited, and excessive nano particle is reunited, and the filter efficiency of tunica fibrosa reduces instead, and is using Inorganic nanoparticles can be fallen off in the process, be threatened to health of people.(2) porous fibre, patent are prepared CN103952783A discloses " a kind of the porous PLA nanofiber of a beading and preparation method thereof ", using low boiling point solvent, in spinning In the process, solvent quickly volatilizees, and quickly mutually separation and the solidification of induced jet surface solution forms beading porous fibrous structure, Realize efficient low-resistance.But porous fibrous material mechanical property is poor, while a large amount of low boiling point solvents quickly volatilize in experimentation People's health can be jeopardized.(3) to nano fibrous membrane electret, patent CN104289042A discloses that " a kind of Static Spinning is received Rice fiber electret filtering material and its preparation " passes through control inorganic nanoparticles content, polymer solution temperature and Nanowire Dimension molding instantaneous cooling technique is prepared for nanofiber electret filtering material, but does not provide the material and place rear surface electricity Lotus whether the related data of loss.For electret material in storage and use process, moisture and particle in air can accelerate electret Material surface charge loss, makes electret effect gradually decay, and eventually leads to the decline of filtration of material efficiency.Electrostatic spinning nano fiber material Material low output is always to restrict the technological difficulties of its industrialized production, above method and the unresolved electrostatic spinning nano fiber of patent Filtering material is unable to the problem of mass production.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of efficient low-resistance electrostatic spinning nano fiber air filting materials And mass preparation method, this method simple process, controllable and reproducible, air filting material obtained has efficient low-resistance Feature, thickness is uniform, strainability it is stable, it can be achieved that nanofiber filtration material mass production, in field of air filtration There is extraordinary application prospect.
A kind of efficient low-resistance electrostatic spinning nano fiber air filting material of the invention, the filtering material, which is that spunbond is non-, to be knitted Cloth and the spaced sandwich of nanofiber are made, nanofiber is electrostatic spinning nano fiber/microballoon composite membrane, wherein electrostatic Spinning nano fibre/microballoon structure of composite membrane are as follows: the 3 D stereo cavity structure formed between microballoon insertion electrostatic spinning nano fiber.
The spun-bonded non-woven, fibre diameter are 1-10 μm, grammes per square metre 10-120g/m2, exhibits initial filtration efficiency is 0.1%-5%.
The electrostatic spinning nano fiber diameter is 100-300nm;The partial size of microballoon is 500-800nm.
A kind of efficient low-resistance electrostatic spinning nano fiber air filting material of the invention and mass preparation method, comprising:
(1) polymer is added in solvent, stirring obtains the electrostatic spinning polymer solution of high concentration;Wherein Static Spinning The mass percentage concentration of silk polymer solution is 10-40%;
(2) polymer is added in solvent, stirring obtains the electrostatic spray polymer solution of low concentration;Wherein electrostatic The mass percentage concentration of mist polymer solution is 3-30%;
(3) needle-free electrostatic spinning nozzle is used, electrostatic spinning combined technology synchronous with electrostatic spray, system are then passed through Nanofiber/microballoon composite membrane is obtained, using rotating cylinder as reception device, spun-bonded non-woven is to receive substrate, obtains nanometer Fiber/non-weaving cloth composite material can regulate and control electrostatic spinning nano fiber/microballoon composite membrane grammes per square metre by adjusting the spinning time For 0.1-10g/m2
(4) by above-mentioned nanofiber/one layer of non-weaving cloth composite material surface cover spun-bonded non-woven, form that spunbond is non-to knit Cloth and the spaced sandwich of nanofiber are made, then adhesion process is to get electrostatic spinning nano fiber air filting material.
Polymer is polyacrylonitrile, polyurethane, polysulfones, polyvinylpyrrolidone, gathers inclined fluorine in the step (1), (2) One of ethylene, polyethylene glycol oxide, polystyrene, polymethyl methacrylate, polycaprolactone, polycaprolactam, chitosan Or it is several;Solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, acetone, tetrahydrofuran, two One or more of chloromethanes, chloroform, hexafluoroisopropanol, formic acid, acetic acid, ethyl alcohol.
Stirring is magnetic agitation 10-12h in the step (1), (2).
Insulating materials is used in step (3), by needle-free electrostatic spinning nozzle surface from center punishment for identical faces Long-pending or length the part 2-8, is injected into different piece for electrostatic spinning polymer solution and electrostatic spray polymer solution respectively, Spinning is carried out by electrostatic spinning combined technology synchronous with electrostatic spray.
The insulating materials be polytetrafluoroethylene (PTFE), Kynoar, polymethyl methacrylate, polycarbonate, polyethylene, One of polypropylene, polystyrene.
The specific process parameter of electrostatic spinning combined technology synchronous with electrostatic spray in the step (3) are as follows: spinning electricity Press 40-75KV, drum rotation speed 10-400r/min, distance 10-25cm between spray head and roller, spray head transverse moving speed 10-300cm/ Min, liquid supply speed 20-500mL/h, 20-35 DEG C of environment temperature, ambient humidity 20-80%.
Entire spinning machine is closed, and temperature and humidity measure and device for automatically regulating, spinning nozzle and cross are equipped in confined space Telephone-moving structure is connected, and spinning nozzle is connected with perfusion tube, perfusion tube other end connection liquid feed device, in entire spinning process, feed flow Device is sustainedly and stably to spray head feed flow, it is ensured that spinning is carried out continuously, and realizes the mass production of electrostatic spinning nano fiber material.
Adhesion process is ultrasonic bonds in the step (4), and the bonding mode is small to the destruction of nanofiber, after processing Composite material be still able to maintain efficient low-resistance feature, while the strength of filter material is greatly improved.
The present invention uses needle-free electrostatic spinning nozzle, passes through electrostatic spinning combined technology synchronous with electrostatic spray, wound New property is prepared for electrostatic spinning nano fiber/microballoon composite membrane, and one-step shaping obtains high-efficiency low-resistance nano fiber filter material
Filtering material produced by the present invention has 3 D stereo cavity structure and good structure controllability, filter material Material length is 1.6m, breadth 0.6m, and producing the time used in a filter material is 20-30min, and the filtering material is straight to quantity intermediate value Diameter is the particle filtration efficiency of 75nm up to 99.99%, filtration resistance 50-150Pa, and the method provided through the invention is to receiving After rice fiber membrane structure optimizes, compared with common nanofiber filtration material, under identical filter efficiency, filtration resistance drop Low 35%.
Beneficial effect
(1) present invention is by electrostatic spinning combined technology synchronous with electrostatic spray, and polymer highly concentrated solution is by quiet Diameter is formed after Electrospun in the fiber of 100-300nm, can be used as tunica fibrosa support construction.Polymer low concentration solution is by quiet After electron spray formed diameter 500-800nm microballoon, microballoon be embedded in nanofiber between, increased fiber and it is interfibrous away from From formation 3 D stereo cavity structure reduces filtration resistance, and polymer low concentration solution will form directly while forming microballoon Diameter improves filter efficiency in the superfine nano fiber of 80nm or so while reducing filtration resistance, and one-step shaping obtains efficiently low Hinder nanofiber filtration material;
(2) present invention uses needle-free electrostatic spinning nozzle, avoid multiple single needle electrostatic spinning syringe needles and syringe needle it Between electric field interfere with each other, lead to the problem of fiber film uniformity difference obtained;Preparation method provided by the invention, nanometer obtained Fiber film thickness is uniform, and strainability is stablized, high production efficiency, and preparing a length is 1.6m, and breadth is the nanometer mistake of 0.6m Be only 20-30min the time required to filter material material, it can be achieved that electrostatic spinning nano fiber air filting material mass production;
(3) present invention process parameter is simply controllable, and the nanofiber filtration material of preparation has good structure controllable Property, it can be realized by adjusting the jet-flow proportioning of electrostatic spinning and electrostatic spray polymer solution to fibrous material packing density, hole The accuracy controlling of diameter and porosity;
(4) nanofiber filtration material aperture prepared by the present invention is small, porosity is big, and the presence of microballoon has the material There is 3 D stereo cavity structure, which, which makes it in actual use, has biggish dust containing capacity, extends filtering material Service life, have good actual application prospect.
Detailed description of the invention
Fig. 1 is efficient low-resistance electrostatic spinning nano fiber air filting material preparation flow figure of the present invention;
Fig. 2 is the efficient low-resistance electrostatic spinning nano fiber/microballoon composite membrane SEM Electronic Speculum prepared in the embodiment of the present invention 1 Figure.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Embodiment 1
Filtering material is spun-bonded non-woven and the spaced sandwich of nanofiber, and nanofiber is received for Static Spinning Rice fiber/microballoon composite membrane, wherein electrostatic spinning nano fiber/microballoon structure of composite membrane are as follows: microballoon is embedded in electrostatic spinning nano fiber Between the 3 D stereo cavity structure that is formed;Wherein nanofiber diameter is 139nm;The partial size of microballoon is 658nm;Static Spinning is received Rice fiber/microballoon composite membrane grammes per square metre is 1.08g/m2.Spun-bonded non-woven used, composition fibre diameter is 5 μm, and grammes per square metre is 25g/m2, spun-bonded non-woven exhibits initial filtration efficiency is 0.2%.
A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method, specific steps are as follows:
Step 1: polyacrylonitrile powder is placed in a vacuum drying oven, it is dried in vacuo 8 hours at 70 DEG C;
Step 2: the polyacrylonitrile powder after drying is dissolved in n,N-Dimethylformamide solvent, in magnetic stirring apparatus Upper stirring 12 hours is made into the polyacrylonitrile highly concentrated solution that mass fraction is 10wt%;
Polyacrylonitrile powder after drying is dissolved in n,N-Dimethylformamide solvent, 12 are stirred on magnetic stirring apparatus Hour, it is made into the polyacrylonitrile low concentration solution that mass fraction is 5wt%;
Step 3: using umbrella spinning nozzle (CN103088443A), using tenon sheet by nozzle surface from Center punishment makes nozzle surface left-half fill 10wt% for two parts with same circumference length using liquid feed device Polyacrylonitrile highly concentrated solution, nozzle surface right half part fills the polyacrylonitrile low concentration solution of 5wt%, passes through Static Spinning Silk combined technology synchronous with electrostatic spray, is prepared nanofiber/microballoon composite membrane.It is to receive base with spun-bonded non-woven Material, entire spinning process carry out in closed space, spinning voltage 65KV, drum rotation speed 70r/min, spray head and roller spacing From 20cm, spray head transverse moving speed 120cm/min, liquid supply speed 50mL/h, 23 DEG C of environment temperature, ambient humidity 25%, when spinning Between 20min;
Step 4: nanofiber/spun-bonded non-woven the material upper surface obtained in third step one layer of non-woven cloth of lid again, Spun-bonded non-woven and the spaced sandwich of nanofiber are formed, finally obtains electrostatic after ultrasonic bonds are handled Spinning nano fibre air filting material.
The nano-fiber air filter material is reachable to the filter efficiency that quantity median diameter is 75nm particle 99.99%, filtration resistance 130.7Pa.
Embodiment 2
Filtering material is spun-bonded non-woven and the spaced sandwich of nanofiber, and nanofiber is received for Static Spinning Rice fiber/microballoon composite membrane, wherein electrostatic spinning nano fiber/microballoon structure of composite membrane are as follows: microballoon is embedded in electrostatic spinning nano fiber Between the 3 D stereo cavity structure that is formed;Wherein nanofiber diameter is 204nm;The partial size of microballoon is 569nm;Static Spinning is received Rice fiber/microballoon composite membrane grammes per square metre is 1.25g/m2.Spun-bonded non-woven used, composition fibre diameter is 5 μm, and grammes per square metre is 30g/m2, spun-bonded non-woven exhibits initial filtration efficiency is 0.2%.
A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method, specific steps are as follows:
Step 1: polyacrylonitrile powder is placed in a vacuum drying oven, it is dried in vacuo 8 hours at 70 DEG C;
Step 2: the polyacrylonitrile powder after drying is dissolved in dimethyl sulfoxide solvent, stirred on magnetic stirring apparatus 12 hours, it is made into the polyacrylonitrile highly concentrated solution that mass fraction is 12wt%;
Polyacrylonitrile powder after drying is dissolved in dimethyl sulfoxide solvent, is stirred 12 hours on magnetic stirring apparatus, It is made into the polyacrylonitrile low concentration solution that mass fraction is 6wt%;
Step 3: using umbrella spinning nozzle (CN103088443A), using tenon sheet by nozzle surface from Center punishment makes spray head a portion fill 12wt%'s for four parts with same circumference length using liquid feed device Polyacrylonitrile highly concentrated solution, in addition three parts fill the polyacrylonitrile low concentration solution of 6wt%, pass through electrostatic spinning and electrostatic Combined technology is synchronized by spraying, and nanofiber/microballoon composite membrane is prepared.It is to receive substrate with spun-bonded non-woven, entirely Spinning process carries out in closed space, spinning voltage 60KV, drum rotation speed 100r/min, distance between spray head and roller 15cm, spray head transverse moving speed 80cm/min, liquid supply speed 40mL/h, 25 DEG C of environment temperature, ambient humidity 30%, the spinning time 30min;
Step 4: nanofiber/spun-bonded non-woven the material upper surface obtained in third step one layer of non-woven cloth of lid again, Spun-bonded non-woven and the spaced sandwich of nanofiber are formed, finally obtains electrostatic after ultrasonic bonds are handled Spinning nano fibre air filting material.
The nano-fiber air filter material is reachable to the filter efficiency that quantity median diameter is 75nm particle 99.91%, filtration resistance 102.8Pa.
Embodiment 3
Filtering material is spun-bonded non-woven and the spaced sandwich of nanofiber, and nanofiber is received for Static Spinning Rice fiber/microballoon composite membrane, wherein electrostatic spinning nano fiber/microballoon structure of composite membrane are as follows: microballoon is embedded in electrostatic spinning nano fiber Between the 3 D stereo cavity structure that is formed;Wherein nanofiber diameter is 236nm;The partial size of microballoon is 631nm;Static Spinning is received Rice fiber/microballoon composite membrane grammes per square metre is 1.96g/m2.Spun-bonded non-woven used, composition fibre diameter are 10 μm, grammes per square metre For 30g/m2, spun-bonded non-woven exhibits initial filtration efficiency is 0.1%.
A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method, specific steps are as follows:
Step 1: polyurethane particles are placed in a vacuum drying oven, it is dried in vacuo 8 hours at 110 DEG C;
Step 2: the polyurethane particles after drying are dissolved in n,N-Dimethylformamide solvent, on magnetic stirring apparatus Stirring 12 hours is made into the polyurethane highly concentrated solution that mass fraction is 35wt%;
Polyurethane particles after drying are dissolved in n,N-Dimethylformamide solvent, it is small that 12 are stirred on magnetic stirring apparatus When, it is made into the polyurethane low concentration solution that mass fraction is 20wt%;
Step 3: being used using a kind of electrostatic spinning apparatus (CN104593880A) of polymer fiber mass production More one metal wires are punished reservoir for equal length from center as electrostatic spinning nozzle, using tenon sheet Two parts so that reservoir left-half is filled the polyurethane highly concentrated solution of 35wt%, reservoir right half using liquid feed device It is partially filled with the polyurethane low concentration solution of 20wt%, by electrostatic spinning combined technology synchronous with electrostatic spray, is prepared into To nanofiber/microballoon composite membrane.With spun-bonded non-woven be receive substrate, entire spinning process in closed space into Row, spinning voltage 70KV, drum rotation speed 120r/min, distance 25cm between spray head and roller, spray head transverse moving speed 100cm/min, Liquid supply speed 80mL/h, 27 DEG C of environment temperature, ambient humidity 35%, spinning time 25min;
Step 4: nanofiber/spun-bonded non-woven the material upper surface obtained in third step one layer of non-woven cloth of lid again, Spun-bonded non-woven and the spaced sandwich of nanofiber are formed, finally obtains electrostatic after ultrasonic bonds are handled Spinning nano fibre air filting material.
The nano-fiber air filter material is reachable to the filter efficiency that quantity median diameter is 75nm particle 99.26%, filtration resistance 76.3Pa.
Embodiment 4
Filtering material is spun-bonded non-woven and the spaced sandwich of nanofiber, and nanofiber is received for Static Spinning Rice fiber/microballoon composite membrane, wherein electrostatic spinning nano fiber/microballoon structure of composite membrane are as follows: microballoon is embedded in electrostatic spinning nano fiber Between the 3 D stereo cavity structure that is formed;Wherein nanofiber diameter is 152nm;The partial size of microballoon is 670nm;Static Spinning is received Rice fiber/microballoon composite membrane grammes per square metre is 1.68g/m2.Spun-bonded non-woven used, composition fibre diameter are 10 μm, grammes per square metre For 35g/m2, spun-bonded non-woven exhibits initial filtration efficiency is 0.2%.
A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method, specific steps are as follows:
Step 1: polyacrylonitrile powder is placed in a vacuum drying oven, it is dried in vacuo 8 hours at 70 DEG C;Inclined fluorine will be gathered Ethylene powder is placed in a vacuum drying oven, and is dried in vacuo 8 hours at 130 DEG C;
Step 2: the polyacrylonitrile powder after drying is dissolved in dimethyl sulfoxide solvent, stirred on magnetic stirring apparatus 12 hours, it is made into the polyacrylonitrile highly concentrated solution that mass fraction is 10wt%;
Kynoar powder after drying is dissolved in n,N-Dimethylformamide solvent, is stirred on magnetic stirring apparatus 12 hours, it is made into the Kynoar low concentration solution that mass fraction is 6wt%;
Step 3: being used using a kind of electrostatic spinning apparatus (CN104593880A) of polymer fiber mass production Reservoir is divided into four with equal length as electrostatic spinning nozzle, using tenon sheet by more one metal wires Point, using liquid feed device, reservoir a portion is made to fill the polyacrylonitrile highly concentrated solution of 10wt%, in addition three parts are infused The Kynoar low concentration solution of full 6wt% is prepared and is received by electrostatic spinning combined technology synchronous with electrostatic spray Rice fiber/microballoon composite membrane.It is to receive substrate with spun-bonded non-woven, entire spinning process carries out in closed space, spins Filament voltage 55KV, drum rotation speed 140r/min, distance 20cm between spray head and roller, spray head transverse moving speed 60cm/min, feed flow Speed 30mL/h, 25 DEG C of environment temperature, ambient humidity 40%, spinning time 30min;
Step 4: nanofiber/spun-bonded non-woven the material upper surface obtained in third step one layer of non-woven cloth of lid again, Spun-bonded non-woven and the spaced sandwich of nanofiber are formed, finally obtains electrostatic after ultrasonic bonds are handled Spinning nano fibre air filting material.
The nano-fiber air filter material is reachable to the filter efficiency that quantity median diameter is 75nm particle 99.82%, filtration resistance 95.1Pa.

Claims (8)

1. a kind of mass preparation method of efficient low-resistance electrostatic spinning nano fiber air filting material, comprising:
(1) polymer is added in solvent, stirring obtains the electrostatic spinning polymer solution of high concentration;Wherein electrostatic spinning is poly- The mass percentage concentration of polymer solution is 10-40%;
(2) polymer is added in solvent, stirring obtains the electrostatic spray polymer solution of low concentration;Wherein electrostatic spray is poly- The mass percentage concentration of polymer solution is 3-30%;
(3) needle-free electrostatic spinning nozzle is used, then by electrostatic spinning combined technology synchronous with electrostatic spray, is made and receives Rice fiber/microballoon composite membrane, using rotating cylinder as reception device, spun-bonded non-woven be reception substrate, obtain nanofiber/ Non-weaving cloth composite material, wherein nanofiber/microballoon structure of composite membrane are as follows: formed between microballoon insertion electrostatic spinning nano fiber 3 D stereo cavity structure, electrostatic spinning nano fiber diameter is 100-300nm, and the partial size of microballoon is 500-800nm;
(4) by above-mentioned nanofiber/one layer of non-weaving cloth composite material surface cover spun-bonded non-woven, spun-bonded non-woven is formed The spaced sandwich with nanofiber, then adhesion process is to get electrostatic spinning nano fiber air filting material.
2. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 1 Method, it is characterised in that: in the step (1), (2) polymer be polyacrylonitrile, polyurethane, polysulfones, polyvinylpyrrolidone, Kynoar, polyethylene glycol oxide, polystyrene, polymethyl methacrylate, polycaprolactone, polycaprolactam, in chitosan One or more;Solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, acetone, tetrahydro furan It mutters, one or more of methylene chloride, chloroform, hexafluoroisopropanol, formic acid, acetic acid, ethyl alcohol.
3. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 1 Method, it is characterised in that: stirring is magnetic agitation 10-12h in the step (1), (2).
4. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 1 Method, it is characterised in that: in step (3) use insulating materials, by needle-free electrostatic spinning nozzle surface from center punishment for Electrostatic spinning polymer solution and electrostatic spray polymer solution are injected into not by the part 2-8 of same area or length respectively Same part carries out spinning by electrostatic spinning combined technology synchronous with electrostatic spray.
5. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 4 Method, it is characterised in that: the insulating materials be polytetrafluoroethylene (PTFE), Kynoar, polymethyl methacrylate, polycarbonate, One of polyethylene, polypropylene, polystyrene.
6. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 1 Method, it is characterised in that: the specific process parameter of electrostatic spinning combined technology synchronous with electrostatic spray in the step (3) are as follows: Spinning voltage 40-75KV, drum rotation speed 10-400r/min, distance 10-25cm between spray head and roller, spray head transverse moving speed 10- 300cm/min, liquid supply speed 20-500mL/h, 20-35 DEG C of environment temperature, ambient humidity 20-80%;Entire spinning machine is closed, Temperature and humidity measure and device for automatically regulating are equipped in confined space, spinning nozzle is connected with transverse-moving mechanism, spinning nozzle with it is defeated Liquid pipe is connected, perfusion tube other end connection liquid feed device, and in entire spinning process, liquid feed device is sustainedly and stably supplied to spray head Liquid, it is ensured that spinning is carried out continuously.
7. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 1 Method, it is characterised in that: adhesion process is ultrasonic bonds in the step (4).
8. a kind of mass preparation side of efficient low-resistance electrostatic spinning nano fiber air filting material according to claim 1 Method, it is characterised in that: spun-bonded non-woven in the step (4), fibre diameter are 1-10 μm, grammes per square metre 10-120g/m2, just Beginning filter efficiency is 0.1%-5%.
CN201610784058.9A 2016-08-30 2016-08-30 A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method Expired - Fee Related CN106237717B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610784058.9A CN106237717B (en) 2016-08-30 2016-08-30 A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610784058.9A CN106237717B (en) 2016-08-30 2016-08-30 A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method

Publications (2)

Publication Number Publication Date
CN106237717A CN106237717A (en) 2016-12-21
CN106237717B true CN106237717B (en) 2019-04-09

Family

ID=58080278

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610784058.9A Expired - Fee Related CN106237717B (en) 2016-08-30 2016-08-30 A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method

Country Status (1)

Country Link
CN (1) CN106237717B (en)

Families Citing this family (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106621590B (en) * 2016-12-30 2019-02-26 东华大学 A kind of filtering material and preparation method thereof having antibacterial functions
CN106621840B (en) * 2016-12-30 2019-03-29 东华大学 A kind of function filtering material capable of releasing far infrared ray and preparation method thereof
CN106669384B (en) * 2016-12-30 2020-05-26 东华大学 Composite anti-haze window screen capable of releasing negative ions and electrostatic spinning device and method thereof
CN107158969B (en) * 2017-06-15 2020-12-22 华南理工大学 Functionalized nanofiber filtering material and preparation method and application thereof
CN107299456A (en) * 2017-06-27 2017-10-27 江南大学 A kind of composite nano-fiber membrane and its preparation method and application
CN108097066A (en) * 2017-09-21 2018-06-01 惠州德赛信息科技有限公司 A kind of efficient low-resistance antibacterial of sandwich style removes the preparation method of formaldehyde composite Nano filtering material
CN108842298A (en) * 2018-06-28 2018-11-20 江苏弗瑞仕环保科技有限公司 The preparation method of high efficiency filter composite cellulosic membrane
JP6847893B2 (en) * 2018-07-02 2021-03-24 株式会社東芝 Electrode structure and rechargeable battery
CN109837763A (en) * 2019-02-01 2019-06-04 湖南工程学院 A kind of preparation method of pearl powder base uvioresistant fabric
CN110904531A (en) * 2019-11-28 2020-03-24 苏州市雄林新材料科技有限公司 High-hydrophobicity TPU film and preparation method thereof
CN111359452B (en) * 2020-03-18 2021-11-12 北京化工大学 Structure-enhanced hydrotalcite-immobilized composite fiber membrane, and preparation method and application thereof
CN113491960A (en) * 2020-04-03 2021-10-12 中国科学院宁波材料技术与工程研究所 High-temperature-resistant oil-water separation membrane and preparation method and application thereof
CN111688288A (en) * 2020-05-22 2020-09-22 南京金思博纳米科技有限公司 Flexible nanofiber filter membrane and preparation method thereof
US20220042206A1 (en) * 2020-08-05 2022-02-10 Nano And Advanced Materials Institute Limited Particle-coated fiber and method for forming the same
CN112195565B (en) * 2020-09-27 2022-11-01 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of electrostatic spinning multilayer nanofiber membrane for indoor air humidity adjustment, product and application
CN112755651B (en) * 2020-12-31 2022-07-08 东华大学 Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof
CN113171654A (en) * 2021-04-28 2021-07-27 广东溢达纺织有限公司 Filter fiber layer, preparation method thereof and mask
CN113584893A (en) * 2021-08-03 2021-11-02 上海工程技术大学 Nano-fiber medical heat-preservation protective clothing fabric and preparation method thereof
CN114277509B (en) * 2021-12-24 2023-01-03 江南大学 Electrostatic spinning polyimide uniform small-aperture nanofiber membrane and preparation method and application thereof
CN114635230B (en) * 2022-04-02 2024-03-26 天津工业大学 Bulk super-hydrophobic nanofiber membrane for membrane distillation and preparation method thereof
CN114917765B (en) * 2022-05-20 2023-05-02 厦门大学 Preparation method of fluff nanofiber antibacterial high-efficiency low-resistance air filtering membrane
CN115008849A (en) * 2022-06-15 2022-09-06 东华大学 Non-woven material-based self-bonding and self-reinforcing multi-stage structure micro-nano composite film and preparation method thereof
CN115161882B (en) * 2022-07-14 2024-02-27 苏州凯姆勒绝缘材料有限公司 Low-dielectric polyimide/polytetrafluoroethylene microsphere composite nanofiber membrane and preparation method thereof
CN115178105A (en) * 2022-08-25 2022-10-14 中国矿业大学 Long-acting filtering membrane with uniformly distributed biological electrets on polylactic acid nanofiber surface and preparation method thereof
CN115538181A (en) * 2022-11-04 2022-12-30 广东省美净滤清器有限公司 Efficient fade-resistant electret filter material for dust removal and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101947415A (en) * 2010-08-13 2011-01-19 东华大学 Combination of electrostatic spinning and electrostatic spraying for preparing nanofibre base composite separation membrane
CN103768660A (en) * 2014-02-25 2014-05-07 江南大学 Method for preparing surface medicinal coating of gastric tube
CN104645715A (en) * 2015-01-08 2015-05-27 东华大学 High-efficiency and low-resistance nanofiber air filtering material for gauze mask and preparation method of filtering material
CN105195028A (en) * 2015-07-03 2015-12-30 东华大学 Preparation method of composite nanofiber ultra-filtration membrane

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101795747B (en) * 2007-09-08 2014-01-01 日本无机株式会社 Filter medium for air filter and air filter

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101947415A (en) * 2010-08-13 2011-01-19 东华大学 Combination of electrostatic spinning and electrostatic spraying for preparing nanofibre base composite separation membrane
CN103768660A (en) * 2014-02-25 2014-05-07 江南大学 Method for preparing surface medicinal coating of gastric tube
CN104645715A (en) * 2015-01-08 2015-05-27 东华大学 High-efficiency and low-resistance nanofiber air filtering material for gauze mask and preparation method of filtering material
CN105195028A (en) * 2015-07-03 2015-12-30 东华大学 Preparation method of composite nanofiber ultra-filtration membrane

Also Published As

Publication number Publication date
CN106237717A (en) 2016-12-21

Similar Documents

Publication Publication Date Title
CN106237717B (en) A kind of efficient low-resistance electrostatic spinning nano fiber air filting material and mass preparation method
Wei et al. Mass production of nanofibers from needleless electrospinning by a novel annular spinneret
CN104289042B (en) A kind of electrostatic spinning nano fiber electret filtering material and preparation method thereof
Koenig et al. A new prototype melt-electrospinning device for the production of biobased thermoplastic sub-microfibers and nanofibers
CN105239184B (en) A kind of bacteria cellulose/graphene/ferroso-ferric oxide composite membrane and preparation method thereof
CN105926161B (en) A kind of preparation method of the thickness combined nano fiber air filtering material with gradient-structure
Stojanovska et al. A review on non-electro nanofibre spinning techniques
CN102242464B (en) Polymer-ceramic compound nanometer fibrous membrane as well as preparation method and application thereof
Zhang et al. Solvent-free electrospinning: opportunities and challenges
Wang et al. Functional polymeric nanofibers from electrospinning
CN102584211B (en) Method for preparing micro/nano porous ceramic fibers by low-temperature electrostatic spinning
CN102534822B (en) Device and method for preparing polysulfonamide nanometer fiber nets by means of airflow-electrostatic combination
CN103394114B (en) A kind of preparation method of medical dressing chitosan-based superfine fiber carrier material
Sharma et al. Electrospinning: the technique and applications
CN110136998B (en) Preparation method and application of metal organic framework carbon fiber composite film
CN104762696B (en) A kind of preparation method of Coaxial Nanofibers
CN102691176A (en) Method for preparing patterning nanofiber membrane by utilizing insulating receiving template static spinning
Chen et al. Review of the principles, devices, parameters, and applications for centrifugal electrospinning
CN105903271B (en) Controllable mixing nanostructured fibers composite filter material and preparation method thereof
CN104451912A (en) Preparing device and method for forming micro-nanofiber
CN101831762A (en) Composite fiber porous membrane composited by ornithoctonus huwena threads and polylactic acid and method for producing same
CN113368712B (en) Efficient air filtration composite nanofiber membrane and preparation method thereof
CN106480518B (en) A kind of preparation method of electrostatic spinning collection device and gradient orientations structure nano fiber
CN109825956A (en) A kind of reverse osmosis membrane backing material and preparation method thereof
Hasan et al. Application of electrospinning techniques for the production of tissue engineering scaffolds: a review

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information

Inventor after: Xiao-Hong Qin

Inventor after: Gao Hanchao

Inventor after: Gao Jing

Inventor after: Yang Yuqiong

Inventor after: Zhang Hongnan

Inventor before: Xiao-Hong Qin

Inventor before: Gao Hanchao

Inventor before: Gao Jing

Inventor before: Zhang Hongnan

CB03 Change of inventor or designer information
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20190409

Termination date: 20210830

CF01 Termination of patent right due to non-payment of annual fee