CN105200539B - A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method and the composite filter material prepared using this method - Google Patents
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method and the composite filter material prepared using this method Download PDFInfo
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Abstract
The present invention relates to a kind of electrospinning process and its nanofiber of preparation/spun-bonded non-woven fabrics composite filter material, the electrospinning process is to be insulated between Multi needle electrostatic spinning, the syringe needle of Multi needle electrostatic spinning；Obtained nanofiber/spun-bonded non-woven fabrics composite filter material is composited for lamination is overlapped successively from low to high by media filtration efficiency from bottom to top with material, make to have the one of electrostatic spinning fiber per layer laminate material upwardly, and covering a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer and the bottom are all spun-bonded non-woven fabrics layer；Adjacent two layers lamination material, one layer of filter efficiency value to 0.02~10 μm of particle is 1.03~1.3 times of following one layer above, the lamination material superposition number of plies is 2~6 layers, spun-bonded non-woven fabrics are formed with the spaced sandwich of electret effect nanofiber, nanofiber/spun-bonded non-woven fabrics composite filter material is made；Nanofiber/spun-bonded non-woven fabrics composite filter material to the filter efficiency of 0.02~10 μm of particle up to 99.999% and more than, pressure drag is maintained at 10~30Pa.
Description
Technical field
The invention belongs to electrostatic spinning technique field, it is related to nanofiber/spunbond of a kind of electrospinning process and its preparation
Non-woven fabric compounded filtering material.
Background technology
During Multi needle electrostatic spinning, electric jamming can be produced between syringe needle, makes the electric-field strength between syringe needle and syringe needle
Degree produces difference, so that cause jet unstable, the uniformity for the tunica fibrosa that final influence spinning is obtained.To in spinning process
Electric-field intensity is controlled so that every spinning head jet keeps stable, can be effectively improved the uniformity of tunica fibrosa, realizes filter
Expect the stabilization of performance.It is main in existing literature that electric field syringe needle is controlled using metal auxiliary electrode, by spinning head
The metal ring of identical with syringe needle application voltage is added at needle point come make jet stability (Buttafoco L, Kolkman N G,
Engbers-Buijtenhuijs P,et al.Electrospinning of collagen and elastin for
tissue engineering applications[J].Biomaterials,2006,27(5):724-34.), or in pin
Head is outside to carry out electric field controls (Kim G, Cho Y-S, Kim W D.Stability analysis for using round metal is logical
multi-jets electrospinning process modified with a cylindrical electrode[J]
.European Polymer Journal,2006,42(9):2031-8.)；Patent CN203583021U discloses a kind of " flat board
The many shower nozzle electrostatic spinning devices of electrode ", it on metallic plate by before spinning head plus a metallic plate, having and that spinning head coordinates is logical
Hole, high voltage power supply is connected with spinning head and metallic plate simultaneously, identical point position is made it have, so that jet stability；Red legend is refined etc.
(red legend is refined, history Jingjing, and poplar grace dragon auxiliary electrodes act on lower pair of nozzle electrospinning electric field and jet force analysis [J] weavings
Journal, 2012,06:6-9.) by installing conical metal auxiliary electrode additional at shower nozzle, auxiliary electrode is connected to reduce with shower nozzle
Electric jamming between needle adjacent.These methods pass through additional metal auxiliary electrode, auxiliary electrode and syringe needle on spinning syringe needle
Apply the method for big small voltage of the same race, improved spinning jet stability.But in high voltage spinning, syringe needle and auxiliary
Electric discharge phenomena easily occur between electrode, the spark of generation easily causes security incident.
Static Spinning is a kind of nanofiber technology of preparing that spinning is carried out using high voltage, while being also a kind of nanofiber
Electret technology, can inject a large amount of space charges among fiber during spinning, space charge is easily by the depth of fibrous inside
Trap is captured, while can induce dipole polarization and produce polarization charge, can pass through electrostatic during being filtered to particle
Suction-operated lifting filter efficiency (Yao Cui pretty young woman fusion-jetting polypropylene filtrate electret Study on influencing factors [D] Donghua University,
2014.).And electret filtering material is during using and storing, due to moisture present in air and particulate etc. and electret
Material is directly contacted, and accelerates surface charge loss in electret material, so that the decay of electret effect accelerates, ultimately results in filtrate
Filter efficiency unstable (Tian Tao, Wu Jinhui, Hao Limei, Lin Song, the storing up electricity performance of poplar Jing Quan polypropylene fibre electret filters
[J] textile journals, 2010,31 (6):25-28.).
The content of the invention
The technical problems to be solved by the invention are to provide nanofiber/spunbond of a kind of electrospinning process and its preparation
Non-woven fabric compounded filtering material.For the problem of electric jamming, using insulation during Multi needle electrostatic spinning in the prior art
Material carries out anti-tampering isolation processing to each syringe needle.
A kind of electrospinning process of the present invention, is Multi needle electrostatic spinning, the syringe needle of the Multi needle electrostatic spinning it
Between insulate.
It is used as preferred technical scheme：
A kind of electrospinning process as described above, the same insulating base of Needle sharing.
Insulation refers to using insulating materials to each syringe needle between a kind of electrospinning process as described above, the syringe needle
Carry out anti-tampering isolation processing；Insulating materials formation isolation groove specially is with the surrounding of the syringe needle, completely cuts off the shape of groove
For square or circle, the depth of isolation groove is 1~5 times of the needle length.When applying high voltage at spinning head, insulation
Material isolation rooved face produces polarization charge, and the polarized electric field of formation is with former direction of an electric field on the contrary, can be to this direction electric-field intensity
Certain negative function is produced, the electric field between needle adjacent is interfered with each other reduction, so that jet stability, and in height
Electric discharge phenomena will not occur in Voltage Static electro-spinning process.
A kind of electrospinning process as described above, the insulating materials be Acrylnitrile-Butadiene-Styrene,
Makrolon, polymethyl methacrylate, polypropylene, polyamide, polystyrene, polyvinyl chloride, polyethylene, polytetrafluoroethylene (PTFE),
Kynoar or PET.
Present invention also offers a kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, concretely comprise the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) titanium dioxide nanofiber or nanometer activated carbon fiber are added in ethanol, and ultrasonic disperse, obtain uniform
Dispersion liquid；
B) taken out after spun-bonded non-woven fabrics are soaked in the dispersion liquid of titanium dioxide nanofiber or nanometer activated carbon fiber,
Hang in baking oven, 50~60 DEG C of drying obtain the spunbond of surface deposition of titanium oxide nanofiber or nanometer activated carbon fiber
Non-woven fabrics base material；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles are added in solvent, and ultrasonic disperse, obtain the dispersed dispersion liquid of nano particle；
B) polymer is added in the dispersion liquid, is configured to uniform and stable spinning solution；
C) spinning solution is carried out insulating between Multi needle electrostatic spinning, the syringe needle of the Multi needle electrostatic spinning；Spun
Polymer nanofiber received with the spun-bonded non-woven fabrics base material that is obtained in step (1), obtain uniform deposition on spun-bonded non-woven fabrics
The composite filtering material of Static Spinning polymer nanofiber, the deposition of polymer nanofiber can be adjusted by adjusting the spinning time
Control；
(3) preparation of superfine nano fiber dispersion
Polyvinyl butyral solution is first prepared, then it is added with superfine nano fiber and divided in high speed beater
Dissipate, obtain uniform superfine nano fiber dispersion；
(4) composite filtering material immersion treatment
Taken out after the composite filtering material is soaked in the superfine nano fiber dispersion, drying obtains composite filtering material
Fiber surface deposits the filtrate of superfine nano fiber；As lamination material；
The superfine nano fiber deposit thickness on the composite filtering material surface after immersion treatment is 20~200nm；
Test obtains filter efficiency value of the lamination material to 0.02~10 μm of particle；
(5) step (1)~(4) are repeated several times, the lamination material of different filter efficiencies, the filtering of lamination material is obtained
Efficiency can be by regulating and controlling in step (1) ultra-fine in dispersion liquid in Static Spinning polymer nanofiber deposition and step (4) receive
The mass fraction of rice fiber is controlled；
(6) by lamination material, it is overlapped compound, is often laminated successively from low to high by media filtration efficiency from bottom to top
Layer material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer
All it is spun-bonded non-woven fabrics layer with the bottom；Adjacent two layers lamination material, above one layer of filtering to 0.02~10 μm of particle
Efficiency value is 1.03~1.3 times of following one layer, forms spun-bonded non-woven fabrics with having electret effect nanofiber spaced
Sandwich, is made nanofiber/spun-bonded non-woven fabrics composite filter material；
The lamination material superposition number of plies is 2~6 layers, forms spun-bonded non-woven fabrics row alternate with having electret effect nanofiber
The sandwich of row, is made nanofiber/spun-bonded non-woven fabrics lamination composite filter material.
A kind of nanofiber/spun-bonded non-woven fabrics lamination composite filter material preparation method as described above, the step (1)
In,
In titanium dioxide nanofiber or the nanometer activated carbon fiber dispersion liquid, fiber quality fraction is 0.1~5%,
Soak time is 5~10min；A diameter of 50~the 100nm of titanium dioxide nanofiber or nanometer activated carbon fiber, length is
100~300nm；
The spun-bonded non-woven fabrics, it is 1~50 μm that it, which constitutes fibre diameter, and non-woven fabrics aperture size is 5~120 μm, grammes per square metre
For 10~300g/m2, exhibits initial filtration efficiency is 5%~40%；
The drying refers to hang in baking oven, and temperature is 50~60 DEG C；
Titanium dioxide nanofiber has photo-catalysis function, and light drop can be carried out to the impurity adsorbed under illumination effect
Solution, nanometer activated carbon fiber is due to its higher specific surface area, with good adsorption function.Sunk using on spun-bonded non-woven fabrics
Product titanium dioxide nanofiber or nanometer activated carbon fiber are as base material, and the product finally given when in use, can be in air
Peculiar smell play absorption and photodegradation.
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method as described above, step (2) described spinning
In solution, the concentration of polymer is 5~40wt%, and the addition of inorganic nanoparticles is polymer and the total matter of inorganic nanoparticles
0.1~10wt% of amount；
The inorganic nanoparticles are silica, alundum (Al2O3), zinc oxide, barium monoxide, titanium dioxide, five oxidations two
Tantalum, barium titanate, lead zirconate titanate, silicon nitride, tourmaline, boehmite or silsesquioxane nano particle；
The mechanism of action of the inorganic nanoparticles is：The inorganic nanoparticles have under conditions of external electric field presence
The injection of space charge and the generation of polarization charge, there is very big humidification, and inorganic nanoparticles to electret effect
The interface produced is mixed with organic polymer can produce interfacial polarization in the presence of external electric field, produce polarization charge, same to increase
Strong electret effect.
The polymer be Kynoar, polybutylene terephthalate, PET, polyarylate,
Polyvinyl acetate, nylon 6, polymethyl methacrylate, polyaniline, polyethylene glycol oxide, polyvinylpyrrolidone, polyacrylonitrile,
Polycaprolactone, polyurethane, fluorinated polyurethane, polysulfones, polyether sulfone, Kynoar-hexafluoropropene, Kynoar-tetrafluoro second
One kind in alkene-perfluoro methyl vinyl ether, Kynoar-CTFE, or be the mixing of several polymer above
Thing；
Wherein described solvent is corresponded to respectively according to type of polymer：
Kynoar：N,N-dimethylformamide (DMF), 1-METHYLPYRROLIDONE (NMP), dimethyl acetamide
(DMAc), triethyl phosphate and dimethyl sulfoxide (DMSO) (DMSO)；
Polybutylene terephthalate：Dichloromethane, tetrahydrofuran (THF), chloroform or acetone；
PET：Dichloromethane, tetrahydrofuran, chloroform or acetone；
Polyarylate：Dichloromethane, tetrahydrofuran, chloroform or acetone；
Polyvinyl acetate：Toluene, acetone, ethanol, acetic acid, ethyl acetate or chloroform；
Nylon 6：Formic acid；
Polymethyl methacrylate：Chloroform, acetic acid, ethyl acetate, acetone or toluene；
Polyaniline：N,N-dimethylformamide or 1-METHYLPYRROLIDONE；
Polyethylene glycol oxide：N,N-dimethylformamide, ethanol, water or chloroform；
Polyvinylpyrrolidone：Water, ethanol, DMAC N,N' dimethyl acetamide or N,N-dimethylformamide；
Polyacrylonitrile：N,N-dimethylformamide or dimethyl sulfoxide (DMSO)；
Polycaprolactone：N,N-dimethylformamide or acetone；
Polyurethane：N,N-dimethylformamide, acetone or 1-METHYLPYRROLIDONE；
Fluorinated polyurethane：N,N-dimethylformamide, acetone or 1-METHYLPYRROLIDONE；
Polysulfones and polyether sulfone：N,N-dimethylformamide, acetone, 1-METHYLPYRROLIDONE, dimethyl acetamide or tetrahydrochysene
Furans；
Kynoar-hexafluoropropene：N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl acetamide, phosphoric acid
Triethyl or dimethyl sulfoxide (DMSO)；
Kynoar-tetrafluoroethylene-perfluoro methyl vinyl ether：N,N-dimethylformamide, 1-METHYLPYRROLIDONE,
Dimethyl acetamide, triethyl phosphate or dimethyl sulfoxide (DMSO)；
Kynoar-CTFE：N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl acetamide, phosphorus
Triethylenetetraminehexaacetic acid ester or dimethyl sulfoxide (DMSO)；
In the step a), the ultrasonic disperse time is 20~70 minutes；
In the step b), after polymer is added in the dispersion liquid, magnetic agitation 8~10 hours；
In the step c), the process conditions of Multi needle electrostatic spinning are：10~60KV of supply voltage, spinning environment condition
For 15~35 DEG C of temperature, relative humidity 25~90%；Multi needle spinneret unit syringe needle 2~30cm of spacing, spinneret unit syringe needle number
Measure as 6~90；In a kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method as described above, step (3),
Solute mass fraction is 0.1~5% in the polyvinyl butyral solution；Used in the preparation polyvinyl butyral solution
Solvent is tetrahydrofuran, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, acetone, chloroform, cresols, dimethyl sulfoxide (DMSO), second
Alcohol, normal propyl alcohol, isopropanol, n-butanol, DAA, methyl acetate, ethyl acetate, butyl acetate, toluene, N- crassitudes
One or more of mixtures in ketone, MEK, methyl ethyl ketone；The preparation polyvinyl butyral solution solvent for use
Solubility parameter at least differ 4 with the solubility parameter numerical value of polymer used in electrostatic spinning fiber, can dissolve poly- well
Ethanol butyral still will not destroy the structure for the nanofiber to be disperseed, will not to electrostatic spinning fiber inside electret effect into
Loss, the wherein unit of solubility parameter are (J/cm3)1/2。
Mass fraction shared by superfine nano fiber is 0.01%~5% in the nanofiber dispersion liquid；The Nanowire
A diameter of 10~150nm is tieed up, length is 100~150nm；
The superfine nano fibrous material be polystyrene, polyester, polyvinyl acetate, nylon 6, nylon66 fiber, polyvinyl alcohol,
One in polymethyl methacrylate, polyaniline, polyethylene glycol oxide, polyacrylonitrile, polycaprolactone, polyurethane, polysulfones, polyether sulfone
Kind or two kinds and above polymer mixture；
The rotating speed of the high speed beater is 5000 revs/min~8000 revs/min, and the quick of cutter head is beaten during this
Shear action, is conducive to reducing the length of institute's dispersing ultrafine nanofiber, and obtains uniform superfine nano fiber dispersion.
It is described in a kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method as described above, step (4)
The time of immersion is 5~30min；The drying refers to hang in baking oven, 25~50 DEG C of drying；The deposition of nanofiber with
And the thickness of sedimentary can be by controlling in dispersion liquid the mass ratio of nanofiber and the time of impregnation process to control.
It is described in a kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method as described above, step (5)
Multiplicating refers to repeat 2~6 times, namely obtains 2~6 layers of lamination material.
High-flexibility, superfine nano fiber are deposited by the composition fiber surface in composite filtering material, formed on main fibre
Lamination material containing " point shape secondary structure ".Main body crude fibre for the larger particle of particle diameter there is preferably filtering to imitate
Really, while forming larger aperture structure is conducive to passing through for air-flow, and two grades of fractal structures have for ultra-fine grain it is excellent
Different strainability, while its more soft characteristic so that have high velocity air by when will not produce barrier effect to air-flow,
So as to which the increase of resistance pressure drop will not be caused.The effect of thin nanofiber dispersion liquid is prepared using polyvinyl butyral solution
It is：Polyvinyl butyral solution can adhere to superfine nano fiber in composite filtering material immersion treatment step as adhesive
In the composition fiber surface of composite filtering material；In addition, PVOH butyral has hydrophobicity, meeting after composite filtering material immersion treatment is existed
Composite filtering material composition fiber surface formation can assign composite filtering material certain hydrophobicity.
Present invention also offers a kind of nanofiber/spun-bonded non-woven fabrics composite filter material, the nanofiber/spunbond without
It is that gradient is laminated composite filtering material to spin cloth composite filter material, for by lamination material from bottom to top by media filtration efficiency by it is low to
Height is overlapped is composited successively, makes to have the one of electrostatic spinning fiber per layer laminate material upwardly, and in most last layer
Surface covers a spun-bonded non-woven fabrics, it is ensured that top layer and the bottom are all spun-bonded non-woven fabrics layer；Adjacent two layers lamination material, above
One layer of filter efficiency value to 0.02~10 μm of particle is 1.03~1.3 times of following one layer, and lamination is superimposed the number of plies with material
For 2~6 layers, formed spun-bonded non-woven fabrics with the spaced sandwich of electret effect nanofiber, be made nanofiber/
Spun-bonded non-woven fabrics composite filter material；The nanofiber/spun-bonded non-woven fabrics composite filter material is to 0.02~10 μm of particle
Filter efficiency up to more than 99.999%, pressure drag is maintained at 10~30Pa.
For electret material in above-mentioned background technology when directly being contacted with surrounding environment, by moisture in air and other
The influence of factor, can accelerate the dissipation of electret material electric charge, make the problem of electret effect weakens, and complex form is laminated using gradient
Resulting electrostatic spinning fiber and spun-bonded non-woven fabrics are carried out it is interspersed be superimposed, construct electrostatic spinning fiber interlayer spun-bonded non-woven fabrics it
Between structure.On the one hand this structure forms classified filtering, is favorably improved filtrate efficiency；On the other hand, containing electret effect
Electrostatic spinning fiber interlayer reduces between the spun-bonded non-woven fabrics Jing Guo hydrophobic treatment and is directly contacted with external environment and electricity is produced
The intensity of raw lotus influence, can slow down the decay of electret effect, so as to be conducive to the maintenance of media performance.
Beneficial effect
1. by the present invention in that make spinning to carrying out anti-tampering isolation processing between Multi needle Static Spinning syringe needle with insulating materials
Electric jamming weakens between silk syringe needle, is conducive to the stabilization of spinning jet, the Nanowire obtained by such a mode electrostatic spinning
Dimension film has good uniformity.Meanwhile, will not occur electric discharge phenomena during using this mode high voltage electrostatic spinning, be conducive to peace
Full production.
2. the present invention passes through deposition high-flexibility on the nano fibrous membrane and spun-bonded non-woven fabrics that are obtained in electrostatic spinning, ultra-fine
Nanofiber, to form on main fibre the composite filter material for containing " point shape secondary structure ".Main body crude fibre is for particle diameter
Larger particle has preferable filter effect, while forming larger aperture structure is conducive to passing through for air-flow, and two grades
Fractal structure has excellent strainability for ultra-fine grain, while its more soft characteristic so that there is high velocity air to lead to
It is out-of-date to produce barrier effect to air-flow, so that the increase of resistance pressure drop will not be caused.The filter material obtained using the manner
There is material high filtration to imitate filter, the characteristics of low pressure hinders.
3. the present invention by by the electrostatic spinning nano fiber film of different filter capacities and hydrophilic spunbonded nonwoven cloth according to filtering
Efficiency form from low to high carries out interspersed superposition, make the nano fibrous membrane interlayer with electret effect spun-bonded non-woven fabrics it
Between, hinder the electrostatic spinning fiber acted on electret and directly contacted with external environment, obtained electrostatic spinning fiber/spunbond nonwoven
Cloth composite filtering material has good Charge Storage Stability, so that filter effect maintenance is good.
Brief description of the drawings
Fig. 1 is Static Spinning syringe needle isolating device schematic diagram, wherein, 1 is insulating materials dividing plate, and 2 be spinning head apparatus, and 3 are
Spinneret base.
Fig. 2 is nanofiber/spun-bonded non-woven fabrics composite filter material schematic diagram, wherein, 4 be spun-bonded non-woven fabrics, and 5 be electrostatic
Spinning nano fibre.
Fig. 3 is electrostatic spinning nano fiber/hydrophilic spunbonded nonwoven cloth composite filtering material and electrostatic spinning nano fiber/common spunbond
Non-woven fabric compounded filtrate crosses performance with placing number of days graph of a relation, wherein, 23 DEG C of environment temperature, humidity 80%, bright of the chart is specially
Nanofiber/spun-bonded non-woven fabrics composite filter material prepared by profit has excellent electric charge storage stability, so that filter effect
With good maintenance.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
A kind of electrospinning process of the present invention, is exhausted between Multi needle electrostatic spinning, the syringe needle of Multi needle electrostatic spinning
Edge.Wherein, the same insulating base of Needle sharing；Insulation refers to anti-tampering to the progress of each syringe needle using insulating materials between syringe needle
Isolation is handled；Insulating materials formation isolation groove specially is with the surrounding of syringe needle, completely cut off groove is shaped as square or circle,
The depth for completely cutting off groove is 1~5 times of needle length；Insulating materials be Acrylnitrile-Butadiene-Styrene, makrolon,
Polymethyl methacrylate, polypropylene, polyamide, polystyrene, polyvinyl chloride, polyethylene, polytetrafluoroethylene (PTFE), Kynoar
Or PET.
Embodiment 1
A kind of electrospinning process, is to be insulated between Multi needle electrostatic spinning, the syringe needle of Multi needle electrostatic spinning.Fig. 1 is
Static Spinning syringe needle isolating device schematic diagram, wherein, 1 is insulating materials dividing plate, and 2 be spinning head apparatus, and 3 be spinneret base；Syringe needle
Share same insulating base；Insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between syringe needle；Tool
Body is is with insulating materials formation isolation groove in the surrounding of syringe needle, and being shaped as isolation groove is square, and the depth of isolation groove is syringe needle
1 times of length；Insulating materials is Acrylnitrile-Butadiene-Styrene.
Embodiment 2
A kind of electrospinning process, is to be insulated between Multi needle electrostatic spinning, the syringe needle of Multi needle electrostatic spinning.Wherein,
The same insulating base of Needle sharing；Insulation refers to carry out at anti-tampering isolation each syringe needle using insulating materials between syringe needle
Reason；Insulating materials formation isolation groove specially is with the surrounding of syringe needle, completely cuts off the circle that is shaped as of groove, the depth of isolation groove is
3 times of needle length；Insulating materials is makrolon.
Embodiment 3
A kind of electrospinning process, is to be insulated between Multi needle electrostatic spinning, the syringe needle of Multi needle electrostatic spinning.
Concretely comprise the following steps：
(1) inorganic nanoparticles titania nanoparticles are added in solvent DMF, and ultrasound point
Dissipate 30 minutes, obtain the dispersed dispersion liquid of nano particle；
(2) polymer polysulfones is added in dispersion liquid, magnetic agitation 8 hours, is configured to uniform and stable spinning solution,
Wherein, the mass fraction of polysulfones is 12%, and the addition of inorganic nanoparticles is polymer and inorganic nanoparticles gross mass
10%；
(3) spinning solution is subjected to Multi needle electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：Supply voltage
45KV, spinning environment condition is 35 DEG C of temperature, relative humidity 25%, spinning solution rate of flooding 4mL/h；Multi needle spinneret unit pin
Head spacing 3cm, spinneret unit syringe needle quantity is 60, and the spinning time is 40min；Between the syringe needle of Multi needle electrostatic spinning absolutely
Edge, wherein, the same insulating base of Needle sharing；Insulation refers to anti-tampering to the progress of each syringe needle using insulating materials between syringe needle
Isolation is handled；Insulating materials formation isolation groove specially is with the surrounding of syringe needle, being shaped as isolation groove is square, isolation groove
Depth is 2 times of needle length；Insulating materials is Acrylnitrile-Butadiene-Styrene；The polymer nanofiber spun
Received with spun-bonded non-woven fabrics base material, obtain the composite filtering material of spun-bonded non-woven fabrics deposited on substrates Static Spinning polymer nanofiber,
Wherein, spun-bonded non-woven fabrics, it is 20 μm that it, which constitutes fibre diameter, and non-woven fabrics aperture size is 30 μm, and grammes per square metre is 10g/m2, initial mistake
It is 5% to filter efficiency；
(4) composite filtering material that Static Spinning polysulfones nanofiber is deposited on spun-bonded non-woven fabrics is made by step (1)~(3),
Obtained composite filtering material is divided into two parts, a part is used to test grammes per square metre, and a part is used to test strainability.
10 parts will be cut into for testing the composite filtering material of grammes per square metre, electrostatic spinning fiber layer in every part of composite filtering material is tested respectively
Grammes per square metre.It is 30g/m to measure electrostatic spinning fiber layer grammes per square metre value2、34g/m2、33g/m2、33g/m2、32g/m2、33g/m2、33g/
m2、34g/m2、32g/m2、33g/m2, the grammes per square metre coefficient of variation is 3.36%；
10 test points are taken at random on the composite filtering material for testing strainability, its to 0.02~10 μm is tested
The filter efficiency of grain, obtain filter efficiency value for 93.1225%, 93.1456%, 93.1458%, 93.1267%,
93.1258%th, 93.0321%, 93.1467%, 93.1367%, 93.1457%, 93.1299%；Corresponding pressure drag be 19Pa,
20Pa、19Pa、19Pa、20Pa、18Pa、19Pa、19Pa、20Pa、19Pa.Calculate the variation lines of composite filtering material filter efficiency
Number is 0.035%, and the coefficient of variation of pressure drag is 3.13%；
Comparative example
This comparative example is the comparative example of embodiment 3
Concretely comprise the following steps：
Step (1) is identical with step (1) in embodiment 3；
Step (2) is identical with step (2) in embodiment 3；
In step (3) in addition to spinning syringe needle is without anti-tampering isolation processing, remaining parameter and step (3) in embodiment 3
It is identical；
(4) composite filter that Static Spinning polyacrylonitrile nanofiber is deposited on spun-bonded non-woven fabrics is made by step (1)~(3)
Material, is divided into two parts by obtained composite filtering material, and a part is used to test grammes per square metre, and a part is used to test strainability.
10 parts will be cut into for testing the composite filtering material of grammes per square metre, electrostatic spinning fiber layer in every part of composite filtering material is tested respectively
Grammes per square metre.It is 30g/m to measure electrostatic spinning fiber layer grammes per square metre value2、28g/m2、34g/m2、40g/m2、34g/m2、28g/m2、29g/
m2、36g/m2、31g/m2、33g/m2, the coefficient of variation of grammes per square metre is：11.34%.
10 test points are taken at random on the composite filtering material for testing strainability, its to 0.02~10 μm is tested
The filter efficiency of grain, obtain filter efficiency value for 90.1577%, 89.9892%, 92.0976%, 90.9104%,
90.2801%th, 92.9726%, 92.0023%, 92.1078%, 93.1998%, 91.0947%；Corresponding pressure drag be 20Pa,
18Pa、18Pa、20Pa、20Pa、19Pa、23Pa、19Pa、21Pa、17Pa.Calculate the variation lines of composite filtering material filter efficiency
Number is 1.13%, and the coefficient of variation of pressure drag is 8.35%.
All values for coefficient of variation in the example in contrast of comparative example 3, it is possible to find the composite filtering material obtained in embodiment 3 is quiet
The coefficient of variation of the electro spinning nano fiber layer coefficient of variation of grammes per square metre, composite filtering material filter efficiency and pressure drag is than phase in its comparative example
The value answered is small, illustrates using the composite filtering material ratio obtained after Static Spinning syringe needle isolating device without using Static Spinning syringe needle isolating device
Obtained composite filtering material is uniform.
Embodiment 4
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, is concretely comprised the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) titanium dioxide nanofiber is added in ethanol, and ultrasonic disperse, uniform dispersion liquid is obtained, wherein, disperse
Fiber quality fraction is 0.1% in liquid, and soak time is 5min；The a diameter of 50nm of titanium dioxide nanofiber, length is
100nm；
B) take out, hang in baking oven, 50 after spun-bonded non-woven fabrics are soaked in the dispersion liquid of titanium dioxide nanofiber
DEG C drying, obtain surface deposition of titanium oxide nanofiber spun-bonded non-woven fabrics base material.Wherein, spun-bonded non-woven fabrics, it constitutes fine
A diameter of 50 μm are tieed up, non-woven fabrics aperture size is 30 μm, and grammes per square metre is 68g/m2, exhibits initial filtration efficiency is 15%；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles nano SiO 2 particle is added in solvent DMF, and ultrasonic disperse
30 minutes, obtain the dispersed dispersion liquid of nano particle；
B) polymer polyvinylidene fluoride is added in dispersion liquid, magnetic agitation 8 hours, is configured to uniform and stable spinning
Solution, wherein, the mass fraction of Kynoar is 20%, and the addition of inorganic nanoparticles is polymer and inorganic nano
The 9% of grain gross mass；
C) spinning solution is subjected to Multi needle electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：Supply voltage
15KV, spinning environment condition is 35 DEG C of temperature, relative humidity 25%, spinning solution rate of flooding 6mL/h；Multi needle spinneret unit pin
Head spacing 2cm, spinneret unit syringe needle quantity is 90；Insulated between the syringe needle of Multi needle electrostatic spinning, wherein, Needle sharing is same
One insulating base；Insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between syringe needle；Specially exist
The surrounding of syringe needle is with insulating materials formation isolation groove, and being shaped as isolation groove is square, and the depth of isolation groove is the 1 of needle length
Times；Insulating materials is Acrylnitrile-Butadiene-Styrene；The polymer nanofiber spun is with obtaining in step (1)
Spun-bonded non-woven fabrics base material is received, and obtains the composite filtering material of uniform deposition Static Spinning polymer nanofiber on base material；
(3) preparation of superfine nano fiber dispersion
The polyvinyl butyral solution that Solute mass fraction is 0.1% is first prepared, polyvinyl butyral solution is prepared
Solvent for use is n-butanol；Prepare and gather used in the solubility parameter and electrostatic spinning fiber of polyvinyl butyral solution solvent for use
The solubility parameter numerical value difference 6 of compound, then it added in high speed beater carry out with superfine nano fiber polystyrene
Scattered, the rotating speed of high speed beater is 5000 revs/min, obtains uniform superfine nano fiber dispersion, superfine nano fiber
Mass fraction shared by nanofiber is 0.01% in dispersion liquid；Superfine nano fibre diameter is 10nm, and length is 100nm；
(4) composite filtering material immersion treatment
Composite filtering material is soaked in superfine nano fiber dispersion and taken out after 5min, is hung in baking oven, 25 DEG C of drying,
Obtain the filtrate that composite filtering material fiber surface deposits superfine nano fiber；As lamination material；Answering after immersion treatment
The superfine nano fiber deposit thickness for closing filter material surface is 20nm；
(5) step (1)~(4) are repeated 4 times, namely obtain 4 lamination materials, the filter efficiency of every lamination material
It can be determined by the electrostatic spinning time in rate-determining steps (2).The spinning time is respectively 5min, 6min, 7min and 9min, correspondence
Every lamination be respectively 20.1442% to the filter efficiency value of 0.02~10 μm of particle with material, 22.6656%,
24.3764% and 26.5243%；
(6) by lamination material, it is overlapped compound, is often laminated successively from low to high by media filtration efficiency from bottom to top
Layer material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer
All it is spun-bonded non-woven fabrics layer with the bottom；Adjacent two layers lamination material, above one layer of filter efficiency value be following one layer 1.1
Times, the lamination material superposition number of plies is 4 layers, forms spun-bonded non-woven fabrics and with the spaced interlayer of electret effect nanofiber
Structure, is made nanofiber/spun-bonded non-woven fabrics composite filter material, as shown in Fig. 2 wherein, 4 be spun-bonded non-woven fabrics, and 5 be electrostatic
Spinning nano fibre；Nanofiber/spun-bonded non-woven fabrics composite filter material reaches to the filter efficiency of 0.02~10 μm of particle
99.999%, pressure drag is maintained at 16Pa, and as shown in figure 3, obtained electrostatic spinning fiber/glass fibre composite filter paper have it is good
Good Charge Storage Stability, filter effect maintenance is good.
Embodiment 5
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, is concretely comprised the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) nanometer activated carbon fiber is added in ethanol, and ultrasonic disperse, uniform dispersion liquid is obtained, wherein, dispersion liquid
Middle fiber quality fraction is 1%, and soak time is 8min；The a diameter of 100nm of nanometer activated carbon fiber, length is 300nm；
B) take out, hang in baking oven, 60 DEG C after spun-bonded non-woven fabrics are soaked in the dispersion liquid of nanometer activated carbon fiber
Drying, obtains the spun-bonded non-woven fabrics base material of surface deposition of titanium oxide nanofiber or nanometer activated carbon fiber.Wherein, spunbond without
Cloth is spun, it is 40 μm that it, which constitutes fibre diameter, and non-woven fabrics aperture size is 35 μm, and grammes per square metre is 40g/m2, exhibits initial filtration efficiency is
20%；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles titanium dioxide is added in DMF, and ultrasonic disperse 60 minutes, obtain
The dispersed dispersion liquid of nano particle；
B) polymer polysulfones is added in dispersion liquid, magnetic agitation 10 hours, is configured to uniform and stable spinning solution,
Wherein, the mass fraction of polysulfones is 10%, and the addition of inorganic nanoparticles is polymer and inorganic nanoparticles gross mass
5%；
C) spinning solution is subjected to Multi needle electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：Supply voltage
20KV, spinning environment condition is 18 DEG C of temperature, relative humidity 35%, spinning solution rate of flooding 4mL/h；Multi needle spinneret unit pin
Head spacing 10cm, spinneret unit syringe needle quantity is 20；Insulated between the syringe needle of Multi needle electrostatic spinning, wherein, Needle sharing
Same insulating base；Insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between syringe needle；Specially
Insulating materials formation isolation groove is with the surrounding of syringe needle, being shaped as isolation groove is square, and the depth of isolation groove is needle length
2 times；Insulating materials is PET；The polymer nanofiber spun is with the spunbond obtained in step (1)
Non-woven fabrics base material is received, and obtains the composite filtering material of uniform deposition Static Spinning polymer nanofiber on spun-bonded non-woven fabrics；
(3) preparation of superfine nano fiber dispersion
The polyvinyl butyral solution that Solute mass fraction is 2.5% is first prepared, polyvinyl butyral solution is prepared
Solvent for use is ethanol；The solubility parameter of polyvinyl butyral solution solvent for use is prepared with used in electrostatic spinning fiber to polymerize
The solubility parameter numerical value difference 5 of thing, then adds the mixture of itself and superfine nano fiber polystyrene and polyester at a high speed
Disperseed in beater, wherein the mass ratio of polystyrene and polyester is 1:1, the rotating speed of high speed beater is 5000 revs/min
Clock, obtaining mass fraction shared by nanofiber in uniform superfine nano fiber dispersion, superfine nano fiber dispersion is
2.5%；Superfine nano fibre diameter is 80nm, and length is 150nm；
(4) composite filtering material immersion treatment
Composite filtering material is soaked in superfine nano fiber dispersion and taken out after 15min, is hung in baking oven, 35 DEG C of bakings
It is dry, obtain the filtrate that composite filtering material fiber surface deposits superfine nano fiber；As lamination material；After immersion treatment
The superfine nano fiber deposit thickness on composite filtering material surface is 80nm；
(5) step (1)~(4) are repeated 3 times, namely obtain 3 layers of lamination material, the filtering effect of every lamination material
Rate can be determined by the electrostatic spinning time in rate-determining steps (2).The spinning time is respectively 8min, 9.5min and 11min, correspondence
Every lamination with material be respectively to the filter efficiency value of 0.02~10 μm of particle 30.1248%, 31.6015% and
33.0743%；
(6) by lamination material, it is overlapped compound, is often laminated successively from low to high by media filtration efficiency from bottom to top
Layer material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer
All it is spun-bonded non-woven fabrics layer with the bottom；Adjacent two layers lamination material, above one layer of filter efficiency value be following one layer
1.05 times, the lamination material superposition number of plies is 3 layers, forms spun-bonded non-woven fabrics with having electret effect nanofiber spaced
Sandwich, is made nanofiber/spun-bonded non-woven fabrics composite filter material；Nanofiber/spun-bonded non-woven fabrics composite filter material
To the filter efficiency of 0.02~10 μm of particle up to 99.999%, pressure drag is maintained at 23Pa, and as shown in figure 3, what is obtained is quiet
Electrospinning fibre/glass fibre composite filter paper has good Charge Storage Stability, and filter effect maintenance is good.
Embodiment 6
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, is concretely comprised the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) titanium dioxide nanofiber is added in ethanol, and ultrasonic disperse, uniform dispersion liquid is obtained, wherein, disperse
Mass fraction is 1% to fiber altogether in liquid, and soak time is 8min；The a diameter of 80nm of titanium dioxide nanofiber, length
For 200nm；
B) take out, hang in baking oven, 55 after spun-bonded non-woven fabrics are soaked in the dispersion liquid of titanium dioxide nanofiber
DEG C drying, obtain surface deposition of titanium oxide nanofiber spun-bonded non-woven fabrics base material.Wherein, spun-bonded non-woven fabrics, it constitutes fine
A diameter of 32 μm are tieed up, non-woven fabrics aperture size is 20 μm, and grammes per square metre is 145g/m2, exhibits initial filtration efficiency is 35%；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles titanium dioxide is added in DMF, and ultrasonic disperse 45 minutes, obtain
The dispersed dispersion liquid of nano particle；
B) polymer polyvinylidene fluoride-tetrafluoroethylene-perfluoro methyl vinyl ether is added in dispersion liquid, magnetic agitation 8
Hour, uniform and stable spinning solution is configured to, wherein, the matter of Kynoar-tetrafluoroethylene-perfluoro methyl vinyl ether
It is 18% to measure fraction, and the addition of inorganic nanoparticles is the 3% of polymer and inorganic nanoparticles gross mass；
C) spinning solution is subjected to Multi needle electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：Supply voltage
55KV, spinning environment condition is 20 DEG C of temperature, relative humidity 30%, spinning solution rate of flooding 5mL/h；Multi needle spinneret unit pin
Head spacing 6cm, spinneret unit syringe needle quantity is 18；Insulated between the syringe needle of Multi needle electrostatic spinning, wherein, Needle sharing is same
One insulating base；Insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between syringe needle；Specially exist
The surrounding of syringe needle is with insulating materials formation isolation groove, and being shaped as isolation groove is square, and the depth of isolation groove is the 2 of needle length
Times；Insulating materials is PET；The polymer nanofiber spun is with the spunbond nonwoven obtained in step (1)
Cloth base material is received, and obtains the composite filtering material of uniform deposition Static Spinning polymer nanofiber on spun-bonded non-woven fabrics；
(3) preparation of superfine nano fiber dispersion
The polyvinyl butyral solution that Solute mass fraction is 3% is first prepared, polyvinyl butyral solution institute is prepared
It is methyl ethyl ketone with solvent；Prepare used in the solubility parameter and electrostatic spinning fiber of polyvinyl butyral solution solvent for use
The solubility parameter numerical value difference 5 of polymer, it then added to enter in high speed beater with superfine nano fiber polystyrene
Row is scattered, and the rotating speed of high speed beater is 5000 revs/min, obtains uniform superfine nano fiber dispersion, and superfine nano is fine
It is 3.5% to tie up mass fraction shared by nanofiber in dispersion liquid；Superfine nano fibre diameter is 60nm, and length is 70nm；
(4) composite filtering material immersion treatment
Composite filtering material is soaked in superfine nano fiber dispersion and taken out after 20min, is hung in baking oven, 40 DEG C of bakings
It is dry, obtain the filtrate that composite filtering material fiber surface deposits superfine nano fiber；As lamination material；After immersion treatment
The superfine nano fiber deposit thickness on composite filtering material surface is 60nm；
(5) step (1)~(4) are repeated 2 times, namely obtain 2 layers of lamination material, the filtering effect of every lamination material
Rate can be determined by the electrostatic spinning time in rate-determining steps (2).The spinning time is respectively 15min and 17min, corresponding every
Lamination is respectively 54.1062% and 63.9901% to the filter efficiency value of 0.02~10 μm of particle with material；
(6) by lamination material, it is overlapped compound, is often laminated successively from low to high by media filtration efficiency from bottom to top
Layer material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer
All it is spun-bonded non-woven fabrics layer with the bottom；Adjacent two layers lamination material, above one layer of filter efficiency value be following one layer 1.2
Times, the lamination material superposition number of plies is 2 layers, forms spun-bonded non-woven fabrics and with the spaced interlayer of electret effect nanofiber
Structure, is made nanofiber/spun-bonded non-woven fabrics composite filter material；Nanofiber/spun-bonded non-woven fabrics composite filter material pair
The filter efficiency of 0.02~10 μm of particle is up to 99.999%, and pressure drag is maintained at 21Pa, and as shown in figure 3, obtained electrostatic
Spinning fiber/glass fibre composite filter paper has good Charge Storage Stability, and filter effect maintenance is good.
Embodiment 7
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, is concretely comprised the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) titanium dioxide nanofiber is added in ethanol, and ultrasonic disperse, uniform dispersion liquid is obtained, wherein, disperse
Fiber quality fraction is 5% in liquid, and soak time is 10min；The a diameter of 70nm of titanium dioxide nanofiber, length is
150nm；
B) take out, hang in baking oven, 50 after spun-bonded non-woven fabrics are soaked in the dispersion liquid of titanium dioxide nanofiber
DEG C drying, obtain surface deposition of titanium oxide nanofiber spun-bonded non-woven fabrics base material.Wherein, spun-bonded non-woven fabrics, it constitutes fine
A diameter of 30 μm are tieed up, non-woven fabrics aperture size is 43 μm, and grammes per square metre is 50g/m2, exhibits initial filtration efficiency is 15%；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles titanium dioxide is added in solvent, and ultrasonic disperse 40 minutes, obtain nano particle uniform
Scattered dispersion liquid；
B) mixture of polymer polyvinylidene fluoride and polybutylene terephthalate is added in dispersion liquid, wherein poly- inclined
The mass ratio of PVF and polybutylene terephthalate is 1:1, magnetic agitation 8 hours is configured to uniform and stable spinning
Solution, wherein, the mass fraction of the mixture of Kynoar and polybutylene terephthalate two kinds of polymer is 25%, nothing
The addition of machine nano particle is the 2.5% of polymer and inorganic nanoparticles gross mass；
C) spinning solution is subjected to Multi needle electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：Supply voltage
60KV, spinning environment condition is 25 DEG C of temperature, relative humidity 40%, spinning solution rate of flooding 2mL/h；Multi needle spinneret unit pin
Head spacing 4cm, spinneret unit syringe needle quantity is 50；Insulated between the syringe needle of Multi needle electrostatic spinning, wherein, Needle sharing is same
One insulating base；Insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between syringe needle；Specially exist
The surrounding of syringe needle is with insulating materials formation isolation groove, and being shaped as isolation groove is square, and the depth of isolation groove is the 2 of needle length
Times；Insulating materials is PET；The polymer nanofiber spun with the spunbond obtained by step (1) without
Spin cloth base material to receive, obtain the composite filtering material of uniform deposition Static Spinning polymer nanofiber on spun-bonded non-woven fabrics base material；
(3) preparation of superfine nano fiber dispersion
The polyvinyl butyral solution that Solute mass fraction is 3.2% is first prepared, polyvinyl butyral solution is prepared
Solvent for use is the mixture of normal propyl alcohol, DAA and ethanol, and wherein the mass ratio of normal propyl alcohol, DAA and ethanol is 1:
2:1；Prepare the solubility of polymer used in the solubility parameter and electrostatic spinning fiber of polyvinyl butyral solution solvent for use
Parameter values difference 5, then it added disperseed in high speed beater with superfine nano filled nylon 6, high speed beater
Rotating speed be 5500 revs/min, obtain nanofiber in uniform superfine nano fiber dispersion, superfine nano fiber dispersion
Shared mass fraction is 4%；Superfine nano fibre diameter is 90nm, and length is 100nm；
(4) composite filtering material immersion treatment
Composite filtering material is soaked in the superfine nano fiber dispersion and taken out after 16min, is hung in baking oven, 25 DEG C
Drying, obtains the filtrate that composite filtering material fiber surface deposits superfine nano fiber；As lamination material；After immersion treatment
The composite filtering material surface superfine nano fiber deposit thickness be 28nm；
(5) step (1)~(4) are repeated 5 times, namely obtain 5 layers of lamination material, the filtering effect of every lamination material
Rate can be determined by the electrostatic spinning time in rate-determining steps (2).The spinning time be respectively 6min, 7.5min, 10min,
12.5min and 15min, corresponding lamination is respectively to the filter efficiency value of 0.02~10 μm of particle with material
22.52351%th, 23.7671%, 25.5739%, 27.7328%, 29.9331%；
(6) by lamination material, it is overlapped compound, is often laminated successively from low to high by media filtration efficiency from bottom to top
Layer material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer
All it is spun-bonded non-woven fabrics layer with the bottom；Adjacent two layers lamination material, above one layer of filter efficiency value be following one layer
1.08 times, the lamination material superposition number of plies is 5 layers, forms spun-bonded non-woven fabrics with having electret effect nanofiber spaced
Sandwich, is made nanofiber/spun-bonded non-woven fabrics composite filter material；Nanofiber/spun-bonded non-woven fabrics composite filter material
To the filter efficiency of 0.02~10 μm of particle up to 99.999%, pressure drag is maintained at 23Pa, and as shown in figure 3, what is obtained is quiet
Electrospinning fibre/glass fibre composite filter paper has good Charge Storage Stability, and filter effect maintenance is good.
Embodiment 8
A kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, is concretely comprised the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) nanometer activated carbon fiber is added in ethanol, and ultrasonic disperse, uniform dispersion liquid is obtained, wherein, dispersion liquid
Middle fiber quality fraction is 3%, and soak time is 8min；The a diameter of 90nm of nanometer activated carbon fiber, length is 250nm；
B) take out, hang in baking oven, 54 DEG C after spun-bonded non-woven fabrics are soaked in the dispersion liquid of nanometer activated carbon fiber
Drying, obtains the spun-bonded non-woven fabrics base material that surface deposits nanometer activated carbon fiber.Wherein, it is 30 μm, nothing that it, which constitutes fibre diameter,
It is 100 μm to spin cloth aperture size, and grammes per square metre is 140g/m2, exhibits initial filtration efficiency is 15%；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles titanium dioxide is added in solvent, and ultrasonic disperse 45 minutes, obtain nano particle uniform
Scattered dispersion liquid；
B) mixture of polymer polyurethane, fluorinated polyurethane and polysulfones is added in dispersion liquid, polyurethane, the poly- ammonia of fluorination
The mass ratio of ester and polysulfones is 1：2：1, magnetic agitation 8 hours is configured to uniform and stable spinning solution, wherein, polyurethane,
The mass fraction of the mixture of fluorinated polyurethane and polysulfones is 30%, and the additions of inorganic nanoparticles is polymer and inorganic receives
The 6.5% of rice grain gross mass；
C) spinning solution is subjected to Multi needle electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：Supply voltage
50KV, spinning environment condition is 10 DEG C of temperature, relative humidity 40%, spinning solution rate of flooding 3mL/h；Multi needle spinneret unit pin
Head spacing 10cm, spinneret unit syringe needle quantity is 25；Insulated between the syringe needle of Multi needle electrostatic spinning, wherein, Needle sharing
Same insulating base；Insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between syringe needle；Specially
Insulating materials formation isolation groove is with the surrounding of syringe needle, being shaped as isolation groove is square, and the depth of isolation groove is needle length
2 times；Insulating materials is PET；Spinning of the polymer nanofiber spun obtained by step (1)
Bonded non-woven fabrics base material is received, and obtains the composite filtering material of uniform deposition Static Spinning polymer nanofiber on spun-bonded non-woven fabrics base material；
(3) preparation of superfine nano fiber dispersion
The polyvinyl butyral solution that Solute mass fraction is 0.1% is first prepared, polyvinyl butyral solution is prepared
Solvent for use is the mixture of ethanol and normal propyl alcohol, and wherein the mass ratio of ethanol and normal propyl alcohol is 2:1；Prepare polyvinyl alcohol contracting fourth
The solubility parameter of aldehyde solution solvent for use differs 5 with the solubility parameter numerical value of polymer used in electrostatic spinning fiber, then will
Disperseed in itself and the mixture addition high speed beater of superfine nano fiber polystyrene, polyester and polyvinyl acetate, its
In, the mass ratio of polystyrene, polyester and polyvinyl acetate is 2:1:1, the rotating speed of high speed beater is 5500 revs/min, is obtained
To uniform superfine nano fiber dispersion, mass fraction shared by nanofiber is 4.0% in superfine nano fiber dispersion；It is super
Thin nanofiber diameter is 70nm, and length is 105nm；
(4) composite filtering material immersion treatment
Composite filtering material is soaked in superfine nano fiber dispersion and taken out after 12min, is hung in baking oven, 45 DEG C of bakings
It is dry, obtain the filtrate that composite filtering material fiber surface deposits superfine nano fiber；As lamination material；After immersion treatment
The superfine nano fiber deposit thickness on composite filtering material surface is 60nm；
(5) step (1)~(3) are repeated 6 times, namely obtain 6 layers of lamination material, the filtering effect of every lamination material
Rate can be determined by the electrostatic spinning time in rate-determining steps (2).The spinning time be respectively 5min, 5.5min, 6min,
8.5min, 10min and 11min, corresponding lamination material are distinguished the filter efficiency value of the particle of 0.02~10 μm of the mistake of grain
For 20.2158%, 20.9103%, 21.7903%, 22.8130%, 23.7562% and 24.7810%；
(6) by lamination material, it is overlapped compound, is often laminated successively from low to high by media filtration efficiency from bottom to top
Layer material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer
All it is spun-bonded non-woven fabrics layer with the bottom；Adjacent two layers lamination material, above one layer of filter efficiency value be following one layer
1.03 times, the lamination material superposition number of plies is 6 layers, forms spun-bonded non-woven fabrics with having electret effect nanofiber spaced
Sandwich, is made nanofiber/spun-bonded non-woven fabrics composite filter material；Nanofiber/spun-bonded non-woven fabrics composite filter material
To the filter efficiency of 0.02~10 μm of particle up to 99.999%, pressure drag is maintained at 28Pa, and as shown in figure 3, what is obtained is quiet
Electrospinning fibre/glass fibre composite filter paper has good Charge Storage Stability, and filter effect maintenance is good.
Embodiment 9-56 preparation processes be the same as Example 4, wherein solution parameter, technological parameter and composite filter material performance ginseng
Number is as shown in table 1-6：
Table 1：
Table 2：
Table 3：
Table 4：
Table 5：
Table 6：
Embodiment 56-69 preparation processes be the same as Example 5, wherein solution parameter, technological parameter and composite filter material performance
Parameter is as shown in table 7-8：
Table 7：
Table 8：
Embodiment 70-78 preparation processes be the same as Example 6, wherein solution parameter, technological parameter and composite filter material performance
Parameter is as shown in table 9-10：
Table 9
Table 10：
Claims (9)
1. a kind of nanofiber/spun-bonded non-woven fabrics composite filter material preparation method, it is characterized in that concretely comprising the following steps：
(1) spun-bonded non-woven fabrics pre-treatment
Step is：
A) titanium dioxide nanofiber or nanometer activated carbon fiber are added in ethanol, and ultrasonic disperse, uniformly disperseed
Liquid；
B) drying is taken out after spun-bonded non-woven fabrics are soaked in the dispersion liquid of titanium dioxide nanofiber or nanometer activated carbon fiber,
Obtain the spun-bonded non-woven fabrics base material of surface deposition of titanium oxide nanofiber or nanometer activated carbon fiber；
(2) electrostatic spinning
Step is：
A) inorganic nanoparticles are added in solvent, and ultrasonic disperse, obtain the dispersed dispersion liquid of nano particle；
B) polymer is added in the dispersion liquid, is configured to uniform and stable spinning solution；
C) spinning solution is carried out insulating between Multi needle electrostatic spinning, the syringe needle of the Multi needle electrostatic spinning；That is spun is poly-
Compound nanofiber is received with spun-bonded non-woven fabrics base material, obtains uniform deposition Static Spinning polymer nanocomposite on spun-bonded non-woven fabrics base material
The composite filtering material of fiber；
(3) preparation of superfine nano fiber dispersion
Polyvinyl butyral solution is first prepared, then it is added with superfine nano fiber and disperseed in high speed beater,
Obtain uniform superfine nano fiber dispersion；
(4) composite filtering material immersion treatment
Taken out after the composite filtering material is soaked in the superfine nano fiber dispersion, drying obtains composite filtering material fiber
Surface deposits the filtrate of superfine nano fiber；As lamination material；
The superfine nano fiber deposit thickness on the composite filtering material surface after immersion treatment is 20~200nm；
Test obtains filter efficiency value of the lamination material to 0.02~10 μm of particle；
(5) step (1)~(4) are repeated several times, the lamination material of different filter efficiencies is obtained；
(6) by lamination material, it is overlapped compound, the use per layer laminate successively from low to high by media filtration efficiency from bottom to top
Material makes to have the one of electrostatic spinning fiber upwardly, and covers a spun-bonded non-woven fabrics in most last layer surface, it is ensured that top layer and most
Bottom is all spun-bonded non-woven fabrics layer；Adjacent two layers lamination material, above one layer of filter efficiency to 0.02~10 μm of particle
It is worth 1.03~1.3 times for following one layer, forms the spun-bonded non-woven fabrics interlayer spaced with having electret effect nanofiber
Structure, is made nanofiber/spun-bonded non-woven fabrics composite filter material.
2. a kind of nanofiber according to claim 1/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In, in step (1), in titanium dioxide nanofiber or the nanometer activated carbon fiber dispersion liquid, fiber quality fraction be 0.1~
5%, soak time is 5~10min；A diameter of 50~the 100nm of titanium dioxide nanofiber or nanometer activated carbon fiber, it is long
Spend for 100~300nm；The spun-bonded non-woven fabrics, it is 1~50 μm that it, which constitutes fibre diameter, and non-woven fabrics aperture size is 5~120 μ
M, grammes per square metre is 10~300g/m2, exhibits initial filtration efficiency is 5%~40%；The drying refers to hang in baking oven, and temperature is 50
~60 DEG C；
In step (2), in the spinning solution, the concentration of polymer is 5~40wt%, and the addition of inorganic nanoparticles is poly-
0.1~10wt% of compound and inorganic nanoparticles gross mass；
The inorganic nanoparticles be silica, alundum (Al2O3), zinc oxide, barium monoxide, titanium dioxide, tantalum pentoxide,
Barium titanate, lead zirconate titanate, silicon nitride, tourmaline, boehmite or silsesquioxane nano particle；
The polymer is Kynoar, polybutylene terephthalate, PET, polyarylate, poly-vinegar
Sour ethene, nylon 6, polymethyl methacrylate, polyaniline, polyethylene glycol oxide, polyvinylpyrrolidone, polyacrylonitrile, gather oneself
Lactone, polyurethane, fluorinated polyurethane, polysulfones, polyether sulfone, Kynoar-hexafluoropropene, Kynoar-tetrafluoroethene-complete
One kind in methyl fluoride vinyl ethers, Kynoar-CTFE, or be the mixture of several polymer above；
Wherein described solvent is corresponded to respectively according to type of polymer：
Kynoar：N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl acetamide, triethyl phosphate and diformazan
Base sulfoxide；
Polybutylene terephthalate：Dichloromethane, tetrahydrofuran, chloroform or acetone；
PET：Dichloromethane, tetrahydrofuran, chloroform or acetone；
Polyarylate：Dichloromethane, tetrahydrofuran, chloroform or acetone；
Polyvinyl acetate：Toluene, acetone, ethanol, acetic acid, ethyl acetate or chloroform；
Nylon 6：Formic acid；
Polymethyl methacrylate：Chloroform, acetic acid, ethyl acetate, acetone or toluene；
Polyaniline：N,N-dimethylformamide or 1-METHYLPYRROLIDONE；
Polyethylene glycol oxide：N,N-dimethylformamide, ethanol, water or chloroform；
Polyvinylpyrrolidone：Water, ethanol, DMAC N,N' dimethyl acetamide or N,N-dimethylformamide；
Polyacrylonitrile：N,N-dimethylformamide or dimethyl sulfoxide (DMSO)；
Polycaprolactone：N,N-dimethylformamide or acetone；
Polyurethane：N,N-dimethylformamide, acetone or 1-METHYLPYRROLIDONE；
Fluorinated polyurethane：N,N-dimethylformamide, acetone or 1-METHYLPYRROLIDONE；
Polysulfones and polyether sulfone：N,N-dimethylformamide, acetone, 1-METHYLPYRROLIDONE, dimethyl acetamide or tetrahydrofuran；
Kynoar-hexafluoropropene：N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl acetamide, tricresyl phosphate second
Ester or dimethyl sulfoxide (DMSO)；
Kynoar-tetrafluoroethylene-perfluoro methyl vinyl ether：N,N-dimethylformamide, 1-METHYLPYRROLIDONE, diformazan
Yl acetamide, triethyl phosphate or dimethyl sulfoxide (DMSO)；
Kynoar-CTFE：N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl acetamide, tricresyl phosphate
Ethyl ester or dimethyl sulfoxide (DMSO)；
In the step a) of electrostatic spinning, the ultrasonic disperse time is 20~70 minutes；
In the step b) of electrostatic spinning, after polymer is added in the dispersion liquid, magnetic agitation 8~10 hours；
In the step c) of electrostatic spinning, the process conditions of Multi needle electrostatic spinning are：10~60KV of supply voltage, spinning environment bar
Part is 15~35 DEG C of temperature, relative humidity 25~90%；Multi needle spinneret unit syringe needle 2~30cm of spacing, spinneret unit syringe needle
Quantity is 6~90.
3. a kind of nanofiber according to claim 1/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In in step (3), Solute mass fraction is 0.1~5% in the polyvinyl butyral solution；The preparation polyvinyl alcohol
Butyral solution solvent for use is tetrahydrofuran, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, acetone, chloroform, first
Phenol, dimethyl sulfoxide (DMSO), ethanol, normal propyl alcohol, isopropanol, n-butanol, DAA, methyl acetate, ethyl acetate, butyl acetate,
One or more of mixtures in toluene, 1-METHYLPYRROLIDONE, MEK, methyl ethyl ketone；The preparation polyvinyl alcohol
The solubility parameter of butyral solution solvent for use is at least differed with the solubility parameter numerical value of polymer used in electrostatic spinning fiber
4, the wherein unit of solubility parameter is (J/cm3)1/2；
Mass fraction shared by nanofiber is 0.01%~5% in the superfine nano fiber dispersion；The superfine nano is fine
A diameter of 10~150nm is tieed up, length is 100~150nm；
The material of the superfine nano fiber is polystyrene, polyester, polyvinyl acetate, nylon 6, nylon66 fiber, polymethyl
One or two kinds of in sour methyl esters, polyaniline, polyethylene glycol oxide, polyacrylonitrile, polycaprolactone, polyurethane, polysulfones, polyether sulfone
And the mixture of above polymer；
The rotating speed of the high speed beater is 5000 revs/min~8000 revs/min.
4. a kind of nanofiber according to claim 1/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In in step (4), the time of the immersion is 5~30min；The drying refers to hang in baking oven, 25~50 DEG C of drying.
5. a kind of nanofiber according to claim 1/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In in step (5), the multiplicating refers to repeat 2~6 times, namely obtains 2~6 lamination materials.
6. a kind of nanofiber according to claim 1/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In the same insulating base of Needle sharing.
7. a kind of nanofiber according to claim 6/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In insulation refers to carry out anti-tampering isolation processing to each syringe needle using insulating materials between the syringe needle；Specially described
The surrounding of syringe needle is with insulating materials formation isolation groove, completely cuts off the square or circle that is shaped as of groove, the depth of isolation groove is institute
State needle length 1~5 times.
8. a kind of nanofiber according to claim 7/spun-bonded non-woven fabrics composite filter material preparation method, its feature exists
In, the insulating materials be Acrylnitrile-Butadiene-Styrene, makrolon, polymethyl methacrylate, polypropylene,
Polyamide, polystyrene, polyvinyl chloride, polyethylene, polytetrafluoroethylene (PTFE), Kynoar or PET.
9. such as a kind of nanofiber according to any one of claims 1 to 8/spun-bonded non-woven fabrics composite filter material preparation method
Obtained nanofiber/spun-bonded non-woven fabrics composite filter material, it is characterized in that：Nanofiber/the spun-bonded non-woven fabrics are combined
Filtering material is that gradient is laminated composite filtering material, for lamination material is entered successively from low to high by media filtration efficiency from bottom to top
Row superimposion is formed, and makes to have the one of electrostatic spinning fiber per layer laminate material upwardly, and in the covering of most last layer surface
One spun-bonded non-woven fabrics, it is ensured that top layer and the bottom are all spun-bonded non-woven fabrics layer；Adjacent two layers lamination material, above one layer it is right
The filter efficiency value of 0.02~10 μm of particle is 1.03~1.3 times of following one layer, and the lamination material superposition number of plies is 2~6
Layer, formed spun-bonded non-woven fabrics with the spaced sandwich of electret effect nanofiber, be made nanofiber/spunbond without
Spin cloth composite filter material；The nanofiber/filtering of the spun-bonded non-woven fabrics composite filter material to 0.02~10 μm of particle
Efficiency up to 99.999% and more than, pressure drag is maintained at 10~30Pa.
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