CN107497182A - A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof - Google Patents

A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof Download PDF

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Publication number
CN107497182A
CN107497182A CN201710706839.0A CN201710706839A CN107497182A CN 107497182 A CN107497182 A CN 107497182A CN 201710706839 A CN201710706839 A CN 201710706839A CN 107497182 A CN107497182 A CN 107497182A
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polymer
filtering material
composite nano
nano fiber
photocatalysis
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CN107497182B (en
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丁彬
廖亚龙
李玉瑶
赵兴雷
印霞
俞建勇
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Donghua University
National Dong Hwa University
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Donghua University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8634—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/103—Agents inhibiting growth of microorganisms
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/52—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated carboxylic acids or unsaturated esters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/0216—Bicomponent or multicomponent fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/025—Types of fibres, filaments or particles, self-supporting or supported materials comprising nanofibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Biomedical Technology (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
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  • Multicomponent Fibers (AREA)

Abstract

The present invention relates to a kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, described filtering material, including supporting layer and it is attached to the Nanofiber filter layer of support layer surface, layers of nanofibers is uniformly filled with photochemical catalyst and antiseptic, and preparation method comprises the following steps：1) preparation of spinning solution：By the dispersed electrostatic spinning solution for forming dispersion liquid in a solvent, high polymer formation stable uniform being added after supersound process of a certain amount of photochemical catalyst and antiseptic；2) electrostatic spinning, electrospinning parameters is set, realize that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle using electrostatic spinning；3) use recycling design steam to carry out slightly soluble processing to composite nano fiber filtering material surface with certain rate of release, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.The present invention efficiently solves existing electrostatic spinning syringe needle/susceptible to plugging problem of shower nozzle outlet end, is used directly for the decomposition of organic pollution under visible ray, inactivation of microbial pathogens etc., is provided simultaneously with the strainability of brilliance.

Description

A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and its system Preparation Method
Technical field
The present invention relates to a kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently, more particularly to one Kind preparation method, i.e., realize that polymer solution spun is drawn at solid metal silk tip using electrostatic spinning with combined type syringe needle Silk is stretched out, while uses recycling design steam to be carried out with certain rate of release to composite nano fiber filtering material surface at slightly soluble Reason, belongs to function filtering material field.
Background technology
Haze and PM2.5 have been to be concerned by more and more people and paid attention to, and the source of haze and harm are also increasingly by people It is known.Interior is except the air pollution sources such as PM2.5, the also volatile organic matter such as formaldehyde, benzene and bacterium, virus, fungi etc. Pollutant, greatly endangered to human body health care belt.Therefore requirement of the people to filtering material except intercept fine particle beyond the region of objective existence, It is also desirable that it possesses the functions such as bacterium, fungi and the microorganism decomposed in the organic pollutions such as indoor formaldehyde, killing air.Due to The reasons such as a large amount of uses of the relative closure, air-conditioning of indoor environment, the increase of ski dome easily grow various bacteriums, true Bacterium and microorganism.
Patent of invention " nano antiseptic material-polysulphone composite microporous filter film and preparation method thereof " (CN200510051363.9), the miillpore filter is the nano anti-biotic material group with mixing by the polysulfones being dissolved in selected solvent Into, with dry/wetting phase conversion method knifing, film forming in immersion coagulating bath, but its nano anti-biotic material is easy to fall off；Patent of invention is " a kind of Graphene oxide/polymer composite antibacterial material and preparation method thereof " (CN201610588724.1), it is on polymeric matrix Graphene oxide antimicrobial coating, polymeric matrix after activation is immersed in coupling agent solution after soaking and eluted with deionized water Composite antibacterial material is obtained afterwards and after naturally dry, but the binding strength between its antibiotic layer and matrix is not apparent；Utility model Patent " a kind of delicate fragrance type antimicrobial filtering material " (CN201520335153.1) provides a kind of impurity that can be adsorbed in air Grain and dust, and the delicate fragrance type antimicrobial filtering material of antibacterial functions is accompanied with, anti-bacterial fibre layer is the antibacterial for scribbling antiseptic Layer, but its filter effect to fine particles such as PM2.5 is not high, and antibiotic layer binding strength is not high.
The content of the invention
The purpose of the present invention is：Effectively solves existing electrostatic spinning syringe needle/susceptible to plugging problem of shower nozzle outlet end, to first Aldehyde, amine and toluene all have good photocatalysis efficiency and inhibited to bacterium, virus and microorganism, are provided simultaneously with Remarkable strainability.
In order to achieve the above object, the technical scheme is that providing a kind of composite Nano with photo-catalysis function The preparation method of fiber filter material, it is characterised in that comprise the following steps：
1) preparation of spinning solution：Dispersion liquid is formed in a solvent by a certain amount of photochemical catalyst and antiseptic are dispersed, is surpassed The electrostatic spinning solution that high polymer forms stable uniform is added after sonication；
2) electrostatic spinning：Electrospinning parameters are set, realize that spinning polymer is molten with combined type syringe needle using electrostatic spinning Liquid carries out stretching wire vent at solid metal silk tip；
3) recycling design steam is used to be carried out with certain rate of release to composite nano fiber filtering material surface at slightly soluble Reason, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Preferably, the solvent be formic acid, tetrahydrofuran, water, DMF, DMA, Acetone, chloroform, cresols, dimethyl sulfoxide (DMSO), methanol, ethanol, propyl alcohol, isopropanol, butanol, isobutanol, toluene, N- crassitudes One kind in ketone, MEK, or two kinds and two or more mixtures.
Preferably, the mass concentration of the electrostatic spinning solution is respectively：
Polymer is nylon 6, and the mass concentration of polymer solution is 4-10%；
Polymer is polyurethane, and the mass concentration of polymer solution is 6-18%；
Polymer is Kynoar, and the mass concentration of polymer solution is 18-25%；
Polymer is polybutylene terephthalate, and the mass concentration of polymer solution is 19-25%；
Polymer is PET, and the mass concentration of polymer solution is 20-25%；
Polymer is polyarylate, and the mass concentration of polymer solution is 20-25%；
Polymer is polyvinyl acetate, and the mass concentration of polymer solution is 8-12%；
Polymer is polyvinyl alcohol, and the mass concentration of polymer solution is 6-13%；
Polymer is polymethyl methacrylate, and the mass concentration of polymer solution is 3-9%；
Polymer is polyaniline, and the mass concentration of polymer solution is 10-18%；
Polymer is polyethylene glycol oxide, and the mass concentration of polymer solution is 11-18%；
Polymer is polyvinylpyrrolidone, and the mass concentration of polymer solution is 6-14%；
Polymer is polyacrylonitrile, and the mass concentration of polymer solution is 15-22%；
Polymer is polycaprolactone, and the mass concentration of polymer solution is 16-19%；
Polymer is polyethylene glycol, and the mass concentration of polymer solution is 5-14%；
Polymer is polyvinyl butyral resin, and the mass concentration of polymer solution is 20-25%；
Polymer is polysulfones, and the mass concentration of polymer solution is 15-25%.
Preferably, the photochemical catalyst is one kind in titanium dioxide, zinc oxide, tin oxide, zirconium dioxide, cadmium sulfide, Particle diameter is 10~80nm, and photocatalyst concentrations are 0.5~5wt%.
Preferably, the antiseptic includes：
1) inorganic antiseptic such as silver ion class, zinc oxide, cupric oxide, ammonium dihydrogen phosphate, lithium carbonate；
2) anilid class, imidazoles, thiazoles, isothiazolone derivative, quaternary ammonium salt, double croak classes, phenols etc. are organic Antiseptic；
3) natural antibacterial agent such as chitin, mustard, castor oil, horseradish；
Antiseptic addition is 0.05~1wt%.
Preferably, it is to utilize ultrasonic wave separating apparatus 20~120min of thermostatic ultrasonic to be ultrasonically treated described in step 1), ultrasound 20~40kHz of frequency, 20~80 DEG C of ultrasonic temperature, power 200W.
Preferably, it is characterised in that electrospinning parameters are arranged in step 2)：5~80kV of voltage, reception distance 10~ 80cm, 0.075~10mL/h of rate of flooding, 17~32 DEG C of temperature, relative humidity 18~80%.
Preferably, electrostatic spinning described in step 2) with combined type syringe needle by hollow stainless steel syringe needle and belt discharge tip Stainless steel needle mount forms.
Preferably, the specific method of the step 3) is：
Recovered solvent steam is discharged using solvent vapor recovery device, composite nano fiber filtering material surface is entered The processing of row slightly soluble, the photochemical catalyst and antiseptic part that will be attached to nanofiber surface be exposed, and rate of release is 0.5~ 10L/min。
Another technical scheme of the present invention there is provided a kind of composite nano fiber mistake for having photocatalysis/antibacterial functions concurrently Filter material material, it is characterised in that be prepared using above-mentioned preparation method, including supporting layer and be attached to receiving for support layer surface Rice fibrous filter layer, layers of nanofibers are uniformly filled with photochemical catalyst and antiseptic, are 0.25~10 μm of particle to particle diameter Filter efficiency be 85~99.999%, resistance pressure drop be the organic gas such as 5~80Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia clearance >= 95%, staphylococcus aureus (gram-positive bacteria), Escherichia coli, Carlos Kleiber Salmonella (Gram-negative bacteria), white are read Sterilizing rate >=97% of pearl bacterium, Pseudomonas aeruginosa etc..
Preferably, the supporting layer is polypropylene, polyethylene, polyvinyl chloride, polyethylene terephthalate, fiber One kind in element, polyacrylonitrile, polyamide, polyester, wire, carbon fiber or glass, aperture be 1~500 μm, grammes per square metre be 10~ 300g/m2。
Preferably, the layers of nanofibers be nylon 6, it is polyurethane, Kynoar, polybutylene terephthalate, poly- PETP, polyarylate, polyvinyl acetate, polyvinyl alcohol, polymethyl methacrylate, polyaniline, polyoxyethylene One kind in alkene, polyvinylpyrrolidone, polyacrylonitrile, polycaprolactone, polyethylene glycol, polyvinyl butyral resin, polysulfones, or It is the mixture of any two or three of polymer in above polymer.
Beneficial effect：
(1) present invention realizes that polymer solution spun enters at solid metal silk tip using electrostatic spinning with combined type syringe needle Row stretching wire vent, efficiently solves the deficiencies of existing electrostatic spinning is easily blocked with syringe needle/shower nozzle outlet end, improves the unit interval The liquid outlet quantity of interior spinning solution, greatly improve the spinning speed of electrostatic spinning；
(2) present invention uses recycling design steam to be carried out with certain rate of release to composite nano fiber filtering material surface Slightly soluble processing, by the effective recycling of solvent waste gas, the photochemical catalyst/antiseptic part that will be attached to nanofiber surface is sudden and violent Expose, effectively decompose the organic pollutions such as indoor formaldehyde, kill bacterium, fungi and microbial pathogens etc. in air；
(3) nano-fiber material has the advantages that fibre diameter is thin, aperture is small, specific surface area is big, fully material can be made to exist While keeping filtration efficiency, there is relatively low resistance pressure drop, so as to meet that the performance of composite nano materials efficient low-resistance will Ask.
Brief description of the drawings
Fig. 1 is a kind of scanning electron microscope (SEM) photograph for the composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently of the present invention.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Fixed scope.
Embodiment 1
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By titanium dioxide optical catalyst (addition 0.5wt%, particle diameter 10nm) and silver ion class antibacterial Agent (addition 0.5wt%) is dispersed in formic acid, formed dispersion liquid, using ultrasonic wave separating apparatus (supersonic frequency 40kHz, 80 DEG C of ultrasonic temperature) after ultrasonic agitation 20min, nylon 6 (weight average molecular weight be 50,000) is added in dispersion liquid, used after sealing Magnetic stirring apparatus continuously stirs 15 hours, is finally prepared into stabilization, the polymer dope that uniform mass concentration is 10%；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 60kV, distance 25cm, rate of flooding 3.2mL/h are received, temperature 24 DEG C of degree, relative humidity 43%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 0.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polypropylene that supporting layer, which receives base material, Non-woven fabrics, grammes per square metre 100g/m2, aperture size is 300 μm；Nanofiber composition of layer is nylon 6, fibre diameter 80nm, gram Weight is 6g/m2.Gained has the composite nano fiber filtering materials of photocatalysis/antibacterial functions concurrently to that particle diameter is 0.25~10 μm The filter efficiency of grain is that the clearance of the organic gas such as 87%, resistance pressure drop 5Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 97%.
Embodiment 2
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By titanium dioxide optical catalyst (addition 1wt%, particle diameter 15nm) and zinc oxide antiseptic (addition 0.1wt%) is dispersed in DMA, forms dispersion liquid, utilizes ultrasonic wave separating apparatus (ultrasound Frequency 40kHz, 70 DEG C of ultrasonic temperature) after ultrasonic agitation 30min, polyurethane (weight average molecular weight be 80,000) is added to dispersion liquid In, continuously stirred 8 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration be 15% it is poly- Compound spinning solution；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 57kV, receive distance 30cm, rate of flooding 2mL/h, temperature 26 DEG C, relative humidity 48%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 1L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is cellulose that supporting layer, which receives base material, Non-woven fabrics, grammes per square metre 70g/m2, aperture size is 250 μm；Nanofiber composition of layer is polyurethane, fibre diameter 100nm, gram Weight is 5g/m2.Gained has the composite nano fiber filtering materials of photocatalysis/antibacterial functions concurrently to that particle diameter is 0.25~10 μm The filter efficiency of grain is that the clearance of the organic gas such as 98%, resistance pressure drop 60Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 98.3%.
Embodiment 3
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By titanium dioxide optical catalyst (addition 1.5wt%, particle diameter 18nm) and copper oxide anti-bacteria agent (addition 0.8wt%) is dispersed in DMF, forms dispersion liquid, utilizes ultrasonic wave separating apparatus (ultrasound Frequency 35kHz, 50 DEG C of ultrasonic temperature) after ultrasonic agitation 40min, Kynoar (weight average molecular weight be 320,000) is added to point In dispersion liquid, continuously stirred 9 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration is 18% Polymer dope；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 40kV, distance 25cm, rate of flooding 0.5mL/h are received, temperature 24 DEG C of degree, relative humidity 30%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 1.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polytetrafluoro that supporting layer, which receives base material, Ethene non-woven fabrics, grammes per square metre 60g/m2, aperture size is 150 μm；Nanofiber composition of layer is Kynoar, and fibre diameter is 200nm, grammes per square metre 8g/m2.Gained have concurrently the composite nano fiber filtering materials of photocatalysis/antibacterial functions be 0.25 to particle diameter~ The filter efficiency of 10 μm of particle is that the clearance of the organic gas such as 96.6%, resistance pressure drop 24Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 97.4%.
Embodiment 4
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By photocatalyst of zinc oxide (addition 2wt%, particle diameter 20nm) and biphosphate ammonium antimicrobial agent (addition 0.4wt%) is dispersed in tetrahydrofuran, is formed dispersion liquid, is utilized ultrasonic wave separating apparatus (supersonic frequency 30kHz, 40 DEG C of ultrasonic temperature) after ultrasonic agitation 50min, polybutylene terephthalate (weight average molecular weight be 120,000) is added Into dispersion liquid, continuously stirred 8 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration is 23% polymer dope；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 55kV, receive distance 30cm, rate of flooding 2mL/h, temperature 26 DEG C, relative humidity 48%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 2L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polypropylene that supporting layer, which receives base material, Non-woven fabrics, grammes per square metre 120g/m2, aperture size is 350 μm；Nanofiber composition of layer is polybutylene terephthalate, fiber A diameter of 300nm, grammes per square metre 15g/m2.Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently to particle diameter Filter efficiency for 0.25~10 μm of particle is 89%, resistance pressure drop 14Pa, and the organic gas such as PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is gone Except rate is 95.2%.
Embodiment 5
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By photocatalyst of zinc oxide (addition 2.4wt%, particle diameter 12nm) and lithium carbonate antiseptic (addition 0.2wt%) is dispersed in dichloromethane, is formed dispersion liquid, is utilized ultrasonic wave separating apparatus (supersonic frequency 30kHz, 35 DEG C of ultrasonic temperature) after ultrasonic agitation 60min, PET (weight average molecular weight be 40,000) is added Into dispersion liquid, continuously stirred 10 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration is 25% polymer dope；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 35kV, distance 15cm, rate of flooding 0.2mL/h are received, temperature 22 DEG C of degree, relative humidity 28%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 2.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, supporting layer receive base material be polypropylene/ Polyethylene nonwoven, grammes per square metre 120g/m2, aperture size is 350 μm；Nanofiber composition of layer is poly terephthalic acid second two Ester, fibre diameter 400nm, grammes per square metre 20g/m2.Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently The filter efficiency for particle diameter being 0.25~10 μm of particle is 86%, resistance pressure drop 5Pa, the organic gas such as PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia Clearance be 95.3%.
Embodiment 6
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By photocatalyst of zinc oxide (addition 4wt%, particle diameter 22nm) and anilid class antiseptic (addition 0.05wt%) is dispersed in chloroform, is formed dispersion liquid, is utilized ultrasonic wave separating apparatus (supersonic frequency 25kHz, 35 DEG C of ultrasonic temperature) after ultrasonic agitation 70min, polyarylate (weight average molecular weight be 110,000) is added in dispersion liquid, Continuously stirred 12 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, the polymerization that uniform mass concentration is 21% Thing spinning solution；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 65kV, receive distance 30cm, rate of flooding 4mL/h, temperature 25 DEG C, relative humidity 45%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 3L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polychlorostyrene second that supporting layer, which receives base material, Alkene non-woven fabrics, grammes per square metre 200g/m2, aperture size is 320 μm；Nanofiber composition of layer is polyarylate, and fibre diameter is 320nm, grammes per square metre 30g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is 0.25 to particle diameter The filter efficiency of~10 μm of particle is that the clearance of the organic gas such as 94%, resistance pressure drop 34Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 95.7%.
Embodiment 7
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By tin oxide photochemical catalyst (addition 2.4wt%, particle diameter 30nm) and imidazoles antiseptic (addition 0.25wt%) is dispersed in acetic acid, forms dispersion liquid, (supersonic frequency 20kHz, is surpassed using ultrasonic wave separating apparatus 30 DEG C of sound temperature) after ultrasonic agitation 80min, polyvinyl acetate (weight average molecular weight be 140,000) is added in dispersion liquid, sealed Continuously stirred 6 hours with magnetic stirring apparatus afterwards, be finally prepared into stabilization, the polymer spinning that uniform mass concentration is 9% Liquid；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 38kV, distance 18cm, rate of flooding 0.2mL/h are received, temperature 22 DEG C of degree, relative humidity 28%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 3.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polychlorostyrene second that supporting layer, which receives base material, Alkene non-woven fabrics, grammes per square metre 200g/m2, aperture size is 320 μm；Nanofiber composition of layer is polyvinyl acetate, and fibre diameter is 190nm, grammes per square metre 27g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is 0.25 to particle diameter The filter efficiency of~10 μm of particle is that the clearance of the organic gas such as 94%, resistance pressure drop 39Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 97.7%.
Embodiment 8
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By tin oxide photochemical catalyst (addition 0.8wt%, particle diameter 80nm) and thiazoles antiseptic (addition 0.3wt%) is dispersed in water, forms dispersion liquid, utilizes ultrasonic wave separating apparatus (supersonic frequency 20kHz, ultrasound 30 DEG C of temperature) after ultrasonic agitation 90min, polyvinyl alcohol (weight average molecular weight be 40,000) is added in dispersion liquid, magnetic is used after sealing Power agitating device continuously stirs 13 hours, is finally prepared into stabilization, the polymer dope that uniform mass concentration is 12%；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 65kV, receive distance 30cm, rate of flooding 4mL/h, temperature 25 DEG C, relative humidity 45%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 4L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is cellulose that supporting layer, which receives base material, Non-woven fabrics, grammes per square metre 120g/m2, aperture size is 330 μm；Nanofiber composition of layer is polyvinyl alcohol, and fibre diameter is 240nm, grammes per square metre 34g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is 0.25 to particle diameter The filter efficiency of~10 μm of particle is that the clearance of the organic gas such as 92%, resistance pressure drop 22Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 96.2%.
Embodiment 9
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By tin oxide photochemical catalyst (addition 1.9wt%, particle diameter 43nm) and isothiazolone derivative Antiseptic (addition 1wt%) is dispersed in chloroform, is formed dispersion liquid, is utilized ultrasonic wave separating apparatus (supersonic frequency 25kHz, 20 DEG C of ultrasonic temperature) after ultrasonic agitation 100min, polymethyl methacrylate (weight average molecular weight be 140,000) is added Into dispersion liquid, continuously stirred 10 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration is 7% polymer dope；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 38kV, distance 18cm, rate of flooding 0.2mL/h are received, temperature 22 DEG C of degree, relative humidity 28%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 4.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is cellulose that supporting layer, which receives base material, Non-woven fabrics, grammes per square metre 120g/m2, aperture size is 330 μm；Nanofiber composition of layer is polymethyl methacrylate, and fiber is straight Footpath is 80nm, grammes per square metre 6g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is to particle diameter The filter efficiency of 0.25~10 μm of particle is the removal of the organic gas such as 90%, resistance pressure drop 16Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia Rate is 96%.
Embodiment 10
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By zirconium dioxide photochemical catalyst (addition 5wt%, particle diameter 10nm) and quaternary ammonium salt antiseptic (addition 0.7wt%) is dispersed in DMF, forms dispersion liquid, utilizes ultrasonic wave separating apparatus (ultrasound Frequency 25kHz, 25 DEG C of ultrasonic temperature) after ultrasonic agitation 110min, polyaniline (weight average molecular weight be 70,000) is added to dispersion liquid In, continuously stirred 7 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration be 14% it is poly- Compound spinning solution；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 65kV, receive distance 30cm, rate of flooding 4mL/h, temperature 25 DEG C, relative humidity 45%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, supporting layer receive base material be polyester without Spin cloth, grammes per square metre 80g/m2, aperture size is 440 μm；Nanofiber composition of layer is polyaniline, fibre diameter 70nm, grammes per square metre For 8g/m2.Gained has the composite nano fiber filtering materials of photocatalysis/antibacterial functions concurrently to particle that particle diameter is 0.25~10 μm Filter efficiency be that the clearance of the organic gas such as 89.4%, resistance pressure drop 9Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 95%.
Embodiment 11
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By zirconium dioxide photochemical catalyst (addition 2.6wt%, particle diameter 56nm) and double croak class antiseptics (addition 0.9wt%) is dispersed in ethanol, forms dispersion liquid, (supersonic frequency 30kHz, is surpassed using ultrasonic wave separating apparatus 30 DEG C of sound temperature) after ultrasonic agitation 120min, polyethylene glycol oxide (weight average molecular weight be 300,000) is added in dispersion liquid, sealed Continuously stirred 15 hours with magnetic stirring apparatus afterwards, be finally prepared into stabilization, the polymer spun that uniform mass concentration is 18% Silk liquid；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 50kV, receive distance 23cm, rate of flooding 1mL/h, temperature 24 DEG C, relative humidity 43%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 5.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, supporting layer receive base material be polyester without Spin cloth, grammes per square metre 80g/m2, aperture size is 440 μm；Nanofiber composition of layer is polyethylene glycol oxide, fibre diameter 80nm, Grammes per square metre is 9g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is 0.25~10 μm to particle diameter The filter efficiency of particle is that the clearance of the organic gas such as 92%, resistance pressure drop 45Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 95.3%.
Embodiment 12
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By zirconium dioxide photochemical catalyst (addition 4wt%, particle diameter 20nm) and chitin antibacterial agent (addition 0.35wt%) is dispersed in ethanol, forms dispersion liquid, (supersonic frequency 30kHz, is surpassed using ultrasonic wave separating apparatus 40 DEG C of sound temperature) after ultrasonic agitation 110min, polyvinylpyrrolidone (weight average molecular weight be 90,000) is added in dispersion liquid, Continuously stirred 9 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, the polymer that uniform mass concentration is 13% Spinning solution；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 70kV, receive distance 34cm, rate of flooding 3mL/h, temperature 26 DEG C, relative humidity 45%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 6L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, supporting layer receive base material be polyester without Spin cloth, grammes per square metre 90g/m2, aperture size is 470 μm；Nanofiber composition of layer is polyvinylpyrrolidone, and fibre diameter is 88nm, grammes per square metre 9.7g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is 0.25 to particle diameter The filter efficiency of~10 μm of particle is that the clearance of the organic gas such as 95%, resistance pressure drop 30Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 96.1%.
Embodiment 13
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：Cadmium sulfide photochemical catalyst (addition 3wt%, particle diameter 50nm) and castor oil antiseptic (are added Dosage 0.45wt%) it is dispersed in DMA, dispersion liquid is formed, utilizes ultrasonic wave separating apparatus (supersonic frequency Rate 35kHz, 50 DEG C of ultrasonic temperature) after ultrasonic agitation 100min, polyacrylonitrile (weight average molecular weight be 60,000) is added to dispersion liquid In, continuously stirred 8 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration be 20% it is poly- Compound spinning solution；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 50kV, distance 27cm, rate of flooding 1.4mL/h are received, temperature 24 DEG C of degree, relative humidity 49%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 6.5L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is glass fibre yarn that supporting layer, which receives base material, Net, grammes per square metre 150g/m2, aperture size is 800 μm；Nanofiber composition of layer is polyacrylonitrile, fibre diameter 130nm, gram Weight is 30g/m2.The composite nano fiber filtering material that gained has photocatalysis/antibacterial functions concurrently is 0.25~10 μm to particle diameter The filter efficiency of particle is that the clearance of the organic gas such as 98%, resistance pressure drop 64Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 96.8%.
Embodiment 14
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：By cadmium sulfide photochemical catalyst (addition 1wt%, 10~80nm of particle diameter) and horseradish antiseptic (addition 0.5wt%) is dispersed in DMF, forms dispersion liquid, utilizes ultrasonic wave separating apparatus (ultrasound Frequency 35kHz, 60 DEG C of ultrasonic temperature) after ultrasonic agitation 90min, polysulfones (weight average molecular weight be 80,000) is added in dispersion liquid, Continuously stirred 11 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, the polymerization that uniform mass concentration is 24% Thing spinning solution；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 70kV, distance 40cm, rate of flooding 2.5mL/h are received, temperature 25 DEG C of degree, relative humidity 45%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 7L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is glass fibre yarn that supporting layer, which receives base material, Net, grammes per square metre 120g/m2, aperture size is 600 μm；Nanofiber composition of layer is polysulfones, and fibre diameter 110nm, grammes per square metre are 26g/m2.Gained has the composite nano fiber filtering materials of photocatalysis/antibacterial functions concurrently to particle that particle diameter is 0.25~10 μm Filter efficiency be that the clearance of the organic gas such as 99%, resistance pressure drop 67Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 98.3%.
Embodiment 15
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：Cadmium sulfide photochemical catalyst (addition 1.2wt%, particle diameter 70nm) and mustard antiseptic (are added Dosage 0.6wt%) it is dispersed in water, dispersion liquid is formed, utilizes ultrasonic wave separating apparatus (supersonic frequency 40kHz, ultrasonic temperature 70 DEG C) after ultrasonic agitation 80min, polyethylene glycol (weight average molecular weight be 80,000) is added in dispersion liquid, stirred after sealing with magnetic force Mix device to continuously stir 12 hours, be finally prepared into stabilization, the polymer dope that uniform mass concentration is 10%；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 50kV, distance 26cm, rate of flooding 0.6mL/h are received, temperature 23 DEG C of degree, relative humidity 40%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 8L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polyester yarn that supporting layer, which receives base material, Net, grammes per square metre 50g/m2, aperture size is 300 μm；Nanofiber composition of layer is polyethylene glycol, fibre diameter 220nm, grammes per square metre For 34g/m2.Gained has the composite nano fiber filtering materials of photocatalysis/antibacterial functions concurrently to that particle diameter is 0.25~10 μm The filter efficiency of grain is that the clearance of the organic gas such as 99.9%, resistance pressure drop 70Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia is 98%.
Embodiment 16
A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof, preparation method bag Include following steps：
1) preparation of spinning solution：Cadmium sulfide photochemical catalyst (addition 3.6wt%, particle diameter 35nm) and phenolic antiseptic (are added Dosage 0.8wt%) it is dispersed in DMF, dispersion liquid is formed, utilizes ultrasonic wave separating apparatus (supersonic frequency 40kHz, 80 DEG C of ultrasonic temperature) after ultrasonic agitation 70min, polyvinyl butyral resin (weight average molecular weight be 30,000) is added to first In acid, continuously stirred 15 hours with magnetic stirring apparatus after sealing, be finally prepared into stabilization, uniform mass concentration is 23wt% Polymer dope；
2) electrostatic spinning：The polymer dope prepared is sucked in spinneret module by liquid feed device, utilizes electrostatic Spinning realizes that polymer solution spun carries out stretching wire vent at solid metal silk tip with combined type syringe needle；
The process conditions of wherein electrostatic spinning are：Spinning voltage 80kV, distance 40cm, rate of flooding 1.8mL/h are received, temperature 25 DEG C of degree, relative humidity 47%；
3) post-process：Recovered solvent steam is discharged using solvent vapor recovery device, with certain rate of release to multiple Close nanofiber filtration material surface and carry out slightly soluble processing, the photochemical catalyst part that will be attached to nanofiber surface exposes Come, rate of release 9L/min, produce the final composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently.
Gained has the composite nano fiber filtering material of photocatalysis/antibacterial functions concurrently, including supporting layer and is attached to support The Nanofiber filter layer of layer surface, layers of nanofibers are uniformly filled with photochemical catalyst, and it is polyester yarn that supporting layer, which receives base material, Net, grammes per square metre 70g/m2, aperture size is 320 μm；Nanofiber composition of layer is polyvinyl butyral resin, and fibre diameter is 80nm, grammes per square metre 6g/m2.Gained have concurrently the composite nano fiber filtering materials of photocatalysis/antibacterial functions be 0.25 to particle diameter~ The filter efficiency of 10 μm of particle is the clearance of the organic gas such as 99.999%, resistance pressure drop 75Pa, PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia For 99%.

Claims (12)

1. a kind of preparation method of the composite nano fiber filtering material with photo-catalysis function, it is characterised in that including following Step：
1) preparation of spinning solution：Dispersion liquid is formed in a solvent by a certain amount of photochemical catalyst and antiseptic are dispersed, at ultrasound The electrostatic spinning solution that high polymer forms stable uniform is added after reason；
2) electrostatic spinning：Electrospinning parameters are set, realize that polymer solution spun exists with combined type syringe needle using electrostatic spinning Solid metal silk tip carries out stretching wire vent；
3) recycling design steam is used to carry out slightly soluble processing to composite nano fiber filtering material surface with certain rate of release, i.e., Obtain the composite nano fiber filtering material for finally having photocatalysis/antibacterial functions concurrently.
A kind of 2. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that the solvent is formic acid, tetrahydrofuran, water, DMF, DMA, Acetone, chloroform, cresols, dimethyl sulfoxide (DMSO), methanol, ethanol, propyl alcohol, isopropanol, butanol, isobutanol, toluene, N- crassitudes One kind in ketone, MEK, or two kinds and two or more mixtures.
A kind of 3. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that the mass concentration of the electrostatic spinning solution is respectively：
Polymer is nylon 6, and the mass concentration of polymer solution is 4-10%；
Polymer is polyurethane, and the mass concentration of polymer solution is 6-18%；
Polymer is Kynoar, and the mass concentration of polymer solution is 18-25%；
Polymer is polybutylene terephthalate, and the mass concentration of polymer solution is 19-25%；
Polymer is PET, and the mass concentration of polymer solution is 20-25%；
Polymer is polyarylate, and the mass concentration of polymer solution is 20-25%；
Polymer is polyvinyl acetate, and the mass concentration of polymer solution is 8-12%；
Polymer is polyvinyl alcohol, and the mass concentration of polymer solution is 6-13%；
Polymer is polymethyl methacrylate, and the mass concentration of polymer solution is 3-9%；
Polymer is polyaniline, and the mass concentration of polymer solution is 10-18%；
Polymer is polyethylene glycol oxide, and the mass concentration of polymer solution is 11-18%；
Polymer is polyvinylpyrrolidone, and the mass concentration of polymer solution is 6-14%；
Polymer is polyacrylonitrile, and the mass concentration of polymer solution is 15-22%；
Polymer is polycaprolactone, and the mass concentration of polymer solution is 16-19%；
Polymer is polyethylene glycol, and the mass concentration of polymer solution is 5-14%；
Polymer is polyvinyl butyral resin, and the mass concentration of polymer solution is 20-25%；
Polymer is polysulfones, and the mass concentration of polymer solution is 15-25%.
A kind of 4. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that the photochemical catalyst is one kind in titanium dioxide, zinc oxide, tin oxide, zirconium dioxide, cadmium sulfide, Particle diameter is 10~80nm, and photocatalyst concentrations are 0.5~5wt%.
A kind of 5. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that the antiseptic includes inorganic antiseptic, organic antibacterial agent and natural antibacterial agent, antiseptic addition For 0.05~1wt%.
A kind of 6. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that it is to utilize ultrasonic wave separating apparatus 20~120min of thermostatic ultrasonic to be ultrasonically treated described in step 1), ultrasound 20~40kHz of frequency, 20~80 DEG C of ultrasonic temperature, power 200W.
A kind of 7. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that electrospinning parameters are arranged in step 2)：5~80kV of voltage, receive 10~80cm of distance, perfusion 0.075~10mL/h of speed, 17~32 DEG C of temperature, relative humidity 18~80%.
A kind of 8. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that electrostatic spinning described in step 2) is with combined type syringe needle by hollow stainless steel syringe needle and belt discharge tip Stainless steel needle mount composition.
A kind of 9. preparation of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 1 Method, it is characterised in that the specific method of the step 3) is：
Recovered solvent steam is discharged using solvent vapor recovery device, composite nano fiber filtering material surface is carried out micro- Molten processing, the photochemical catalyst and antiseptic part that will be attached to nanofiber surface are exposed, and rate of release is 0.5~10L/ min。
10. a kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently, it is characterised in that will using such as right The preparation method described in 1 is asked to be prepared, including supporting layer and the Nanofiber filter layer for being attached to support layer surface, Nanowire Dimension layer is uniformly filled with photochemical catalyst and antiseptic, and the filter efficiency for particle diameter being 0.25~10 μm of particle is 85~ 99.999%, resistance pressure drop is 5~80Pa, to clearance >=95% of organic gas, sterilizing rate >=97%.
11. a kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently according to claim 10, it is special Sign is that the supporting layer is polypropylene, polyethylene, polyvinyl chloride, polyethylene terephthalate, cellulose, polypropylene One kind in nitrile, polyamide, polyester, wire, carbon fiber or glass, aperture are 1~500 μm, and grammes per square metre is 10~300g/m2。
12. a kind of composite nano fiber filtering material with photo-catalysis function according to claim 10, its feature exist In the layers of nanofibers is nylon 6, polyurethane, Kynoar, polybutylene terephthalate, poly terephthalic acid second Diester, polyarylate, polyvinyl acetate, polyvinyl alcohol, polymethyl methacrylate, polyaniline, polyethylene glycol oxide, polyvinyl pyrrole One kind in alkanone, polyacrylonitrile, polycaprolactone, polyethylene glycol, polyvinyl butyral resin, polysulfones, or above polymer In any two or three of polymer mixture.
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