CN108295675A - A kind of antibacterial air filter film and preparation method thereof based on polyacrylonitrile/graphene oxide/tea polyphenol compound - Google Patents
A kind of antibacterial air filter film and preparation method thereof based on polyacrylonitrile/graphene oxide/tea polyphenol compound Download PDFInfo
- Publication number
- CN108295675A CN108295675A CN201810138322.0A CN201810138322A CN108295675A CN 108295675 A CN108295675 A CN 108295675A CN 201810138322 A CN201810138322 A CN 201810138322A CN 108295675 A CN108295675 A CN 108295675A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- polyacrylonitrile
- air filter
- filter film
- electrostatic spinning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/39—Electrospinning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Filtering Materials (AREA)
Abstract
The present invention discloses a kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, using non-woven fabrics as base material, the surface deposition of base material has a composite membrane that polyacrylonitrile/graphene oxide/tea polyphenol compound is formed, the polyacrylonitrile, graphene oxide, tea polyphenols mass ratio be（16‑30）︰（4‑10）︰（1‑16）.There is provided its corresponding preparation method simultaneously.The microstructure of antibacterial air filter film of the present invention is：Polyacrylonitrile（PAN）Nanofiber constitutes reticular structure aggregation staggeredly, between diameter is about 50 300nm, graphene oxide（GO）It is dispersed between PAN fiber between fiber and the crosspoint of fiber, the diameter distribution of GO is larger, is um grades, GO forms the structure that nanofiber is combined with micrometer laminar object with PAN.This structure can improve filter membrane thickness simultaneously, keep the voidage of filter membrane, improve membrane filtration efficiency, effectively keep the pressure drop of filter membrane, had PM2.5 effects in air filtering, and anti-microbial property is good.
Description
Technical field
The present invention relates to a kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound and its
Preparation method.
Background technology
In recent years, with the development of industrialization and urbanization, air pollution increasingly sharpens.Wherein, small in air
The residence time is long in air, propagation distance is remote by grain PM2.5, and can pass through the upper and lower respiratory tract of human body, is finally deposited on human body
Lung, or even blood is entered by lung, human body is caused a significant threat, respiratory disease, heart disease etc. can be caused, also may be used
Pregnant woman is set to have premature delivery risk.And air-filtering membrane can effectively remove the molecule in air, can be applied to respirator,
Indoor air cleaner, industrial gas purifying etc..Therefore, the environmental problem of getting worse makes people to the air that has excellent performance
The demand of filter membrane is increasingly sharpened.But a diameter of micron level of traditional filtering material fiber, gap too greatly cannot be effective
The molecule in air filtering is crossed, studies have shown that with the reduction of fibre diameter, the strainability of material gradually increases, and works as fibre
When a diameter of nanoscale of dimension, strainability of the material to PM2.5 can be significantly improved.Because of smaller gap and larger ratio
The area effect that surface area generates can the effective molecule crossed in air filtering.
Invention content
Present invention aims at provide a kind of antibacterial air based on polyacrylonitrile/graphene oxide/tea polyphenol compound
Filter membrane, while another goal of the invention that its corresponding preparation method is the present invention being provided.
Based on above-mentioned purpose, the present invention takes following technical scheme：
A kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, using non-woven fabrics as base material, base
The surface deposition of material has a composite membrane that polyacrylonitrile/graphene oxide/tea polyphenols is formed, the polyacrylonitrile, graphene oxide,
The mass ratio of tea polyphenols is（16-30）︰（4-10）︰（1-16）.
The thickness of the base material is 0.06-0.09mm, and the thickness of composite membrane is 0.02-0.05mm.
The method for preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, including it is following
Step：
1）The preparation of graphene oxide DMF dispersion liquids：A certain amount of DMF solution is added into graphene oxide water solution（N-N bis-
Methylformamide）, rotate, obtain graphene oxide DMF dispersion liquids；
2）The preparation of electrostatic spinning liquid：To step 1）Graphene oxide DMF dispersion liquids in add polyacrylonitrile successively and tea is more
Phenol mixes to obtain electrostatic spinning liquid；The polyacrylonitrile, graphene oxide, tea polyphenols, DMF solution mass ratio be（16-30）︰
（4-10）︰（1-16）︰ (75-194)；
3）The preparation of antibacterial air filter film：By step 2）Electrostatic spinning liquid the surface shape of base material is deposited on using method of electrostatic spinning
At composite membrane, antibacterial air filter film is obtained.
Step 3）Method of electrostatic spinning is：First base material is wound on the spinning axis of electrostatic spinning, then electrostatic spinning liquid is drawn
To electrostatic spinning is carried out in syringe pump, electrostatic spinning liquid deposits to the surface of base material and forms composite membrane, and the surface density of composite membrane is
2.5 -4.9 g/m2, obtain antibacterial air filter film.
Technological parameter when electrostatic spinning is：The syringe needle flow of electrostatic spinning voltage 20-24 kV, syringe pump are 0.1-0.4
ML/h, needle diameter are 0.8-1.2 mm, and spinning distance is 16-20 cm, and spinning temperature is 20-30 DEG C, relative humidity 30-
50%, the velocity of rotation for spinning axis is 500-700 r/h.
Step 2）The step of mixing includes magnetic agitation, ultrasonic disperse, and magnetic stirring speed is 60-160 r/min, stirring
Time is 4-12 h, and ultrasonic power is 8-12 KHz, and ultrasonic time is 1-3 h.
Step 1）When middle revolving, revolving temperature is 51-54 DEG C, and the speed of rotation is 80-120r/min, and relative degree of vacuum is
-0.095MPa。
Polyacrylonitrile (Polyacrylonitrile, PAN) has excellent weatherability, is placed for a long time still outdoor
Original intensity can be kept, in addition, polyacrylonitrile chemical stability is good, it can inorganic acid resistance, hydrogen peroxide and general organic examination
Agent.It takes method of electrostatic spinning to be applied to air-filtering membrane polyacrylonitrile fibre, recycling can be repeated several times.But Static Spinning
Silk prepares air filter film, and with the increase of filter membrane thickness, filter efficiency improves, and the pressure drop of filter membrane gradually increases, according to demonstration be by
Cause in the decline of voidage.
Graphene thin layer is two-dimensional layer nanostructure, carbon atom Sp2The monoatomic layer that hydridization is formed, can be in two-dimensional space
It is unlimited to extend, it is the network crystal structure of Hexagonal close arrangement.Graphene oxide (GO) is due to oxidation, on this basis
In the presence of oxygen-containing functional groups such as a large amount of-OH ,-COOH ,-C=O- ,-C-O-.Graphene oxide has stronger antibiotic property, can
Resist most of bacteriums.Graphene oxide, which is introduced into, prepares air-filtering membrane, prepares graphene oxide/polyacrylonitrile combined filtration
Film, the composite filtering film not only have stronger anti-microbial property, since graphene oxide has larger extension in two-dimensional space
Property, therefore, micron order, even grade material can be formed, one-dimensional nano line can be formed with polyacrylonitrile and mutually tied with two-dimensional layer
The nanostructure of conjunction, graphene oxide are introduced into the voidage increased in air filter film, while improving filter efficiency, energy
Enough significant pressure drops for reducing filter membrane, compensate for the deficiency of polyacrylonitrile.
Tea polyphenols (Tea Polyphenols, TP) are the more carboxyl phenolic compounds of one kind extracted from tealeaves, are one
The natural broad-spectrum antiseptic material of kind.For graphene oxide as anti-biotic material, dispersed permeability is limited, in order to increase air-filtering membrane
Anti-microbial property, a certain amount of tea polyphenols are added in electrostatic spinning liquid.
Compared with prior art, the invention has the advantages that：
1）The microstructure of antibacterial air filter film of the present invention is：Polyacrylonitrile（PAN）Nanofiber constitutes netted knot staggeredly
Structure aggregation constitutes mesh skeleton, between diameter is about 50-300nm, graphene oxide（GO）It is dispersed between PAN fiber
Between fiber and the crosspoint of fiber, the diameter distribution of GO is larger, is um grades, GO and PAN forms nanofiber and micron
The structure that nonwoven fabric from filaments is combined.GO has good electric conductivity, during electrostatic spinning, under the action of forceful electric power field force, and GO
It is mutually exclusive so that fiber and GO aggregations are loose.This structure can improve filter membrane thickness simultaneously, keep the voidage of filter membrane,
Therefore, while improving membrane filtration efficiency, the pressure drop of filter membrane is effectively kept.In addition, from the scanning electron microscope (SEM) photograph of filtration membrane
It can be seen that, the diameter for adding PAN nanofibers in the air filter film of GO is significantly smaller, mainly since the excellent electric conductivity of GO is led
It causes.Studies show that, when the diameter of air filter film reduces, air circulation is very fast, is conducive to the filtering effect for increasing air filter film
It answers.Tea polyphenols（TP）It is combined, is evenly distributed with PAN fiber completely, increase the anti-microbial property of air-filtering membrane.Air filter film
Macrostructure be：On a surface of non-woven fabrics, PAN/GO/TP composite membranes are the composite membrane uniform deposition of PAN/GO/TP compositions
Filtering material and anti-biotic material had PM2.5 effects in air filtering, and anti-microbial property is good；
2）The air filter film prepared using method of electrostatic spinning has high open porosity, high-specific surface area, permeability etc. excellent
Performance, preparation method are simple, easy to operate.
Description of the drawings
Fig. 1 is the electron scanning micrograph of the air filter film of embodiment 1；
Fig. 2 is anti-microbial property test result figure.
Specific implementation mode
Embodiment 1
A kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, using non-woven fabrics as base material, base
The surface deposition of material has the composite membrane that polyacrylonitrile/graphene oxide/tea polyphenol compound is formed, the polyacrylonitrile, oxidation
Graphene, tea polyphenols mass ratio be 16 ︰, 4 ︰ 8, the thickness of the base material is 0.07mm, and the thickness of composite membrane is 0.03mm.
The method for preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, including it is following
Step：
1）The preparation of graphene oxide DMF dispersion liquids：It is added into the graphene oxide aqueous dispersions of a concentration of 2 mg/ml of 50g
50g DMF solutions, obtain mixed dispersion liquid, and mixed liquor, which is placed in revolving to its quality in Rotary Evaporators, not to be substantially change
（It is to judge benchmark with the 0.1g of poor quality that is no more than of the last mixed liquor rotated twice of sampling observation, removes the water in mixed liquor）,
It is 53 DEG C to rotate temperature, and the speed of rotation is 80 r/min, and relative degree of vacuum is -0.095MPa, obtains a concentration of 3mg/ml oxidations stone
Black alkene DMF dispersion liquids；(revolving is to convert the aqueous dispersions of GO to the DMF dispersion liquids of GO, because of the boiling point of water and DMF solution
Different, so only having water that can be evaporated out in dispersion liquid when 53 degree, DMF solution will be in 58 degree of temperatures above
It can be evaporated out.)
2）The preparation of electrostatic spinning liquid：Take 20g steps 1）A concentration of 3mg/ml graphene oxides DMF dispersion liquids in add successively
2.4g polyacrylonitrile and 1.2g tea polyphenols, magnetic agitation, ultrasonic disperse obtain electrostatic spinning liquid, and magnetic stirring speed is 160 r/
Min, mixing time 4h, ultrasonic power 10KHz, ultrasonic time are 2 h；The polyacrylonitrile, graphene oxide, tea are more
Phenol, DMF solution mass ratio be 16 ︰, 4 ︰, 8 ︰ 105；
3）The preparation of antibacterial air filter film：By step 2）Electrostatic spinning liquid the surface shape of base material is deposited on using method of electrostatic spinning
At composite membrane, the surface density of composite membrane is 4.7 g/m2, base material is thickness 0.07mm, 42 g/m of surface density2Non-woven fabrics, ruler
Very little is the cm of 16cm × 14, obtains antibacterial air filter film；Method of electrostatic spinning is：First base material is wound on the spinning axis of electrostatic spinning, then
Electrostatic spinning liquid is drawn in syringe pump and carries out electrostatic spinning, electrostatic spinning liquid deposits to the surface of base material and forms composite membrane,
Obtain antibacterial air filter film.
Technological parameter when electrostatic spinning is：The syringe needle flow of 24 kV of electrostatic spinning voltage, syringe pump are 0.4 mL/h,
Needle diameter is 1.2 mm, and spinning distance is 20 cm, and spinning temperature is DEG C that relative humidity 50%, the velocity of rotation for spinning axis is
500 r/h。
The step 1 of embodiment 1-4）Middle graphene oxide aqueous dispersions are purchased from coal institute of the Chinese Academy of Sciences.
Embodiment 2
A kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, using non-woven fabrics as base material, base
The surface deposition of material has the composite membrane that polyacrylonitrile/graphene oxide/tea polyphenol compound is formed, the polyacrylonitrile, oxidation
Graphene, tea polyphenols mass ratio be 30 ︰, 10 ︰ 16.The thickness of the base material is 0.07mm, and the thickness of composite membrane is 0.03mm.
The method for preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, including it is following
Step：
1）The preparation of graphene oxide DMF dispersion liquids：It is added into the graphene oxide aqueous dispersions of a concentration of 2 mg/ml of 50g
50g DMF solutions, obtain mixed dispersion liquid, and mixed liquor, which is placed in revolving to its quality in Rotary Evaporators, not to be substantially change
（It is to judge benchmark with the 0.1g of poor quality that is no more than of the last mixed liquor rotated twice of sampling observation, removes the water in mixed liquor）,
It is 53 DEG C to rotate temperature, and the speed of rotation is 80 r/min, and relative degree of vacuum is -0.095MPa；Then revolving temperature is adjusted to 60
DEG C revolving（The wherein Solute mass of GO is improved, contents of the GO in air filter film is further increased）, obtain a concentration of 5mg/ml oxygen
Graphite alkene DMF dispersion liquids；
2）The preparation of electrostatic spinning liquid：Take 20g (density of DMF solution is 0.95g/mL in the present invention) step 1）It is a concentration of
Add 2.4g polyacrylonitrile and 1.2g tea polyphenols in 5mg/mL graphite alkene DMF dispersion liquids successively, magnetic agitation, ultrasonic disperse,
Electrostatic spinning liquid is obtained, magnetic stirring speed is 60 r/min, mixing time 12h, ultrasonic power 12KHz, ultrasonic time 3
h；The polyacrylonitrile, graphene oxide, tea polyphenols, DMF solution mass ratio be 30 ︰, 10 ︰, 16 ︰ 194；
3）The preparation of antibacterial air filter film：By step 2）Electrostatic spinning liquid the surface shape of base material is deposited on using method of electrostatic spinning
At composite membrane, the surface density of composite membrane is 4.7 g/m2, base material is thickness 0.07mm, 42 g/m of surface density2Non-woven fabrics, ruler
Very little is the cm of 16cm × 14, obtains antibacterial air filter film；Method of electrostatic spinning is：First base material is wound on the spinning axis of electrostatic spinning, then
Electrostatic spinning liquid is drawn in syringe pump and carries out electrostatic spinning, electrostatic spinning liquid deposits to the surface of base material and forms composite membrane,
Obtain antibacterial air filter film.
Technological parameter when electrostatic spinning is：The syringe needle flow of electrostatic spinning voltage 20kV, syringe pump are 0.1 mL/h, needle
A diameter of 0.8 mm, spinning distance are 20 cm, and spinning temperature is DEG C relative humidity 30%, and the velocity of rotation for spinning axis is
700 r/h。
Embodiment 3
A kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, using non-woven fabrics as base material, base
The surface deposition of material has the composite membrane that polyacrylonitrile/graphene oxide/tea polyphenol compound is formed, the polyacrylonitrile, oxidation
Graphene, tea polyphenols mass ratio be 16 ︰, 4 ︰ 4, the thickness of the base material is 0.07mm, and the thickness of composite membrane is 0.03mm.
The method for preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, including it is following
Step：
1）The preparation of graphene oxide DMF dispersion liquids：It is added into the graphene oxide aqueous dispersions of a concentration of 2mg/ml of 50g
50gDMF solution, obtains mixed dispersion liquid, and mixed dispersion liquid, which is placed in revolving to its quality in Rotary Evaporators, not to change（With
The 0.1g of poor quality that is no more than of the last mixed liquor rotated twice of sampling observation is to judge benchmark, removes the superfluous water in mixed liquor
Point）, revolving temperature is 53 DEG C, and the speed of rotation is 80 r/min, and relative degree of vacuum is -0.095MPa, obtains DMF points of graphene oxide
Dispersion liquid；
2）The preparation of electrostatic spinning liquid：Take 20g steps 1）A concentration of 3mg/ml graphene oxides DMF dispersion liquids in add successively
3.0g polyacrylonitrile and 1.2g tea polyphenols, magnetic agitation, ultrasonic disperse obtain electrostatic spinning liquid, and magnetic stirring speed is 160 r/
Min, mixing time 4h, ultrasonic power 10KHz, ultrasonic time are 2 h；The polyacrylonitrile, graphene oxide, tea are more
Phenol, DMF solution mass ratio be 16 ︰, 4 ︰, 4 ︰ 109；
3）The preparation of antibacterial air filter film：By step 2）Electrostatic spinning liquid the surface shape of base material is deposited on using method of electrostatic spinning
At composite membrane, the surface density of composite membrane is 4.7 g/m2, base material is thickness 0.07mm, 42 g/m of surface density2Non-woven fabrics, ruler
Very little is the cm of 16cm × 14, obtains antibacterial air filter film；Method of electrostatic spinning is：First base material is wound on the spinning axis of electrostatic spinning, then
Electrostatic spinning liquid is drawn in syringe pump and carries out electrostatic spinning, electrostatic spinning liquid deposits to the surface of base material and forms composite membrane,
Obtain antibacterial air filter film.
Technological parameter when electrostatic spinning is：The syringe needle flow of 24 kV of electrostatic spinning voltage, syringe pump are 0.4 mL/h,
Needle diameter is 1.2 mm, and spinning distance is 16 cm, and spinning temperature is 25 DEG C, and relative humidity 50% spins the velocity of rotation of axis
For 500 r/h.
Embodiment 4
A kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, using non-woven fabrics as base material, base
The surface deposition of material has the composite membrane that polyacrylonitrile/graphene oxide/tea polyphenol compound is formed, the polyacrylonitrile, oxidation
Graphene, tea polyphenols mass ratio be 16 ︰, 4 ︰ 2, the thickness of the base material is 0.07mm, and the thickness of composite membrane is 0.03mm.
The method for preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, including it is following
Step：
1）The preparation of graphene oxide DMF dispersion liquids：It is added into the graphene oxide water solution of a concentration of 2mg/ml of 50g
50gDMF solution, obtains mixed liquor, and mixed liquor, which is placed in revolving to its quality in Rotary Evaporators, not to be substantially change（With sampling observation
The 0.1g of poor quality that is no more than of the last mixed liquor rotated twice be judge benchmark, the excessive moisture in removal mixed liquor）, rotation
It is 53 DEG C to steam temperature, and the speed of rotation is 80 r/min, relative degree of vacuum -0.095MPa, obtains a concentration of 3mg/ml graphene oxides
DMF dispersion liquids；
2）The preparation of electrostatic spinning liquid：Take 20g steps 1）A concentration of 3mg/ml graphene oxides DMF dispersion liquids in add successively
2.4g polyacrylonitrile and 0.48g tea polyphenols, magnetic agitation, ultrasonic disperse obtain electrostatic spinning liquid, and magnetic stirring speed is 160 r/
Min, mixing time 4h, ultrasonic power 10KHz, ultrasonic time are 2 h；The polyacrylonitrile, graphene oxide, tea are more
Phenol, DMF solution mass ratio be 16 ︰, 4 ︰, 2 ︰ 111；
3）The preparation of antibacterial air filter film：By step 2）Electrostatic spinning liquid the surface shape of base material is deposited on using method of electrostatic spinning
At composite membrane, the surface density of composite membrane is 4.7 g/m2, base material is thickness 0.07mm, 42 g/m of surface density2Non-woven fabrics, ruler
Very little is the cm of 16cm × 14, obtains antibacterial air filter film；Method of electrostatic spinning is：First base material is wound on the spinning axis of electrostatic spinning, then
Electrostatic spinning liquid is drawn in syringe pump and carries out electrostatic spinning, electrostatic spinning liquid deposits to the surface of base material and forms composite membrane,
Obtain antibacterial air filter film.
Technological parameter when electrostatic spinning is：The syringe needle flow of 24 kV of electrostatic spinning voltage, syringe pump are 0.4 mL/h,
Needle diameter is 1.2 mm, and spinning distance is 20 cm, and spinning temperature is 25 DEG C, and relative humidity 30% spins the velocity of rotation of axis
For 500 r/h.
5 performance test of embodiment
5.1 scanning electron microscope analysis
Air filter film made from the embodiment of the present invention 1 is intercepted into suitable size, is pasted on copper nut using conducting resinl, is placed
Gold-plated processing is carried out in metal spraying device, the electron scanning micrograph of air filter film is shown in Fig. 1.
From fig. 1, it can be seen that the air filter film of the present invention is made of the graphene oxide of nanofiber and stratiform, wherein oxygen
Graphite alkene is distributed between bundles of nanofibers.
5.2 antibacterial test
Comparative example 1
PAN/GO composite membranes are made with reference to the preparation method of embodiment 1, the difference is that, step 2）It is more that 1.2g tea is not added
Phenol, other are the same as embodiment 1.PAN/GO composite membranes on air filter film are made.
Comparative example 2
PAN/GO composite membranes are made with reference to the preparation method of embodiment 1, the difference is that, step 2）It is middle to the pure DMF of 20g
2.4g polyacrylonitrile and 1.2g tea polyphenols are added successively in solution (density of DMF solution is 0.95 g/mL in the present invention), other
With embodiment 1, PAN/TP composite membranes on air filter film are thus made.
The preparation of inoculum in antibacterial test：10 g of peptone, yeast powder 5g, sodium chloride 10g is taken to be dissolved in 0.9L
Water in, until completely dissolved, its pH value is adjusted to 7.0 using the sodium hydroxide of 1N.Take 25 uL concentration 106 Cfu/mL is golden yellow
Color glucose coccus and Escherichia coli are uniformly coated on the culture dish containing culture solution in an aseptic environment, then will implement
The air filter film prepared in example 1 and comparative example 1 and 2 is cut into the circle of a diameter of 1.8 cm, and the filter membrane after cutting out is immersed in
In culture solution containing staphylococcus aureus and Escherichia coli.Under the conditions of 37 DEG C, 24 h are cultivated.Test result such as Fig. 2 institutes
Show.
As shown in Figure 2, when antibiotic property is tested, no apparent antibacterial ring size generates GO/PAN air filter films, it may be possible to due to
Dispersibilities of the GO in nanofiber causes, due to GO be scattered be distributed in PAN bundles of nanofibers between, existing for no GO
Place is without antibiotic property, therefore the anti-microbial property of GO/PAN air filter films is limited.TP/PAN air filter film antibacterial ring sizes are smaller, and TP/PAN is anti-
Bacterium limited capacity, it may be possible to since the diffusion of TP causes, although relative to GO, dispersions of the TP in PAN fiber is uniform,
It is the blocking of the cladding and gap due to fiber, the antibiotic property of TP/PAN air filter films is still poor.
And the GO/TP/PAN air filter films of the present invention have stronger anti-microbial property, under identical antibiotic property experiment condition,
The antibacterial ring size of GO/TP/PAN air filter films is significantly greater than TP/PAN air filter films.Thus it also turns out, GO/TP/PAN air filter films
Middle GO and TP has synergy in terms of anti-microbial property, wherein GO is dispersed between PAN, and layer structure can be that TP expands
It dissipates and channel is provided, TP disperses in PAN fiber inner homogeneous, ensures that fiber each section is provided with anti-microbial property, therefore both exists
When, play the role of mutually enhancing on anti-microbial property.And individually in the presence of GO, since dispersion diffusion is limited, without apparent antibacterial
Performance, independent TP are weaker since diffusivity is limited anti-microbial property.Therefore, air filter film produced by the present invention has good antibacterial
Effect.
5.3 strainabilities are tested
The air filter film of comparative example 1 and 2 in the air filter film sample and 5.2 that is prepared in embodiment 1 was carried out using TSI8130
Performance evaluation is filtered, uses grain size for the Nacl aerosol particles of 0.26um, test flow is 32 lpm, tests air filter film sample
Size be diameter 10cm circle.(universal method in document)
When test result shows that the strainability of GO/PAN air filter films is 99.997%, pressure drop 382Pa.TP/PAN air filters
With the increase of fiber filter performance, the pressure drop of air filter film gradually increases film, and when strainability is 99.994%, pressure drop is
525Pa, the PM2.5 being unfavorable in air pass through air filter film.
And GO/TP/PAN air filter films of the present invention not only have larger filter efficiency, smaller pressure drop, filter efficiency is
When 99.977 %, pressure drop is 169 Pa.In the case where adding GO, the diameter of PAN nanofibers obviously attenuates, the reason is that,
Addition GO can be such that the electric conductivity of spinning solution enhances, and influence the dielectric constant of spinning solution, to make the PAN fiber diameter to be formed become
It is small.Fibre diameter becomes smaller, and forms laminar flow effect when air circulation, can increase the filter efficiency of filter membrane.
Claims (7)
1. a kind of antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound, which is characterized in that with nothing
Woven fabric is base material, and the surface deposition of base material has the composite membrane that polyacrylonitrile/graphene oxide/tea polyphenol compound is formed, described
Polyacrylonitrile, graphene oxide, tea polyphenols mass ratio be（16-30）︰（4-10）︰（1-16）.
2. the antibacterial air filter film as described in claim 1 based on polyacrylonitrile/graphene oxide/tea polyphenol compound,
It is characterized in that, the thickness of the base material is 0.06-0.09mm, and the thickness of composite membrane is 0.02-0.05mm.
3. preparing the antibacterial air filter film as described in claim 1 based on polyacrylonitrile/graphene oxide/tea polyphenol compound
Method, which is characterized in that include the following steps：
1）The preparation of graphene oxide DMF dispersion liquids：DMF solution is added into graphene oxide aqueous dispersions, is rotated, must be aoxidized
Graphene DMF dispersion liquids；
2）The preparation of electrostatic spinning liquid：To step 1）Graphene oxide DMF dispersion liquids in add polyacrylonitrile successively and tea is more
Phenol mixes to obtain electrostatic spinning liquid；The polyacrylonitrile, graphene oxide, tea polyphenols, DMF solution mass ratio be（16-30）︰
（4-10）︰（1-16）︰ (75-194)；
3）The preparation of antibacterial air filter film：By step 2）Electrostatic spinning liquid the surface shape of base material is deposited on using method of electrostatic spinning
At composite membrane, antibacterial air filter film is obtained.
4. preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound as claimed in claim 3
Method, which is characterized in that step 3）Method of electrostatic spinning is：First base material is wound on the spinning axis of electrostatic spinning, then by electrostatic
Spinning solution, which is drawn in syringe pump, carries out electrostatic spinning, and electrostatic spinning liquid deposits to the surface of base material and forms composite membrane, composite membrane
Surface density be 2.5-4.9 g/m2, obtain antibacterial air filter film.
5. preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound as claimed in claim 4
Method, which is characterized in that technological parameter when electrostatic spinning is：Electrostatic spinning voltage 20-24 kV, the syringe needle stream of syringe pump
Amount is 0.1-0.4 mL/h, and needle diameter is 0.8-1.2 mm, and spinning distance is 16-20 cm, and spinning temperature is 20-30 DEG C,
Relative humidity is 30-50%, and the velocity of rotation for spinning axis is 500-700 r/h.
6. preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound as claimed in claim 3
Method, which is characterized in that step 2）The step of mixing includes magnetic agitation, ultrasonic disperse, magnetic stirring speed 60-160
R/min, mixing time 4-12h, ultrasonic power 8-12KHz, ultrasonic time are 1-3 h.
7. preparing the antibacterial air filter film based on polyacrylonitrile/graphene oxide/tea polyphenol compound as claimed in claim 3
Method, which is characterized in that step 1）When middle revolving, revolving temperature is 51-54 DEG C, and the speed of rotation is 80-120r/min, phase
It is -0.095MPa to vacuum degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810138322.0A CN108295675B (en) | 2018-02-10 | 2018-02-10 | Antibacterial air filter membrane based on polyacrylonitrile/graphene oxide/tea polyphenol compound and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810138322.0A CN108295675B (en) | 2018-02-10 | 2018-02-10 | Antibacterial air filter membrane based on polyacrylonitrile/graphene oxide/tea polyphenol compound and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108295675A true CN108295675A (en) | 2018-07-20 |
| CN108295675B CN108295675B (en) | 2020-01-24 |
Family
ID=62864865
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810138322.0A Expired - Fee Related CN108295675B (en) | 2018-02-10 | 2018-02-10 | Antibacterial air filter membrane based on polyacrylonitrile/graphene oxide/tea polyphenol compound and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108295675B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109730378A (en) * | 2018-12-29 | 2019-05-10 | 青岛融创新材料工程研究院有限公司 | A kind of PM2.5 protective mask and preparation method thereof with static spinning membrane |
| CN109985471A (en) * | 2019-04-25 | 2019-07-09 | 吉首大学 | A kind of tea polyphenol nano is except haze particle solution and its preparation method and purposes |
| CN111589308A (en) * | 2020-06-10 | 2020-08-28 | 杨晓飞 | Composite nanofiltration membrane with heavy metal interception capacity |
| CN112458632A (en) * | 2020-11-27 | 2021-03-09 | 广州美颂化妆品有限公司 | Electrostatic spinning composite tea oil film material and preparation method and application thereof |
| CN113069932A (en) * | 2021-03-26 | 2021-07-06 | 上海喂闹信息科技有限公司 | Preparation method of antibacterial and mildew-removing film for air humidifier |
| CN113975978A (en) * | 2021-12-10 | 2022-01-28 | 江苏巨之澜科技有限公司 | Graphene-enhanced photo-thermal evaporation membrane, membrane assembly and sewage concentration treatment device |
| CN114452840A (en) * | 2022-01-28 | 2022-05-10 | 中山大学 | Graphene oxide modified separation membrane based on electrostatic spraying and preparation and application thereof |
| ES2933047A1 (en) * | 2021-07-26 | 2023-01-31 | Fundacion Instituto De Investig Marques De Valdecilla | Material composed of polyacrylonitrile and graphene nanoplatelets, procedure for obtaining and use as a substrate for in vitro cultures of cancer cells (Machine-translation by Google Translate, not legally binding) |
| CN116575144A (en) * | 2023-07-13 | 2023-08-11 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220361A (en) * | 2015-11-04 | 2016-01-06 | 苏州大学 | The preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane |
| KR20170080798A (en) * | 2015-12-30 | 2017-07-11 | 주식회사 상보 | Method for producing graphene-polymer composite and graphene dispersion, and barrier film using the same |
| CN107475793A (en) * | 2016-06-08 | 2017-12-15 | 南京理工大学 | A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber |
| CN107469614A (en) * | 2017-07-04 | 2017-12-15 | 中国科学院城市环境研究所 | A kind of multifunctional air purifying screen pack |
| CN107583377A (en) * | 2017-08-24 | 2018-01-16 | 清华大学 | A kind of air-filtering membrane of functionalization graphene modification and preparation method thereof |
-
2018
- 2018-02-10 CN CN201810138322.0A patent/CN108295675B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220361A (en) * | 2015-11-04 | 2016-01-06 | 苏州大学 | The preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane |
| KR20170080798A (en) * | 2015-12-30 | 2017-07-11 | 주식회사 상보 | Method for producing graphene-polymer composite and graphene dispersion, and barrier film using the same |
| CN107475793A (en) * | 2016-06-08 | 2017-12-15 | 南京理工大学 | A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber |
| CN107469614A (en) * | 2017-07-04 | 2017-12-15 | 中国科学院城市环境研究所 | A kind of multifunctional air purifying screen pack |
| CN107583377A (en) * | 2017-08-24 | 2018-01-16 | 清华大学 | A kind of air-filtering membrane of functionalization graphene modification and preparation method thereof |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109730378A (en) * | 2018-12-29 | 2019-05-10 | 青岛融创新材料工程研究院有限公司 | A kind of PM2.5 protective mask and preparation method thereof with static spinning membrane |
| CN109985471A (en) * | 2019-04-25 | 2019-07-09 | 吉首大学 | A kind of tea polyphenol nano is except haze particle solution and its preparation method and purposes |
| CN111589308B (en) * | 2020-06-10 | 2022-03-25 | 中煤（北京）环保工程有限公司 | Composite nanofiltration membrane with heavy metal interception capacity |
| CN111589308A (en) * | 2020-06-10 | 2020-08-28 | 杨晓飞 | Composite nanofiltration membrane with heavy metal interception capacity |
| CN112458632A (en) * | 2020-11-27 | 2021-03-09 | 广州美颂化妆品有限公司 | Electrostatic spinning composite tea oil film material and preparation method and application thereof |
| CN113069932A (en) * | 2021-03-26 | 2021-07-06 | 上海喂闹信息科技有限公司 | Preparation method of antibacterial and mildew-removing film for air humidifier |
| ES2933047A1 (en) * | 2021-07-26 | 2023-01-31 | Fundacion Instituto De Investig Marques De Valdecilla | Material composed of polyacrylonitrile and graphene nanoplatelets, procedure for obtaining and use as a substrate for in vitro cultures of cancer cells (Machine-translation by Google Translate, not legally binding) |
| WO2023007044A1 (en) * | 2021-07-26 | 2023-02-02 | Fundación Instituto De Investigación Marqués De Valdecilla Idival | Composite material of polyacrylonitrile and graphene nanoplatelets, obtainment method and use as a substrate for in vitro cultures of cancer cells. |
| CN113975978A (en) * | 2021-12-10 | 2022-01-28 | 江苏巨之澜科技有限公司 | Graphene-enhanced photo-thermal evaporation membrane, membrane assembly and sewage concentration treatment device |
| CN113975978B (en) * | 2021-12-10 | 2023-05-26 | 江苏巨之澜科技有限公司 | Graphene-enhanced photo-thermal evaporation membrane, membrane module and sewage concentration treatment device |
| CN114452840A (en) * | 2022-01-28 | 2022-05-10 | 中山大学 | Graphene oxide modified separation membrane based on electrostatic spraying and preparation and application thereof |
| CN116575144A (en) * | 2023-07-13 | 2023-08-11 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
| CN116575144B (en) * | 2023-07-13 | 2023-09-26 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108295675B (en) | 2020-01-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108295675A (en) | A kind of antibacterial air filter film and preparation method thereof based on polyacrylonitrile/graphene oxide/tea polyphenol compound | |
| Wang et al. | Antibacterial and environmentally friendly chitosan/polyvinyl alcohol blend membranes for air filtration | |
| Xiong et al. | Flexible hydroxyapatite ultralong nanowire-based paper for highly efficient and multifunctional air filtration | |
| CN106984201B (en) | Nanometer spider web/beading fiber composite air-filtering membrane and preparation method thereof | |
| He et al. | Tailoring moisture electroactive Ag/Zn@ cotton coupled with electrospun PVDF/PS nanofibers for antimicrobial face masks | |
| CN109572082B (en) | Composite fiber membrane capable of being used for high-efficiency low-resistance anti-haze mask | |
| CN108993167B (en) | Preparation and application of antibacterial electrostatic spinning nanofiber air filtering material | |
| CN105040165B (en) | Biomass coke tar/Nano Silver/PAN is combined carbon fibre material and preparation method | |
| CN110773002B (en) | Antibacterial composite nanofiber membrane and preparation method and application thereof | |
| CN105544091B (en) | A kind of antibacterial nano fibrous composite and preparation method thereof | |
| CN104083946A (en) | Antibacterial gauze mask filter and preparation method thereof, and antibacterial gauze mask | |
| CN110075815A (en) | Novel haze high efficiency filter silver nanoparticle gauze and the compound porous fiber membrane material of MOFs and preparation method thereof | |
| CN110404339B (en) | High-efficiency low-resistance PM2.5 antibacterial and mildewproof filtering material and preparation method thereof | |
| CN107137979A (en) | A kind of micrometer fibers three-dimensional framework/polymer nanofiber composite filter material and preparation method thereof | |
| CN112755651B (en) | Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof | |
| CN102920067A (en) | Preparation method of nanofiber sandwich type protective facial mask | |
| JP2017177091A (en) | Filter medium for air filter | |
| Chen et al. | Electrospun nanofibrous membranes with asymmetric wettability for unidirectional moisture transport, efficient PM capture and bacteria inhibition | |
| CN110141975A (en) | A kind of multi-walled carbon nanotube-polyacrylonitrile (MWCNT-PAN) composite hyperfiltration membrane and preparation method thereof | |
| CN108786492A (en) | A kind of regulatable air-filtering membrane of quality factor and preparation method thereof | |
| CN113243589B (en) | Washable long-acting filtering graphene antibacterial mask and preparation method thereof | |
| JP2013194329A (en) | Method for producing nanocomposite-nanofiber | |
| CN107261865A (en) | A kind of functional form air filting material | |
| JP2012082566A (en) | Nanofiber | |
| CN107569915B (en) | A kind of material for air purification and preparation method thereof for intercepting PM1.0 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200124 Termination date: 20210210 |