CN105833742A - Preparation method for hydrophilic polyvinylidene fluoride (PVDF) antibacterial ultrafiltration membrane - Google Patents
Preparation method for hydrophilic polyvinylidene fluoride (PVDF) antibacterial ultrafiltration membrane Download PDFInfo
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- CN105833742A CN105833742A CN201610263949.XA CN201610263949A CN105833742A CN 105833742 A CN105833742 A CN 105833742A CN 201610263949 A CN201610263949 A CN 201610263949A CN 105833742 A CN105833742 A CN 105833742A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- 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
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- 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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- 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
Abstract
The invention discloses a preparation method for a hydrophilic polyvinylidene fluoride (PVDF) antibacterial ultrafiltration membrane. The preparation method comprises the following steps: (1) ultrasonically mixing PVP, AgNO3 and F127 in a DMF dispersion liquid of graphene oxide, thereby acquiring a uniformly dispersed mixing casting film liquid system; (2) adding PVDF powder into the mixing casting film liquid system, magnetically stirring for 6-10h and acquiring a pre-reaction solution, wherein PVDF accounts for 15-19% of the total mass of the system; (3) carrying out vacuum degassing and sealing on the pre-reaction solution acquired in the step (2) and then putting into an oil bath at 50-80 DEG C, stirring for 6-12h, standing and de-foaming for 8-12h, thereby acquiring the casting film liquid containing antibacterial active ingredients; and (4) preparing a modified antibacterial ultrafiltration membrane according to an immersion precipitated phase inversion method. The preparation method disclosed by the invention is simple. The acquired PVDF membrane has the advantages of excellent hydrophilicity, high flux, strong anti-pollution capacity and higher antibacterial activity.
Description
Technical field
The invention belongs to material modification preparing technical field, be specifically related to the system of a kind of hydrophilicity kynoar antibacterial ultrafiltration membrane
Preparation Method.
Background technology
Vinylidene is a kind of hypocrystalline high molecular polymer, has good chemical stability, heat resistance, mechanical stability,
And some highly polar organic solvent can be dissolved at a lower temperature, it is easy to use phase inversion masking, can prepare asymmetric
Milipore filter and microfiltration membranes (Flat Membrane and hollow-fibre membrane), and chemical modification can obtain other functions further, preparation
Functional separation film.Processing at water, biological medicine, the field such as food processing is widely used.But as a kind of performance
Excellent new polymers membrane material, PVDF there is also shortcoming, and it is low that the most extremely strong hydrophobicity result in membrane flux, is easily subject to
The Organic Pollutions such as protein and microorganism pollute, and limit its application, therefore, changing of hydrophilic antibiotic pvdf membrane
Journal of Sex Research is the most necessary.At present, the hydrophilic antibiotic modification implementation of film mainly has: one be Physical as by being blended or
Surface coating modified, the method is simple, low cost, but the uniformity coefficient of membrane material is wayward；Two is chemical method such as grafting
Modification, though lasting hydrophilic modifying effect can be obtained, but process mechanism is complicated.Physical and chemical method are implemented in combination in
The modified effect of excellent combination, is also a practicable research direction.
Chinese patent (publication number: 102989329A) discloses a kind of Ag/TiO2Modified PVDF ultrafiltration membrane and preparation thereof
Method and application, prepare, by active component blending and modifying, the PVDF ultrafiltration that good hydrophilic property, photocatalytic activity and antibiotic property are good
Film, but this method cost is high, and film uniformity coefficient is wayward.
Chinese patent (publication number: 103127839A) discloses a kind of method improving pvdf membrane contamination resistance, logical
Cross interpolation nano-component, utilize phase inversion to prepare the pvdf membrane that contamination resistance is strong, but directly add nano-oxide
Add modified cost, be unfavorable for industrial production.
Chinese patent (application number: 2012105215852) discloses one and utilizes modified graphene to strengthen antibiotic property and resistance tocrocking
The preparation method of milipore filter, be prepared for high anti-bacterial and anti-fouling dye ability milipore filter by adding isocyanide acidifying graphene oxide, fill
Divide and make use of graphene dispersion and anti pollution property.
Chinese patent (publication number: 105214511A) disclose a kind of Nano Silver/Graphene/Kynoar hybrid membranes and
Preparation method, (1) by Graphene, polyethylene glycol ultrasonic disperse in DMAC；(2)AgNO3, polyethylene glycol dissolve
In DMAC；(3) DMAC of Nano Silver/Graphene will be prepared after two solution mixing by ultrasonic wave added solvent-thermal process method
Solution；(4) PVDF powder dissolving formation casting solution in above-mentioned solution, Modified Membrane prepared by phase inversion has good
Antibacterial and contamination resistance, and Nano silver grain uniform load is on graphene film.But the consumption of the method silver salt is big, receives
Rice silver forming process is likely to form silver oxide etc., affects the raising of film properties.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide the system of a kind of hydrophilicity kynoar antibacterial ultrafiltration membrane
Preparation Method.The antibacterial ultrafiltration membrane good hydrophilic property that the inventive method prepares, flux is high, and antibacterial ability is strong, and the flux of film
Recovery rate is high.
The present invention provides the preparation method of a kind of hydrophilicity kynoar antibacterial ultrafiltration membrane, specifically comprises the following steps that
(1) by polyvinylpyrrolidone PVP, AgNO3, SYNPERONIC PE/F68 F127 is at graphene oxide
Ultrasonic mixing in DMF dispersion liquid, it is thus achieved that homodisperse mixing casting solution system；
(2) adding PVDF powder in homodisperse mixing casting solution system, PVDF accounts for the 15～19% of total system gross mass,
Magnetic agitation 6～10h under normal temperature, it is thus achieved that pre-reaction liquid；
(3) the pre-reaction liquid vacuum outgas obtained in step (2) is sealed in the oil bath being placed on 50～80 DEG C of temperature, stir 6～12h
After, stand froth breaking 8～12h, it is thus achieved that the casting solution containing Antibacterial Constituents；
(4) with the casting solution containing Antibacterial Constituents as raw material, with pure water as coagulation bath, immersion precipitation phase at a temperature of 20～35 DEG C
The modified antibacterial ultrafiltration membrane of conversion method preparation.
In the present invention, in step (1), the mass ratio of polyvinylpyrrolidone PVP and graphene oxide is 1:1～50:1.
In the present invention, in step (1), polyvinylpyrrolidone PVP and the matter of SYNPERONIC PE/F68 F127
Amount ratio is 0.5:1～2:1.
In the present invention, in step (1), graphene oxide and AgNO3Mass ratio be 0.05:1～1:1.
In the present invention, in step (3), pre-reaction liquid is through vacuum outgas 5～20min, it is to avoid Ag+Oxidation or shape in atmosphere
Become Ag2O affects modified effect.
Compared to the prior art, the beneficial effects of the present invention is:
The present invention regulates and controls with polyvinylpyrrolidone PVP or SYNPERONIC PE/F68 F127 for membrane structure
Agent, AgNO3Making presoma, GO is as disperse matrix and active component carrier, and under DMF effect prepared by in-situ reducing
Hydrophilicity kynoar antibacterial ultrafiltration membrane.Compared to the former film of PVDF, Modified Membrane contact angle is dropped to 50 ° by 75 °, 0.1MPa
Lower pure water flux is up to 295L m2·h-1, flux recovery rate is up to 99%, to 1mg mL-1BSA (MW=67kDa)
Rejection reach 98%, and staphylococcus aureus and colibacillary Bactericidal test result show and can form 3mm respectively
With 2mm inhibition zone, fungistatic effect is notable.
Accompanying drawing explanation
Fig. 1 is comparative example and the dynamic contact angle variation diagram of embodiment 3 rear pvdf membrane before modified.
Fig. 2 is the scanning electron microscope diagram (A: contrast is real in comparative example and embodiment 1,5 modified PVDF membrane cross section
Execute example；B: embodiment 1；C: embodiment 5).
Detailed description of the invention
The present invention is further described below in conjunction with the accompanying drawings.Technical solution of the present invention is not limited to the concrete real of act set forth below
Execute mode, also include any combination between each detailed description of the invention.
Embodiment 1
(1) preparation uniform dispersion: weigh 0.10g GO and be dispersed in 80.9g DMF, adds 1.5gPVP after ultrasonic disperse 2h,
Continue ultrasonic 0.5h, add 0.5g AgNO3Ultrasonic 0.5h forms uniform dispersion.
(2) preparation normal temperature pre-reaction liquid: magnetic agitation is initially charged 1.0g F127 in above-mentioned uniform dispersion simultaneously, stirs
After add 16g PVDF, under normal temperature stir 6h, formed transparent and homogeneous pre-reaction liquid.
(3) casting solution is prepared in in-situ heat reduction: react under the conditions of 60 DEG C of oil baths after being sealed by pre-reaction liquid vacuum outgas 20min
80h, prepares casting solution.
(4) immersion precipitation phase inversion process prepares antibacterial film: is scraped by above-mentioned casting solution on cleaned glass plate, stands 10s in atmosphere
After be immersed in 25 DEG C of pure water, come off after 1min from glass plate film forming.
Embodiment 2
(1) preparation uniform dispersion: weigh 0.15g GO and be dispersed in 78.4g DMF, adds 1.5gPVP after ultrasonic disperse 2h,
Continue ultrasonic 1h, add 0.45g AgNO3Ultrasonic 0.5h forms uniform dispersion.
(2) preparation normal temperature pre-reaction liquid: magnetic agitation is initially charged 1.5g F127 in above-mentioned uniform dispersion simultaneously, stirs
After add 18g PVDF, under normal temperature stir 8h, formed transparent and homogeneous pre-reaction liquid.
(3) casting solution is prepared in in-situ heat reduction: after being sealed by vacuum outgas 5min, pre-reaction liquid reacts under the conditions of 40 DEG C of oil baths
10h, prepares casting solution.
(4) immersion precipitation phase inversion process prepares antibacterial film: is scraped by above-mentioned casting solution on cleaned glass plate, stands 10s in atmosphere
After be immersed in 20 DEG C of pure water, come off after 1min from glass plate film forming.
Embodiment 3
(1) preparation uniform dispersion: weigh 0.65g GO and be dispersed in 76.6g DMF, adds 1.8gPVP after ultrasonic disperse 2h,
Continue ultrasonic 0.5h, add 1.25g AgNO3Ultrasonic 0.5h forms uniform dispersion.
(2) preparation normal temperature pre-reaction liquid: magnetic agitation is initially charged 1.8g F127 in above-mentioned uniform dispersion simultaneously, stirs
After add 18g PVDF, under normal temperature stir 6h, formed transparent and homogeneous reactant liquor.
(3) casting solution is prepared in in-situ heat reduction: react under the conditions of 50 DEG C of oil baths after being sealed by pre-reaction liquid vacuum outgas 10min
10h, prepares casting solution.
(4) immersion precipitation phase inversion process prepares antibacterial film: is scraped by above-mentioned casting solution on cleaned glass plate, stands 10s in atmosphere
After be immersed in 30 DEG C of pure water, come off after 1min from glass plate film forming.
Embodiment 4
(1) preparation uniform dispersion: weigh 0.20g GO and be dispersed in 79.4g DMF, adds 1.0gPVP after ultrasonic disperse 2h,
Continue ultrasonic 0.5h, add 0.4g AgNO3Ultrasonic 0.5h forms uniform dispersion.
(2) preparation normal temperature pre-reaction liquid: magnetic agitation is initially charged 1.0g F127 in above-mentioned uniform dispersion simultaneously, stirs
After add 18g PVDF, under normal temperature stir 6h, formed transparent and homogeneous pre-reaction liquid.
(3) casting solution is prepared in in-situ heat reduction: react under the conditions of 60 DEG C of oil baths after being sealed by pre-reaction liquid vacuum outgas 5min
12h, prepares casting solution.
(4) immersion precipitation phase inversion process prepares antibacterial film: is scraped by above-mentioned casting solution on cleaned glass plate, stands 10s in atmosphere
After, under the conditions of 20 DEG C, it being immersed in the ethanol of 50%, come off after 5min from glass plate film forming.
Embodiment 5
(1) preparation uniform dispersion: weigh 0.05g GO and be dispersed in 78.4g DMF, adds 1.5gPVP after ultrasonic disperse 2h,
Continue ultrasonic 0.5h, add 0.25g AgNO3Ultrasonic 0.5h forms uniform dispersion.
(2) preparation normal temperature pre-reaction liquid: magnetic agitation is initially charged 1.8g F127 in above-mentioned uniform dispersion simultaneously, stirs
After add 18g PVDF, under normal temperature stir 6h, formed transparent and homogeneous pre-reaction liquid.
(3) casting solution is prepared in in-situ heat reduction: react under the conditions of 80 DEG C of oil baths after being sealed by pre-reaction liquid vacuum outgas 7min
6h, prepares casting solution.
(4) immersion precipitation phase inversion process prepares antibacterial film: is scraped by above-mentioned casting solution on cleaned glass plate, stands 10s in atmosphere
After, under the conditions of 30 DEG C, it being immersed in the ethanol of 25%, come off after 5min from glass plate film forming.
Comparative example
Being dissolved in 82gDMF by 18g PVDF, magnetic agitation 6h under normal temperature, form transparent and homogeneous solution, vacuum outgas is close
It is honored as a queen under the conditions of 60 DEG C of oil baths and stirs 10h, prepare casting solution, after standing froth breaking 12h, above-mentioned casting solution is scraped in cleaning
On glass plate, being immersed in 25 DEG C and go in pure water after standing 10s in atmosphere, come off after 1min from glass plate film forming.
Performance test is tested
(1) hydrophilicity evaluation: after being dried by the Modified Membrane normal temperature of preparation, often group film is chosen 5 and is treated test sample, surveys with contact angle
Examination instrument measures the dynamic contact angle of Modified Membrane, the hydrophilicity on research film surface.
(2) strainability evaluation: often group Modified Membrane randomly selects 3 samples, is cut into the filter membrane disk that effective area is 38.5cm,
Filtration experiment is carried out, precompressed half at 0.2 mpa before often group experiment starts with laboratory homemade ultrafiltration membrance filter experimental provision
Subsequent experimental is carried out after hour stable.Filtration experiment is all carried out under 0.1MPa, passes sequentially through pure water 1h, 1mg mL-1's
BSA solution 2h, pure water 0.5h, pure water 1h.In experimentation, by water flux, pollute flux, flux recovery
Rate evaluates the strainability of Modified Membrane.
(3) bacteriostasis property evaluation: the equal high-temperature sterilization of all experimental articles in test, all experiments all operate in aseptic experiment room,
By antibacterial film described in inhibition zone method semiquantitative determination to golden yellow staphylococcus and colibacillary anti-microbial property, by variable concentrations
Bacterium solution be coated on the solid medium of preparation, then the Modified Membrane disk of a diameter of 1cm good for sterilizing is placed on accordingly
On culture medium, after 24h cultivated by sealed thermostat incubator, measure inhibition zone size, the fungistatic effect of quantitative analysis Modified Membrane.
The performance test results is as follows:
(1) Fig. 1 is the PVDF former film dynamic contact angle change contrast with the Modified Membrane of embodiment 3 of comparative example,
Can be seen that the initial contact angle of Modified Membrane is lower than unmodified pvdf membrane contact angle 20 °, its hydrophily improves a lot, and
In 80s, the contact angle of Modified Membrane almost reduces to 0, illustrates that there is good wetability on film surface.
(2) the strainability evaluation result of Modified Membrane shows, the Modified Membrane of preparation pure water flux under 0.1MPa reaches as high as
295L·m2·h-1, flux recovery rate is up to 99%, to 1mg mL-1BSA (MW=67kDa) rejection up to
98%.
(3) bacteriostasis property evaluation shows, bacterial concentration dilution 10-1Staphylococcus aureus again and colibacillary culture medium
In, the inhibition zone maximum of Modified Membrane is respectively 2mm and 3mm.
(4) the cross-sectional scans Electronic Speculum figure of Fig. 2 display comparison embodiment (A), embodiment 1 (B) and embodiment 2 (C) respectively
The antibacterial film difference hole pattern of preparation.Do that the Modified Membrane of coagulation bath presents with deionized water is the most through finger-like pore, with
Different concentration ethanol is done the Modified Membrane of coagulation bath and is presented the sponge hole of fine and close homogeneous, and finger-like pore is of value to the raising of membrane flux, sea
Continuous hole is of value to the raising of rejection.
In sum, what prepared by the preparation method of a kind of hydrophilicity kynoar (PVDF) antibacterial ultrafiltration membrane of the present invention changes
Property PVDF ultrafiltration membrane, good hydrophilic property, flux is high, and contamination resistance is strong, has staphylococcus aureus and Escherichia coli
Good fungistatic effect.
The above is only the citing of embodiments of the present invention, it is noted that for those skilled in the art
For, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement and modification, these improve and modification
Also should be regarded as protection scope of the present invention.
Claims (5)
1. the preparation method of a hydrophilicity kynoar antibacterial ultrafiltration membrane, it is characterised in that specifically comprise the following steps that
(1) by polyvinylpyrrolidone PVP, AgNO3, SYNPERONIC PE/F68 F127 is at graphene oxide
Ultrasonic mixing in DMF dispersion liquid, it is thus achieved that homodisperse mixing casting solution system；
(2) in homodisperse mixing casting solution system add PVDF powder, magnetic agitation 6～10h under normal temperature, it is thus achieved that pre-instead
Liquid, PVDF is answered to account for the 15～19% of pre-reaction liquid gross mass；
(3) the pre-reaction liquid vacuum outgas obtained in step (2) is sealed in the oil bath being placed on 50～80 DEG C of temperature, stir 6～12h
After, stand froth breaking 8～12h, it is thus achieved that the casting solution containing Antibacterial Constituents；
(4) with the casting solution containing Antibacterial Constituents as raw material, with pure water as coagulation bath, immersion precipitation at a temperature of 20～35 DEG C
The modified antibacterial ultrafiltration membrane of phase inversion preparation.
2. preparation method as claimed in claim 1, it is characterised in that: in step (1), polyvinylpyrrolidone PVP and
The mass ratio of graphene oxide is 1:1～50:1.
3. preparation method as claimed in claim 1, it is characterised in that: in step (1), polyvinylpyrrolidone PVP and ring
The mass ratio of oxidative ethane epoxy propane copolymer F127 is 0.5:1～2:1.
4. preparation method as claimed in claim 1, it is characterised in that: in step (1), graphene oxide and AgNO3Matter
Amount ratio is 0.05:1～1:1.
5. preparation method as claimed in claim 1, it is characterised in that: in step (3), pre-reaction liquid is through vacuum outgas 5～20
min。
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Cited By (5)
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| CN106552516A (en) * | 2016-10-11 | 2017-04-05 | 新疆蓝山屯河能源有限公司 | The methods and applications of purifying molecule amount ultrafilter membrane and preparation method thereof and the PTMEG molecular weight that narrows |
| CN107174964A (en) * | 2017-07-24 | 2017-09-19 | 上海应用技术大学 | A kind of use isopropanol coagulation bath regulates and controls the method that hydrophilic F127 PVDF are modified membrane structure |
| CN109277005A (en) * | 2018-09-30 | 2019-01-29 | 天津市金鳞水处理科技有限公司 | A kind of polyvinylidene fluoride modified composite membrane |
| RU2751513C1 (en) * | 2018-01-09 | 2021-07-14 | Вонтрон Мембрейн Текнолоджи Ко., Лтд. | Method for producing a superhydrophylic ultrafiltration membrane with photocatalytic properties |
| CN113843937A (en) * | 2021-10-08 | 2021-12-28 | 西安理工大学 | Migration-resistant hydrogel-based freshness colorimetric indication label and preparation method thereof |
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| CN113843937A (en) * | 2021-10-08 | 2021-12-28 | 西安理工大学 | Migration-resistant hydrogel-based freshness colorimetric indication label and preparation method thereof |
| CN113843937B (en) * | 2021-10-08 | 2024-02-06 | 西安理工大学 | Migration-resistant hydrogel-based freshness colorimetric indication label and preparation method thereof |
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Application publication date: 20160810 |