CN109529637A - A kind of preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane - Google Patents
A kind of preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane Download PDFInfo
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- CN109529637A CN109529637A CN201811555680.8A CN201811555680A CN109529637A CN 109529637 A CN109529637 A CN 109529637A CN 201811555680 A CN201811555680 A CN 201811555680A CN 109529637 A CN109529637 A CN 109529637A
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- capsaicin
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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
- B01D2325/36—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
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to technical field of membrane, more particularly to a kind of preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane, methyl methacrylate (MMA), acryloyl morpholine (ACMO) and 8- methy-N-vanillyl -6- nonenamide (Capsaicin) are dissolved in N-dimethylformamide (DMF) solvent, initiator azodiisobutyronitrile (AIBN) is added after being filled with nitrogen, it is further continued for after being filled with nitrogen, sealed reaction vessel.After reaction, Capsaicin derivative (PMMA-PACMO-Capsaicin) is obtained by precipitating, suction filtration, washing and drying.With Capsaicin derivative (PMMA-PACMO-Capsaicin) for modifying agent, polyethylene glycol (PEG) is additive, by the way that Capsaicin derivative (PMMA-PACMO-Capsaicin) is blended with Kynoar (PVDF), preparative separation film.
Description
Technical field
The invention belongs to technical field of membrane, and in particular to a kind of preparation side of resisting microbial contamination polyvinylidene fluoride separation membrane
Method.
Background technique
Membrane separation technique can be widely used in sewage treatment, sea water desalination, food processing and field of biomedicine, be close
Efficient, the green isolation technics to grow up in year a bit.But fouling membrane is to limit one of factor of its good application.Film
Pollution is a series of seperation film general names for increasing film osmotic resistance factor in the process of running.It refers in the feed liquid contacted with film
There are physics, chemistry, biochemistry or mechanical works between seperation film for particle, colloidal particle, solute transportation or hydrocarbon etc.
With, cause pollutant to adsorb, deposit in film surface or fenestra, membrane aperture caused to become smaller or block, make film generate permeation flux
The phenomenon that being greatly lowered with stalling characteristic.Microbial contamination is one of principal mode of fouling membrane, such as in water treatment by membrane mistake
Cheng Zhong, microorganism easily stick and grow in seperation film, finally form microbial thin film in separation membrane surface, seriously affect separation
The performance of film.
Kynoar (PVDF) is common organic polymer class membrane material, and strong hydrophobicity makes microorganism easily
In film surface tactophily, serious fouling membrane is generated.The hydrophiling and antibacterialization modification of Kynoar (PVDF) film are to mention
The approach of its high resisting microbial contamination performance.The principle of hydrophilic modification is by introducing hydrophilic material in membrane structure
Material, obtains the separation membrane surface with certain hydratability.Since water wetted material can be formed in conjunction with a large amount of hydrone, film surface
Hydrated sheath can prevent the absorption or deposition of pollutant, and then contamination resistance is improved.And antibacterial is modified as separating
Anti-biotic material is introduced in film, makes seperation film itself that there is bactericidal effect.
Polyaeryloyl morpholine (PACMO) is a kind of N- substituted acrylamide class high molecular polymer, it can be dissolved in many
In the solvent of polarity or low pole.Meanwhile polyaeryloyl morpholine (PACMO) is also low etc. with hydrophily, hypotoxicity, immunogenicity
Feature.If can be introduced into acryloyl morpholine (ACMO) in Kynoar (PVDF) film, the hydrophily of film be can be improved, in water
In environment, polyaeryloyl morpholine (PACMO) segment can adsorb a large amount of hydrone, and the hydrone of these high orientations surrounds poly- third
Dimethomorph (PACMO) segment forms one layer of hydrated sheath, and pollutant is prevented to contact with film surface, alleviates the fouling membranes such as Pore Blocking
Phenomenon, this provides reliable candidate material to construct the film surface of resisting microbial contamination.Natural Capsaicin is a kind of vanilla amide
Alkaloid, because it has the effects that excellent analgesia, anti-inflammatory, sterilization, anti-corrosion, be widely used in medicine, coating, biological pesticide,
Diet conservancy, chemical industry and military field.Capsaicin is as a kind of natural antibacterial material, to the gram-negative of coliform bacteria
Property bacterium, the gram-positive bacteria of staphylococcus aureus class and a variety of saccharomycete and marine algae etc. all have extraordinary suppression
Bacterium effect, can be used as the potential candidate for preparing resisting microbial contamination film.
Summary of the invention
The purpose of the present invention is in view of existing Kynoar (PVDF) separation membrane material resisting microbial contamination performance not
Foot, provides a kind of preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane.
A kind of preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane, includes the following steps.
Step 1 nonivamide derivative (PMMA-PACMO-Capsaicin): based on reaction solution total weight percent, claim
Take 10% ~ 30% methyl methacrylate (MMA), 5% ~ 15% acryloyl morpholine (ACMO) and 1% ~ 3% 8- methy-N-vanillyl -6-
Nonenamide (Capsaicin) co-dissolve is in 65% ~ 75% dimethylformamide (DMF).After 15 min of inflated with nitrogen, it is added
0.1% ~ 0.5% initiator azodiisobutyronitrile (AIBN), after being further continued for inflated with nitrogen 10min, sealed reaction vessel, and shift rapidly
Product is precipitated with dehydrated alcohol after reacting 6 h into 60 DEG C of oil bath pans, and with pure water, to remove unreacted list
Body.Finally, product is placed in oven and dried for use.
Step 2 preparative separation film M: based on casting solution total weight percent, weigh 5% ~ 15% Kynoar (PVDF),
1% ~ 8% Capsaicin derivative (PMMA-PACMO-Capsaicin) and 2% ~ 8% polyethylene glycol (PEG) are immersed in 75% ~ 85% N- methyl
In pyrrolidones (NMP) solvent, stirring and dissolving is in N-Methyl pyrrolidone (NMP) solvent at 60 DEG C.Casting solution stands de-
Bubble, by casting solution be added dropwise on a glass, with hymenotome striking primary membrane is scraped, be then immersed in film-forming in coagulating bath, to film from
It after falling off on glass plate, then is placed in pure water 24 hours, completely obtains seperation film with pure water rinsing.
The invention has the advantages that: simple process, it is at low cost, be easy implement, seperation film hydrophily prepared by the present invention is stronger,
The anti-microbial property of film is significantly higher than pure Kynoar (PVDF) film, can be used as sewage treatment separation membrane material and further develops benefit
With.
Detailed description of the invention
Fig. 1 is the profile scanning electron microscope of seperation film M1.
Fig. 2 is the profile scanning electron microscope of seperation film M2.
Fig. 3 is the profile scanning electron microscope of seperation film M3.
Fig. 4 is the water contact angle figure of pure Kynoar (PVDF) seperation film (M0).
Fig. 5 is the water contact angle figure of seperation film M3.
Fig. 6 is antibacterial experiment figure of pure Kynoar (PVDF) seperation film (M0) to staphylococcus aureus.
Fig. 7 is antibacterial experiment figure of the seperation film M3 to staphylococcus aureus.
Specific embodiment
A kind of preparation method of the resisting microbial contamination polyvinylidene fluoride separation membrane of embodiment 1, includes the following steps.
Step 1 nonivamide derivative (PMMA-PACMO-Capsaicin): 16 g methyl methacrylates are weighed
(MMA), 5.7 g acryloyl morpholines (ACMO) and 1 g 8- methy-N-vanillyl -6- nonenamide (Capsaicin) are common molten
Solution is in 50 ml dimethylformamides (DMF).At room temperature after 15 min of inflated with nitrogen, it is different that 0.164g initiator azo two is added
Butyronitrile (AIBN), after continuing inflated with nitrogen 10min, sealed reaction vessel, and be quickly transferred to react 6h in the oil bath pan of 60 oC,
Product is precipitated with dehydrated alcohol after reaction, and with pure water 3 times, to remove unreacted monomer.Finally, by product
It is placed in oven and dried stand-by.
Step 2 preparative separation film M1: 12.5g Kynoar (PVDF), 2.5g Capsaicin derivative (PMMA- are weighed
PACMO-Capsaicin it) is immersed in 82.5g N-Methyl pyrrolidone (NMP) solvent with 2.5g polyethylene glycol (PEG), 60
In oC oil bath pan, heating stirring is to after being completely dissolved, standing and defoaming.Casting solution takes out from oil bath pan, will after being cooled to room temperature
Casting solution is added dropwise on clean glass plate, with the scraper striking plate membrane having a size of 150 μm, is then immersed in 25 DEG C of solidification
Film-forming in bath after film falls off from glass plate, then is placed in pure water 24 ~ 36 hours, is completely divided with pure water rinsing
From film.
The pure water contact angle of gained seperation film M1 is 80.8o, and the antibacterial efficiency to staphylococcus aureus is 65.8%.It is poly-
Ethylene glycol (PEG) number-average molecular weight is 1000-20000, and coagulating bath is pure water.
A kind of preparation method of the resisting microbial contamination polyvinylidene fluoride separation membrane of embodiment 2, includes the following steps.
Step 1 nonivamide derivative (PMMA-PACMO-Capsaicin): 16 g methyl methacrylates are weighed
(MMA), 5.7 g acryloyl morpholines (ACMO) and 1 g 8- methy-N-vanillyl -6- nonenamide (Capsaicin) are common molten
Solution is in 50 ml dimethylformamides (DMF).At room temperature after 15 min of inflated with nitrogen, it is different that 0.164g initiator azo two is added
Butyronitrile (AIBN), after continuing inflated with nitrogen 10min, sealed reaction vessel, and be quickly transferred to react 6 h in the oil bath pan of 60 oC,
Product is precipitated with dehydrated alcohol after reaction, and with pure water 3 times, to remove unreacted monomer.Finally, by product
It is placed in oven and dried stand-by.
Step 2 preparative separation film M2: 10g Kynoar (PVDF), 5g Capsaicin derivative (PMMA-PACMO- are weighed
Capsaicin it) is immersed in 82.5g N-Methyl pyrrolidone (NMP) solvent with 2.5g polyethylene glycol (PEG), in 60oC oil bath
In pot, heating stirring is to after being completely dissolved, standing and defoaming.Casting solution takes out from oil bath pan, after being cooled to room temperature, by casting solution
It is added dropwise on clean glass plate, with the scraper striking plate membrane having a size of 150 μm, is then immersed in 25 DEG C of coagulating bath solid
It is melted into film, after film falls off from glass plate, then is placed in pure water 24-36 hours, completely obtains seperation film with pure water rinsing.
The pure water contact angle of gained seperation film M2 is 66.8o, and the antibacterial efficiency to staphylococcus aureus is 71.5%.It is poly-
Ethylene glycol (PEG) number-average molecular weight is 1000 ~ 20000, and coagulating bath is pure water.
A kind of preparation method of the resisting microbial contamination polyvinylidene fluoride separation membrane of embodiment 3, includes the following steps.
Step 1 nonivamide derivative (PMMA-PACMO-Capsaicin): 16 g methyl methacrylates are weighed
(MMA), 5.7 g acryloyl morpholines (ACMO) and 1 g 8- methy-N-vanillyl -6- nonenamide (Capsaicin) are common molten
Solution is in 50 ml dimethylformamides (DMF).At room temperature after 15 min of inflated with nitrogen, it is different that 0.164g initiator azo two is added
Butyronitrile (AIBN), after continuing inflated with nitrogen 10min, sealed reaction vessel, and be quickly transferred to react 6h in the oil bath pan of 60 oC,
Product is precipitated with dehydrated alcohol after reaction, and with pure water 3 times, to remove unreacted monomer.Finally, by product
It is placed in oven and dried stand-by.
Step 2 preparative separation film M3: 7.5g Kynoar (PVDF), 7.5g Capsaicin derivative (PMMA- are weighed
PACMO-Capsaicin it) is immersed in 82.5g N-Methyl pyrrolidone (NMP) solvent with 2.5g polyethylene glycol (PEG), 60
In oC oil bath pan, heating stirring is to after being completely dissolved, standing and defoaming.Casting solution takes out from oil bath pan, will after being cooled to room temperature
Casting solution is added dropwise on clean glass plate, with the scraper striking plate membrane having a size of 150 μm, is then immersed in 25 DEG C of solidification
Film-forming in bath after film falls off from glass plate, then is placed in pure water 24-36 hours, is completely divided with pure water rinsing
From film.
The pure water contact angle of gained seperation film M3 is 58.6o, and the antibacterial efficiency to staphylococcus aureus is 88.5%.It is poly-
Ethylene glycol (PEG) number-average molecular weight is 1000 ~ 20000, and coagulating bath is pure water.
Comparative example prepares the preparation method of pure Kynoar (PVDF) seperation film M0, includes the following steps.
Step 1 prepares pure Kynoar (PVDF) seperation film M0: by 15 g Kynoar (PVDF) powder and 2.5
G polyethylene glycol (PEG) is immersed in 82.5 g N-Methyl pyrrolidone (NMP) solvents, is stirred at 60 DEG C to being completely dissolved.
After standing and defoaming, casting solution is added dropwise on dry glass plate, and with the scraper striking plate membrane having a size of 150 μm.
Primary membrane is immersed in rapidly in 25 DEG C of pure water baths by step 2, after solidifying completely, cleans film with a large amount of pure water
Sample, and it is stored in pure water.The pure water contact angle of pure Kynoar (PVDF) seperation film is 88.6o, to Staphylococcus aureus
The antibacterial efficiency of bacterium is only 1.5%.
Above-mentioned 3 embodiment results and comparative example are the result shows that Capsaicin derivative (PMMA-PACMO-Capsaicin) is obvious
Improve the hydrophilicity and resisting microbial contamination performance of Kynoar (PVDF) seperation film.
Claims (12)
1. a kind of resisting microbial contamination modifying agent, which is characterized in that the modifying agent is Capsaicin derivative, and Capsaicin derivative is by first
Base methyl acrylate, acryloyl morpholine, 8- methy-N-vanillyl -6- nonenamide are copolymerized and obtain.
2. resisting microbial contamination modifying agent according to claim 1, which is characterized in that methyl methacrylate, acryloyl
Quinoline, 8- methy-N-vanillyl -6- nonenamide weight ratio be 16:5.7:1.
3. a kind of resisting microbial contamination polyvinylidene fluoride separation membrane, which is characterized in that using Capsaicin derivative as modifying agent, Capsaicin spreads out
Biology is blended with PVDF is prepared resisting microbial contamination polyvinylidene fluoride separation membrane, and Capsaicin derivative is by methyl methacrylate
Ester, acryloyl morpholine, 8- methy-N-vanillyl -6- nonenamide are copolymerized and obtain.
4. resisting microbial contamination polyvinylidene fluoride separation membrane according to claim 3, which is characterized in that methyl methacrylate
Ester, acryloyl morpholine, 8- methy-N-vanillyl -6- nonenamide weight ratio be 16:5.7:1.
5. resisting microbial contamination polyvinylidene fluoride separation membrane according to claim 3, which is characterized in that Capsaicin derivative with
The blending mass ratio of PVDF is 1/5 ~ 1/1.
6. resisting microbial contamination polyvinylidene fluoride separation membrane according to claim 3, which is characterized in that use immersion precipitation phase
Conversion method is made.
7. a kind of preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane, which is characterized in that
Step 1: nonivamide derivative: methyl methacrylate (MMA), acryloyl morpholine (ACMO) and 8- methyl-N- vanilla
Base -6- nonenamide (Capsaicin) is copolymerized to obtain Capsaicin derivative；
Step 2: using immersion precipitation phase inversion process preparative separation film, including by Capsaicin derivative and PVDF, pore-foaming agent one
It rises and is dissolved in solvent the step of obtaining casting solution.
8. the preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane according to claim 7, which is characterized in that methyl
Methyl acrylate, acryloyl morpholine, 8- methy-N-vanillyl -6- nonenamide weight ratio (or writing molar ratio) 16:5.7:
1。
9. the preparation method of resisting microbial contamination polyvinylidene fluoride separation membrane according to claim 7, which is characterized in that synthesis
The specific steps of Capsaicin derivative (PMMA-PACMO-Capsaicin) are as follows: based on reaction solution total weight percent, weigh 10% ~
30% methyl methacrylate (MMA), 5% ~ 15% acryloyl morpholine (ACMO) and 1% ~ 3% 8- methy-N-vanillyl -6- nonene acyl
Amine (Capsaicin) co-dissolve is in 65% ~ 75% dimethylformamide (DMF), after 15 min of inflated with nitrogen, addition 0.1% ~
0.5% initiator azodiisobutyronitrile (AIBN), after being further continued for inflated with nitrogen 10min, sealed reaction vessel, and it is quickly transferred to 60
DEG C oil bath pan in react 6 h after product is precipitated with dehydrated alcohol, and with pure water, finally product is put into baking oven and is done
It is dry stand-by.
10. according to the preparation method of any one of the claim 6-9 resisting microbial contamination polyvinylidene fluoride separation membrane, feature
It is, preparative separation film: based on casting solution total weight percent, weighs 5% ~ 15% Kynoar (PVDF), 1% ~ 8% Capsaicin spreads out
Biological (PMMA-PACMO-Capsaicin) and 2% ~ 8% polyethylene glycol (PEG) are immersed in 75% ~ 85% N-Methyl pyrrolidone
(NMP) in solvent, stirring and dissolving is in N-Methyl pyrrolidone (NMP) solvent at 60 DEG C, casting solution standing and defoaming, by casting film
Drop adds on a glass, with hymenotome striking primary membrane is scraped, is then immersed in film-forming in coagulating bath, takes off from glass plate to film
Fall behind, then be placed in pure water 24 hours, completely obtains seperation film with pure water rinsing.
11. a kind of Capsaicin derivative is used to improve the purposes of seperation film stable against biological contamination, which is characterized in that Capsaicin derivative is
It is copolymerized by methyl methacrylate, acryloyl morpholine, 8- methy-N-vanillyl -6- nonenamide and is obtained.
12. Capsaicin derivative is used to improve the purposes of seperation film stable against biological contamination according to claim 10, feature exists
In the weight ratio of methyl methacrylate, acryloyl morpholine and 8- methy-N-vanillyl -6- nonenamide is 16:5.7:1.
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| CN109529637B (en) | 2021-08-03 |
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