CN105498548A - Preparation method of antibacterial nanofiltration membrane containing silver nanoparticles - Google Patents
Preparation method of antibacterial nanofiltration membrane containing silver nanoparticles Download PDFInfo
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- CN105498548A CN105498548A CN201510847615.2A CN201510847615A CN105498548A CN 105498548 A CN105498548 A CN 105498548A CN 201510847615 A CN201510847615 A CN 201510847615A CN 105498548 A CN105498548 A CN 105498548A
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/60—Polyamines
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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
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/06—Flat membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
-
- 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 relates to a preparation method of an antibacterial nanofiltration membrane containing silver nanoparticles and belongs to the field of a membrane anti-pollution technology. The preparation method comprises the followings steps: dissolving polyisophthaloyl metaphenylene diamine in a mixed solution of an organic solvent and a pore forming agent, stirring and mixing, standing at constant temperature and under vacuum condition and defoaming to obtain a membrane casting solution; pouring the membrane casting solution onto a glass plate covered with non-woven fabric to prepare a membrane sample wafer; immersing the membrane sample wafer into a prepared mixed solution of isopropanol and deionized water, cleaning, reacting by letting the membrane contact with a silver nitrate, reacting by letting the membrane contact with a sodium borohydride solution, and finally forming silver nanoparticles on the membrane so as to obtain the antibacterial nanofiltration membrane containing silver nanoparticles. By the method, original excellent characteristics of a polyisophthaloyl metaphenylene diamine nanofiltration membrane are reserved, and stain resistance and antibacterial property of the membrane are further enhanced under the precondition of not influencing original membrane flux. The membrane of the invention has a wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of antibacterial nano filter membrance of silver nanoparticle-containing, particularly one is antibacterial to improve by generating Nano silver grain at NF membrane surface in situ, and the method for anti-pollution ability, belongs to film antipollution technical field.
Background technology
Membrane separation technique is a kind of emerging treatment technology, compared with traditional isolation technics, it have separative efficiency high, free from environmental pollution, be convenient to the advantage such as integrated with other technologies, be widely used in the fields such as petrochemical industry, electronics, pharmacy, food, biochemistry, environment, desalinization.
Nanofiltration (NF) is a kind of pressure-driven membrane separation technique between counter-infiltration (RO) and ultrafiltration (UF), to divalence and above valence state ion and relative molecular mass between 200 ~ 1000 material there is higher rejection.NF membrane is compared with reverse osmosis technology, and its operating pressure is lower, capable of reducing energy consumption; Compared with ultrafiltration membrane technique, it can remove the salt and low molecule organic matter that ultrafiltration cannot retain.Nanofiltration has been widely used in the aspects such as drink water purifying, food and drink waste water, textile printing and dyeing wastewater process with the stalling characteristic of its uniqueness.
NF membrane also exists as shortcomings such as fouling membrane and anti-microbial property differences in concrete separation use procedure, and food and pharmaceuticals industry are to hygienic requirements extremely sternly, and film needs the process such as frequent sterilization, cleaning, makes widely using of this technology be subject to certain impact.Patent CN101053782A, by introducing the antimicrobial nano particle modified through plasma chemistry in cellulose acetate nano filter-membrane, makes NF membrane have antibacterial, sterilizing function, but its complicated process of preparation.Therefore film antipollution how is improved and anti-microbial property needs to study further.Patent CN100335156C nano anti-biotic material one polysulphone composite microporous filter film that utilized phase inversion to prepare, in the process of membrane filtration, can play the effect of sterilizing.US Patent No. 2002013972 describes a kind of preparation method of sticking the antibacterial film of water-insoluble propolis on basement membrane, utilizes the adsorptivity of propolis by the bacterium in water, virus disinfection.Shortcoming bacterium, virus thoroughly can not be removed, and will carry out reprocessing and just can reuse after propolis adsorption capacity reaches capacity, cumbersome.Research finds that Nano silver grain has good anti-microbial property, and not easily forms new pollution, and therefore the silver-colored Modified Membrane of current utilization reaches the focus that antibacterial object becomes research.Patent CN101298026A provides a kind of method utilizing argentiferous polyelectrolyte complex compound and layer upon layer electrostatic self-assembling technique to prepare antibacterial nano filter membrance, achieves good antibacterial effect.Silver is added on film and mainly contain in-situ preparation and blended method.But blend method, there is the problem that nano particle is easily easily reunited in film, and spread to aqueous phase at the time nano particle be separated, be enriched in film surface, the while of enhancing film surface hydrophilic, film section hydrophily strengthens less, promotes limited to film contamination resistance.And in-situ preparation can improve this problem better.Patent CN104117293A utilizes in-situ preparation Nano Silver modification PVDF ultrafiltration membrane, well improves the antibacterial ability of film.But at present, the patent being prepared modification NF membrane by fabricated in situ Nano silver grain is a lot, but based on taking poly as basement membrane, the antimicrobial technology of fabricated in situ Nano silver grain modification NF membrane is adopted to have no report.
Summary of the invention
The object of the invention is, in order to overcome the deficiencies in the prior art, to provide a kind of preparation method of antibacterial nano filter membrance of silver nanoparticle-containing.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A preparation method for the antibacterial nano filter membrance of silver nanoparticle-containing, its step is as follows:
(1) be dissolved in by poly in the mixed solution of organic solvent and pore-foaming agent and be uniformly mixed, under constant temperature, vacuum condition, standing and defoaming obtains casting solution;
(2) by deaeration completely casting solution be cast in and be covered with on the glass plate of non-woven fabrics, by scraper striking film forming, after evaporate to dryness, in immersion precipitation bath water, film-forming dries, and obtains film print;
(3) mixed liquor above-mentioned film print being put into isopropyl alcohol and the deionized water prepared soaks 10-30 minute, puts into deionized water and soaks 24 hours, then store in 4 DEG C after taking out the cleaning of film print.
(4) be 1 ~ 10mM liquor argenti nitratis ophthalmicus haptoreaction 10min by the film print in (3) and concentration, then solution removed;
(5) be that 1 ~ 10mM sodium borohydride solution contacts by the film print in (4) and concentration, active layer reacts 5-10min, form Nano silver grain, then solution is removed;
(6) by the above-mentioned film print washed with de-ionized water having generated Nano silver grain 10 seconds, put into deionized water and preserve, namely obtain the antibacterial nano filter membrance of silver nanoparticle-containing;
In the preparation process of the antibacterial nano filter membrance of above-mentioned silver nanoparticle-containing especially, the consumption of described poly is 10% ~ 30wt%, and described consumption of organic solvent is 50% ~ 90wt%, and described pore-foaming agent consumption is 3% ~ 20wt%.
Further, described organic solvent is be a kind of or two or more arbitrarily mixture in DMA (DMAc), dimethyl formamide, METHYLPYRROLIDONE.
Further, described pore-foaming agent is a kind of or two or more arbitrarily mixture in lithium chloride, polyvinylpyrrolidone, polyethylene glycol, calcium chloride, ammonium chloride;
Further, the amount ratio of the isopropyl alcohol described in step (3) and deionized water is: the consumption of isopropyl alcohol is 10% ~ 30wt%, and the consumption of deionized water is 70% ~ 90wt%;
Preferably, the slot thickness of scraping of described scraper is 0.26mm.
The inventive method has following technical characterstic:
(1) the present invention effectively can control the density on film surface of Nano silver grain by the concentration controlling argentiferous cationic solution and sodium borohydride solution;
(2) although the present invention introduces Nano silver grain on film surface, the original water flux of film is not almost affected;
(3) Nano silver grain that the present invention generates is combined stable with basement membrane, difficult drop-off.
Compared with prior art comparatively, the inventive method, at film surface in situ synthesis Nano silver grain, reaches good anti-microbial property, especially to Escherichia coli, staphylococcus aureus, pseudomonas aeruginosa has good anti-microbial property, and very little on the size impact of water flux and salt rejection.
The inventive method is simple to operate, is convenient to control.Experimental result shows that the method not only remains the originally excellent characteristic of poly NF membrane, under the prerequisite not affecting original membrane flux, improves the resistant antibiotic property of film, is with a wide range of applications.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
First get 5g anhydrous Lithium chloride and be dissolved in 75gN, in N-dimethylacetylamide, 20g poly is dissolved in above-mentioned solution, be placed in the heating of 80 DEG C of baking ovens be uniformly mixed be placed on constant temperature, vacuum condition under standing and defoaming obtain casting solution;
Then control humidity and temperature in casting film room, by deaeration completely casting solution be cast in and be covered with on the glass plate of non-woven fabrics, with scraping the stainless steel scraper striking film forming that slot thickness is 0.26mm, after evaporation a period of time, film-forming in immersion precipitation bath water, dries immediately, obtains film print;
Then above-mentioned film print is put into the mixed liquor containing 20wt% isopropyl alcohol and 80wt% deionized water prepared and soak 15 minutes, clean 3 times, put into deionized water afterwards and soak 24 hours, be then in store in 4 DEG C;
Be placed between one piece of glass plate and rubber framework by ready film print, the size of rubber framework is approximately 8cm*12cm again, and the active layer of film upwards.Be the active layer surface that 1mM liquor argenti nitratis ophthalmicus pours the naked film spilt into by concentration, reaction 10min, then removes solution, only leaves the thin layer of film surface liquor argenti nitratis ophthalmicus;
Finally the sodium borohydride solution of same concentrations is poured among framework, active layer reacts 5min, form Nano silver grain, then solution is removed, to generate the film print washed with de-ionized water 10 seconds of Nano silver grain, put into deionized water to preserve, namely obtain the antibacterial nano filter membrance of silver nanoparticle-containing.
Through this film of test for identification, 94% is reached to colibacillary sterilizing rate, refer to the anti-microbial property of film.
Embodiment 2
First getting 15g polyvinylpyrrolidone is dissolved in 228g dimethyl formamide, and 57g poly is dissolved in above-mentioned solution, be placed in the heating of 80 DEG C of baking ovens be uniformly mixed be placed on constant temperature, vacuum condition under standing and defoaming obtain casting solution;
Then control humidity and temperature in casting film room, by deaeration completely casting solution be cast in and be covered with on the glass plate of non-woven fabrics, with scraping the stainless steel scraper striking film forming that slot thickness is 0.26mm, after evaporation a period of time, film-forming in immersion precipitation bath water, dries immediately, obtains film print;
Then above-mentioned film print is put into the mixed liquor containing 15wt% isopropyl alcohol and 85wt% deionized water prepared and soak 15 minutes, clean 3 times, put into deionized water afterwards and soak 24 hours, be then in store in 4 DEG C;
Be placed between one piece of glass plate and rubber framework by ready film print, the size of rubber framework is approximately 8cm*12cm again, and the active layer of film upwards.Be the active layer surface that 2mM liquor argenti nitratis ophthalmicus pours the naked film spilt into by concentration, reaction 10min, then removes solution, only leaves the thin layer of film surface liquor argenti nitratis ophthalmicus;
Finally the sodium borohydride solution of same concentrations is poured among framework, active layer reacts 8min, form Nano silver grain, then solution is removed, to generate the film print washed with de-ionized water 10 seconds of Nano silver grain, put into deionized water to preserve, namely obtain the antibacterial nano filter membrance of silver nanoparticle-containing.
Reach 95% through the sterilizing rate of this film of test for identification to staphylococcus aureus, refer to the anti-microbial property of film.
Embodiment 3
First getting 11g polyethylene glycol is dissolved in 144gN-N-methyl-2-2-pyrrolidone N-, and 45g poly is dissolved in above-mentioned solution, be placed in the heating of 80 DEG C of baking ovens be uniformly mixed be placed on constant temperature, vacuum condition under standing and defoaming obtain casting solution;
Then control humidity and temperature in casting film room, by deaeration completely casting solution be cast in and be covered with on the glass plate of non-woven fabrics, with scraping the stainless steel scraper striking film forming that slot thickness is 0.26mm, after evaporation a period of time, film-forming in immersion precipitation bath water, dries immediately, obtains film print;
Then above-mentioned film print is put into the mixed liquor containing 25wt% isopropyl alcohol and 75wt% deionized water prepared and soak 30 minutes, clean 3 times, put into deionized water afterwards and soak 24 hours, be then in store in 4 DEG C;
Be placed between one piece of glass plate and rubber framework by ready film print, the size of rubber framework is approximately 8cm*12cm again, and the active layer of film upwards.Be the active layer surface that 5mM liquor argenti nitratis ophthalmicus pours the naked film spilt into by concentration, reaction 10min, then removes solution, only leaves the thin layer of film surface liquor argenti nitratis ophthalmicus;
Finally the sodium borohydride solution of same concentrations is poured among framework, active layer reacts 10min, form Nano silver grain, then solution is removed, to generate the film print washed with de-ionized water 10 seconds of Nano silver grain, put into deionized water to preserve, namely obtain the antibacterial nano filter membrance of silver nanoparticle-containing.
Reach 95% through the sterilizing rate of this film of test for identification to pseudomonas aeruginosa, refer to the anti-microbial property of film.
The above; be only the present invention's preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (5)
1. a preparation method for the antibacterial nano filter membrance of silver nanoparticle-containing, is characterized in that, the method comprises the following steps:
(1) poly is dissolved in the mixed solution of organic solvent and pore-foaming agent and is uniformly mixed, 80 DEG C, standing and defoaming obtains casting solution under vacuum condition;
(2) by deaeration completely casting solution be cast in and be covered with on the glass plate of non-woven fabrics, by scraper striking film forming, after evaporate to dryness, in immersion precipitation bath water, film-forming dries, and obtains film print;
(3) mixed liquor above-mentioned film print being put into isopropyl alcohol and the deionized water prepared soaks 10-30 minute, puts into deionized water and soaks 24 hours, then store in 4 DEG C after taking out the cleaning of film print.
(4) be 1 ~ 10mM liquor argenti nitratis ophthalmicus haptoreaction 10min by the film print in (3) and concentration, then solution removed;
(5) be that 1 ~ 10mM sodium borohydride solution contacts by the film print in (4) and concentration, active layer react 5) 10min, form Nano silver grain, then solution is removed;
(6) by the above-mentioned film print washed with de-ionized water having generated Nano silver grain 10 seconds, put into deionized water and preserve, namely obtain the antibacterial nano filter membrance of silver nanoparticle-containing;
In the preparation process of the antibacterial nano filter membrance of above-mentioned silver nanoparticle-containing, the consumption of described poly is 10% ~ 30wt%, and described consumption of organic solvent is 50% ~ 90wt%, and described pore-foaming agent consumption is 3% ~ 20wt%.
2. the preparation method of the antibacterial nano filter membrance of silver nanoparticle-containing according to claim 1, it is characterized in that, described organic solvent is for N (N) dimethylacetylamide, dimethyl formamide, N) methyl) 2) a kind of or two or more arbitrarily mixture in pyrrolidones.
3. the preparation method of the antibacterial nano filter membrance of silver nanoparticle-containing according to claim 1, it is characterized in that, described pore-foaming agent is a kind of or two or more arbitrarily mixture in lithium chloride, polyvinylpyrrolidone, polyethylene glycol, calcium chloride, ammonium chloride.
4. the preparation method of the antibacterial nano filter membrance of silver nanoparticle-containing according to claim 1, it is characterized in that, the amount ratio of the isopropyl alcohol described in step (3) and deionized water is: the consumption of isopropyl alcohol is 10% ~ 30wt.%, and the consumption of deionized water is 70% ~ 90wt.%.
5. the preparation method of the antibacterial nano filter membrance of silver nanoparticle-containing according to claim 1, is characterized in that, the slot thickness of scraping of described scraper is 0.26mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105727752A (en) * | 2016-05-11 | 2016-07-06 | 贵州省材料产业技术研究院 | Preparation method of high-strength anti-pollution antibacterial hollow fiber nanofiltration membrane and product |
| CN110841492A (en) * | 2019-09-25 | 2020-02-28 | 长春工业大学 | Preparation method of nano-silver modified polytetrafluoroethylene microporous membrane for membrane distillation |
| CN112973473A (en) * | 2021-03-08 | 2021-06-18 | 天津工业大学 | Reverse osmosis composite membrane resisting biological pollution and preparation method thereof |
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| US20030007928A1 (en) * | 2000-10-25 | 2003-01-09 | Gray Bruce Nathaniel | Polymer based radionuclide containing particulate material |
| CN101693024A (en) * | 2009-10-20 | 2010-04-14 | 中国科学院化学研究所 | Radionuclide-labelled biodegradable bioabsorbable biopolymer nano fibrous membrane, preparation process and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105727752A (en) * | 2016-05-11 | 2016-07-06 | 贵州省材料产业技术研究院 | Preparation method of high-strength anti-pollution antibacterial hollow fiber nanofiltration membrane and product |
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| CN110841492A (en) * | 2019-09-25 | 2020-02-28 | 长春工业大学 | Preparation method of nano-silver modified polytetrafluoroethylene microporous membrane for membrane distillation |
| CN112973473A (en) * | 2021-03-08 | 2021-06-18 | 天津工业大学 | Reverse osmosis composite membrane resisting biological pollution and preparation method thereof |
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