CN101298026A - Preparation of antibacterial nano filter membrance - Google Patents
Preparation of antibacterial nano filter membrance Download PDFInfo
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- CN101298026A CN101298026A CNA2008100324151A CN200810032415A CN101298026A CN 101298026 A CN101298026 A CN 101298026A CN A2008100324151 A CNA2008100324151 A CN A2008100324151A CN 200810032415 A CN200810032415 A CN 200810032415A CN 101298026 A CN101298026 A CN 101298026A
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Abstract
The invention relates to a method for preparing an antibacterial nanofiltration membrane, in particular to a method for preparing an antibacterial nanofiltration membrane by adopting a complex containing silver polyelectrolyte and utilizing a layer upon layer electrostatic self-assembly technique, which pertains to the technical field of filtration and separation. The preparation method of the antibacterial nanofiltration membrane is characterized in that: the antibacterial silver containing nanofiltration membrane is prepared first by alternate deposition of a silver containing polycation solution on the surface of a basement membrane and then by in situ reduction of a reducing agent; the preparation process comprises the steps of: (1) the preprocessing of the polysulfone ultrafiltration membrane of the basement membrane; (2) the generation of the primary lamella of polyelectrolyte on the surface of the basement membrane; (3) the preparation of an antibacterial superfine separation layer. The fine membrane is immersed into the silver containing polycation solution, namely the poly allylamine hydrochloride-silver chloride solution, for 5 to 30 minutes for several times and then immersed into a reducing agent NaBH4 solution for 2 to 24 hours and at last the antibacterial nanofiltration membrane is obtained. The nanofiltration membrane has restraining and sterilizing bacteria functions towards microorganism in water and the antibacterial rate reaches more than 99.5 percent.
Description
Technical field
The present invention relates to a kind of preparation method of antibacterial nano filter membrance, specifically, relate to adopt the argentiferous polyelectrolyte complex compound and utilize the layer upon layer electrostatic self-assembling technique to prepare the method for antibacterial nano filter membrance, belong to the membrane filtration separation technology field.
Background technology
NF membrane is meant that in process of osmosis rejection is about the film of 1nm greater than 95% smallest molecule size, and operating pressure should be less than 1.50MPa, and molecular cut off is 200～1000.Most of NF membrane is a charged membrane, and the separating behavior of inorganic salts is subjected to the control influence of chemical potential gradient and potential gradient simultaneously, i.e. the state-of-charge of the separating behavior of NF membrane and its charge, solute and interaction all has relation.NF membrane hinders the infiltration of multivalent ion, so have higher charged solute (as ion and charged organic molecule) rejection under the low-pressure very much by electrostatic interaction.
The stalling characteristic of NF membrane is that reverse osmosis membrane and milipore filter can't replace, and has the total energy-efficient characteristics of membrane technology again, is one of membrane technology of first developing of countries in the world in recent years.The eighties in 20th century, U.S. Filmtec company develops the NF membrane of models such as NF-40, NF-50, NF-70 in succession.Because extensive market, the numerous and confused organizational strength in countries in the world is put in the exploitation of nanofiltration.The kind of NF membrane constantly increases, and performance improves constantly.Membrane material has cellulose acetate, aromatic polyamides, sulfonated polyether sulfone etc.From the engineering of water treatment example of nanofiltration successful operation at home and abroad, its separating property is good, and stable effluent quality is reliable, and energy consumption low, have a Technological Economy preferably.But present employed NF membrane does not all possess antibiotic or sterilizing ability, has a major defect in application process, in use, the micropore of film is easily blocked by solids in the water and microorganism, needs flushing constantly, has a strong impact on the service efficiency of film; In storage and equipment stoppage in transit process, very easily be subjected to the infringement of microorganism in the water, have a strong impact on the service life of film.
Therefore, people adopt the whole bag of tricks to improve antibiotic, the antifouling property of film in recent years.As application number is that 2002013972 United States Patent (USP) has been put down in writing a kind of preparation method of sticking the antibacterial film of water-insoluble propolis on basement membrane, and the adsorptivity of utilizing propolis is with the bacterium in the water, virus sweep.Its shortcoming is bacterium, virus thoroughly can not be removed, and will handle after the propolis adsorption capacity reaches capacity again and could utilize again, uses comparatively trouble.Patent CN100335156C utilizes phase inversion to prepare nano antiseptic material-polysulphone composite microporous filter film, in the process of membrane filtration, can play the effect of sterilizing.Patent CN101053782A makes NF membrane have antibacterial, sterilizing function by introduce the antimicrobial nano particle of modifying through plasma chemistry in cellulose acetate nano filter-membrane, the antimicrobial erosion of energy, and its shortcoming is a complicated process of preparation.
Summary of the invention
The purpose of this invention is to provide a kind of restraining and sterilizing bacteria function that has, and can resist the preparation method of antibiotic NF membrane of the superthin layer structure of microbial attack.
The preparation method of a kind of antibacterial nano filter membrance of the present invention is characterized in that: said polycation solution by argentiferous and polyanion solution are at the alternating deposit of membrane surface, and the method with the reducing agent in-situ reducing makes the argentiferous NF membrane with anti-microbial property again; The process and the step of its preparation method are as follows:
A. the pre-treatment of basement membrane: after with pure water basement membrane being cleaned up, be placed on again and soak 5～10 hours in the pure water; Described basement membrane is a polysulphone super-filter membrane;
B. the generation of membrane surface polyelectrolyte primary layer: above-mentioned treated basement membrane was immersed in the polyanion solution 5～30 minutes,, and soaked 5～30 minutes, form electronegative rete in membrane surface subsequently with the pure water washing; And then in the immersion said polycation solution 5～30 minutes, subsequently with the pure water washing, and soaked 5～30 minutes; Repeat above-mentioned steps, until the polyelectrolyte primary layer that obtains the required number of plies; The number of plies is 2～10 bilayers;
Described polyanion solution is the styrene sulfonic acid sodium solution, and its concentration is 0.01～0.05mol/L, contains the NaCl of 0.5～2.5mol/L, and the pH value is 2～3; Perhaps be sodium polyacrylate solution, its concentration is 0.001～0.005mol/L, and the pH value is 4～5;
Described said polycation solution is a diallyl dimethyl ammoniumchloride solution, and its concentration is 0.01～0.05mol/L, contains the NaCl of 0.5～2.5mol/L, and the pH value is 5～6;
C. the preparation of antibiotic ultra-thin separating layer: have the film of polyelectrolyte primary layer to immerse in the described polyanion solution 5～30 minutes above-mentioned length,, and soaked 5～30 minutes with the pure water washing; Immersed again in the said polycation solution of argentiferous 5～30 minutes, and, and soaked 5～30 minutes subsequently with the pure water washing; Repeat above-mentioned steps, until obtaining the required number of plies; The number of plies is 2～10 bilayers; And then put it into reducing agent NaBH
4Soaked in the solution 2～24 hours; NaBH
4Concentration be 1～10mmol/L; In pure water, soaked again 2～10 hours subsequently, promptly make antibacterial nano filter membrance at last;
Described argentiferous said polycation solution is poly-propyl ammonium chloride-silver chlorate solution; Wherein contain poly diallyldimethylammonium chloride 5～15mmol/L, AgNO
30.5～5mmol/L.
Poly diallyldimethylammonium chloride and AgNO
3Following reaction can take place:
The present invention compares with existing other preparation method, has that technology is simple, the advantage of simple operation.
Antibacterial nano filter membrance of the present invention has following several respects characteristics:
1. prepare the ultra-thin separating layer of NF membrane by the layer upon layer electrostatic self-assembling technique, its structure is controlled, can be according to different performance requirements, and the ultra-thin separating layer of nanofiltration of preparation different structure, excellent performance;
2. prepared argentiferous NF membrane among the present invention, silver particles is evenly distributed in superthin layer, and particle diameter is 100～200nm;
3. the adding of silver particles makes NF membrane have antibacterial, bactericidal property to microorganism in the water.Anti-microbial property test shows to film is about 1.5 * 10 in the 50mL total plate count
4In the water of CFU/mL, its antibiotic rate reaches 99.5%, and antibiotic rate descends less than 0.5% in 15 days.Illustrate that the prepared NF membrane of the present invention has excellent anti-microbial property, and antibiotic property is lasting.
The specific embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
1. after polyether sulfone basement membrane use pure water being cleaned up, be placed in the pure water and soaked 10 hours, water was changed once every 2 hours in the centre.
2. the basement membrane of handling well in the step 1 being immersed concentration is 20min in the 0.05mol/L kayexalate solution, uses the pure water washing, soaks 20min; Immersing concentration is 20min in the 0.05mol/L diallyl dimethyl ammoniumchloride solution, uses the pure water washing, soaks 20min.Repeat above-mentioned steps, until the polyelectrolyte primary layer that obtains alternately forming by 3 strata SSS retes and 3 strata diallyldimethylammonium chloride retes respectively.
3. the film of handling well in the step 2 being immersed concentration is 20min in the 0.002mol/L sodium polyacrylate solution, uses the pure water washing, soaks 20min; Immerse poly diallyldimethylammonium chloride-silver chlorate (10mmol/LPAH+0.5mmol/LAgNO again
3) middle 20min, use the pure water washing, soak 20min.Repeat above-mentioned steps, until the antibiotic superthin layer that obtains alternately forming by 5 strata PAA retes and 5 stratas allyl ammonium chloride-silver chlorate rete respectively.
With the film handled well in the step 3 at reducing agent NaBH
4Soak 12h in the solution, in water, soaked 2 hours again, promptly make corresponding composite nanometer filtering film.
The nanofiltration performance test of the NF membrane that present embodiment makes: test pressure is 5.0bar, and face test fluid flow velocity remains on 100mL/min, to eliminate concentration polarization.To 1000mg/L Na
2SO
4The solution water flux be 0.36m
3M
-2Day
-1, the ion rejection is 70%; To 1000mg/L MgCl
2The solution water flux is 0.35m
3M
-2Day
-1, the ion rejection is 78%; To 1000mg/L MgSO
4The solution water flux is 0.22m
3M
-2Day
-1, the ion rejection is 70%.
The anti-microbial property test of the NF membrane that present embodiment makes in water: the film of diameter 25mm is 1.5 * 10 to the 50mL total number of bacteria
3The water sample sterilizing rate of CFU/mL is 100%, is 1.5 * 10 to the 50mL total number of bacteria
4The water sample sterilizing rate of CFU/mL is 99.5%, is 5.5 * 10 to the 50mL total number of bacteria
4The water sample sterilizing rate of CFU/mL is 98%, and bactericidal property is almost constant within 15 days.
Embodiment 2
1. after polyether sulfone basement membrane use pure water being cleaned up, be placed in the pure water and soaked 10 hours, water was changed once every 2 hours in the centre.
2. the basement membrane of handling well in the step 1 being immersed concentration is 20min in the 0.05mol/L kayexalate solution, uses the pure water washing, soaks 20min; Immersing concentration is 20min in the 0.05mol/L diallyl dimethyl ammoniumchloride solution, uses the pure water washing, soaks 20min.Repeat above-mentioned steps, until the polyelectrolyte primary layer that obtains alternately forming by 3 strata SSS retes and 3 strata diallyldimethylammonium chloride retes respectively.
3. the film of handling well in the step 2 being immersed concentration is 20min in the 0.002mol/L sodium polyacrylate solution, uses the pure water washing, soaks 20min; Immerse poly diallyldimethylammonium chloride-silver chlorate (10mmol/LPAH+0.5mmol/LAgNO again
3) middle 20min, use the pure water washing, soak 20min.Repeat above-mentioned steps, until the antibiotic superthin layer that obtains alternately forming by 3 strata PAA retes and 3 stratas allyl ammonium chloride-silver chlorate rete respectively.
With the film handled well in the step 3 at reducing agent NaBH
4Soak 12h in the solution, in water, soaked 2 hours again.
5. the film of handling well in the step 4 being immersed concentration is 20min in the 0.05mol/L kayexalate solution, uses the pure water washing, soaks 20min, promptly makes corresponding composite nanometer filtering film.
The nanofiltration performance test of the NF membrane that present embodiment makes: test pressure is 5.0bar, and face test fluid flow velocity remains on 100mL/min, to eliminate concentration polarization.To 1000mg/L Na
2SO
4The solution water flux be 0.65m
3M
-2Day
-1, the ion rejection is 93%; To 1000mg/L MgCl
2The solution water flux is 0.68m
3M
-2Day
-1, the ion rejection is 15%; To 1000mg/L MgSO
4The solution water flux is 0.55m
3M
-2Day
-1, the ion rejection is 75%.
The anti-microbial property test of the NF membrane that present embodiment makes in water: the film of diameter 25mm is 1.5 * 10 to the 50mL total number of bacteria
3The water sample sterilizing rate of CFU/mL is 100%, is 1.5 * 10 to the 50mL total number of bacteria
4The water sample sterilizing rate of CFU/mL is 99.5%, is 5.5 * 10 to the 50mL total number of bacteria
4The water sample sterilizing rate of CFU/mL is 98%, and bactericidal property is almost constant within 15 days.
Claims (1)
1, a kind of preparation method of antibacterial nano filter membrance is characterized in that: said polycation solution by argentiferous and polyanion solution are at the alternating deposit of membrane surface, and the method with the reducing agent in-situ reducing makes the argentiferous NF membrane with anti-microbial property again; The process and the step of its preparation method are as follows:
A. the pre-treatment of basement membrane: after with pure water basement membrane being cleaned up, be placed on again and soak 5～10 hours in the pure water; Described basement membrane is a polysulphone super-filter membrane;
B. the generation of membrane surface polyelectrolyte primary layer: above-mentioned treated basement membrane was immersed in the polyanion solution 5～30 minutes,, and soaked 5～30 minutes, form electronegative rete in membrane surface subsequently with the pure water washing; And then in the immersion said polycation solution 5～30 minutes, subsequently with the pure water washing, and soaked 5～30 minutes; Repeat above-mentioned steps, until the polyelectrolyte primary layer that obtains the required number of plies; The number of plies is 2～10 bilayers;
Described polyanion solution is the styrene sulfonic acid sodium solution, and its concentration is 0.01～0.05mol/L, contains the NaCl of 0.5～2.5mol/L, and the pH value is 2～3; Perhaps be sodium polyacrylate solution, its concentration is 0.001～0.005mol/L, and the pH value is 4～5;
Described said polycation solution is a diallyl dimethyl ammoniumchloride solution, and its concentration is 0.01～0.05mol/L, contains the NaCl of 0.5～2.5mol/L, and the pH value is 5～6;
C. the preparation of antibiotic ultra-thin separating layer: have the film of polyelectrolyte primary layer to immerse in the described polyanion solution 5～30 minutes above-mentioned length,, and soaked 5～30 minutes with the pure water washing; Immersed again in the said polycation solution of argentiferous 5～30 minutes, and, and soaked 5～30 minutes subsequently with the pure water washing; Repeat above-mentioned steps, until obtaining the required number of plies; The number of plies is 2～10 bilayers; And then put it into reducing agent NaBH
4Soaked in the solution 2～24 hours; NaBH
4Concentration be 1～10mmol/L; In pure water, soaked again 2～10 hours subsequently, promptly make antibacterial nano filter membrance at last;
Described argentiferous said polycation solution is poly-propyl ammonium chloride-silver chlorate solution; Wherein contain poly diallyldimethylammonium chloride 5～15mmol/L, AgNO
30.5～5mmol/L.
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| CNA2008100324151A CN101298026A (en) | 2008-01-08 | 2008-01-08 | Preparation of antibacterial nano filter membrance |
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ID=40078058
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| CN101829509A (en) * | 2010-05-11 | 2010-09-15 | 杭州水处理技术研究开发中心有限公司 | Preparation method of antibacterial porous membrane |
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| CN102114388A (en) * | 2011-01-13 | 2011-07-06 | 哈尔滨工程大学 | Bacteriostatic nano silver polyvinyl chloride filter membrane and preparation method thereof |
| CN102114389A (en) * | 2011-01-13 | 2011-07-06 | 哈尔滨工程大学 | Silver-loaded nano-titanium dioxide/polrvinyl chloride membrane and preparation method thereof |
| CN102205209A (en) * | 2010-03-30 | 2011-10-05 | 广州美能材料科技有限公司 | Antibacterial macromolecular ultra-filtration membrane and preparation method thereof |
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| CN107486026B (en) * | 2017-08-18 | 2021-04-02 | 清华大学 | Separation membrane resistant to biological contamination and method for preparing same |
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