CN1683061A - Nano antiseptic material-polysulphone composite microporous filter film and its preparing method - Google Patents
Nano antiseptic material-polysulphone composite microporous filter film and its preparing method Download PDFInfo
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- CN1683061A CN1683061A CN 200510051363 CN200510051363A CN1683061A CN 1683061 A CN1683061 A CN 1683061A CN 200510051363 CN200510051363 CN 200510051363 CN 200510051363 A CN200510051363 A CN 200510051363A CN 1683061 A CN1683061 A CN 1683061A
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Abstract
The present invention relates to a kind of composite nano antiseptic material-microporous polysulfone filter film and its preparation process. The microporous filter film consists of polysulfone and nano antiseptic material as well as additive. The preparation process includes the following steps: compounding mixed casting solution with polysulfone, solvent, additive and antiseptic material; letting stand to debubble and filtering to eliminate impurity; scraping film in dry/wet phase converting method and soaking into solidifying bath to form film; and soaking in pure water. The composite nano antiseptic material-microporous polysulfone filter film can filter and sterilize simultaneously while avoiding film pollution. It may be used in medicine production and drinking water purification to raise water quality.
Description
Technical field
The present invention relates to a kind of nano antiseptic material-polysulphone composite microporous filter film and preparation method thereof, relating in particular to the polysulfones is filmogen, is composite microporous filter film of property-modifying additive and preparation method thereof with the nano anti-biotic material.
Background technology
Storage of water or pipeline water often have growing of various bacteriums, virus; in order to suppress their growth; people have taked a lot of measures; add disinfectant in the wherein oriented water; as chlorine; or heating, disinfection by ultraviolet light etc., or the method that adopts ultrafiltration (UF), micro-filtration membrane separation techniques such as (MF) to filter.Yet Xiang Shuizhong adds disinfectant can cause in various degree side effect to human body, and heating disinfection can make the water treatment facilities structure become complicated, the increase expense.
Membrane separation technique such as UF, MF has been widely used in fields such as water treatment and chemical industry, medicine, electronics, environmental project and bioengineering owing to have advantages such as energy consumption is low, separative efficiency is high, simple, easy to operate.In numerous macromolecule member materials, polysulfones is a kind of good heatproof, corrosion-resistant, pH accommodation is wide, mechanical strength is high membrane for water treatment material.But present employed UF film, MF film generally do not have antibacterial ability, and in use, face is multiplied bacterium and contaminated easily, cause performance to descend, and finally influence the long bacterium in the back side of quality, the especially film of product water, influence bigger.
Therefore; in recent years; people are in research; adopting the whole bag of tricks to improve antibiotic, the antifouling property of UF film, MF film, is that 20020139732 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 as application number, and the absorption property that utilizes propolis is with the bacterium in the water, virus sweep; antibacterial film can be placed ethanolic solution after the use; contaminated propolis is eluted, thereby basement membrane is protected, prolong the service life of film.Its shortcoming is bacterium, virus thoroughly can not be removed, and also needs to handle after the propolis adsorption capacity reaches capacity again, and can utilize again, uses comparatively trouble.
Nano material has many characteristics such as particle size is little, specific area is big, surface-active height, and in recent years, people begin to utilize nano material that original material is carried out modification, make the gained material have the excellent properties of the uniqueness that is different from original material.Delivered with nanometer Y-Al as, China " water technology) " Vol.6.No.4. (2004)
2O
3Modification PVDF hollow-fibre membrane, the result shows, has added nanometer γ-Al
2O
3The porosity of the hollow-fibre membrane of particle is enhanced than common PVDF hollow-fibre membrane; The mechanical property of film also has bigger improvement, and maximum stress and fracture strength are respectively from 3.35N/mm
2And 3.09N/mm
2Bring up to 3.58N/mm
2And 3.41N/mm
2" (polymer material science and engineering) " Vol.18.No.5. (2002) has then delivered with nanometer SiO
2Modified PVA prepares the method for composite hyperfiltration membrane, and the result shows, has added nanometer SiO
2Behind the particle, the withstand voltage properties of film all is improved, and in addition, the antipollution experimental study shows that composite membrane has the better pollution resistance ability.All do not mention the anti-microbial property of film in the above bibliographical information." coatings industry) " Vol.34.No.5. (2004) has reported nano-TiO
2The preparation of compound organic antibacterial film coating and performance characterization, wherein organic matter is the styrene-propene acid polymer, and experimental result shows that this organic coating film has good antibiotic/biocidal efficacies, but do not make water treatment MF membrane material, do not study its application in water treatment yet.
Summary of the invention
The purpose of this invention is to provide a kind of antibiotic, resistant to pollution nano antiseptic material-polysulphone composite microporous filter film and preparation method thereof, in membrane filtration, play sterilization, simultaneously, prevent film surface pollution, the biological pollution of water is produced in control, reaches to improve the purpose of producing water quality.
For achieving the above object, the invention provides a kind of nano antiseptic material-polysulphone composite microporous filter film, form with the nano anti-biotic material that mixes by the polysulfones that is dissolved in the selected solvent, wherein, the mass percent of polysulfones in mixture is 5%～25%, nano anti-biotic material accounts for 0.1%～5% of polysulfones content, also has 2%～18% additive in the mixture, and all the other are solvent.
Above-mentioned nano antiseptic material-polysulphone composite microporous filter film, wherein said nano anti-biotic material are one or more mixing wherein of nano titanium oxide, Nano Silver, nanometer zinc and nanometer copper; The mass percent of described polysulfones in mixture is preferably 8%～20%; The percentage that described nano anti-biotic material accounts for polysulfones content is preferably 0.25%～2.75%.
The preparation method of above-mentioned nano antiseptic material-polysulphone composite microporous filter film may further comprise the steps:
1) with the oven dry of polysulfones macromolecular material, the polysulfones of drying is dissolved in the selected solvent, adds additive, stir, obtain the polymer solution of clear;
2) will be in advance in certain solvent the scattered nano anti-biotic material of ultrasonic wave under the ultrasonic wave effect, progressively add in the polymer solution, continue to stir, obtain mixing casting solution;
3) standing and defoaming removes by filter impurity;
4) with doing/wetting phase conversion method knifing, immerse film forming in the coagulating bath;
5) diaphragm after the film forming soaks in pure water, and wherein solvent, additive gone to the greatest extent.
The above-mentioned method for preparing nano antiseptic material-polysulphone composite microporous filter film, the solvent that wherein said step 1) adopts are a kind of in dimethyl formamide, dimethylacetylamide, the N-methyl pyrrolidone or two kinds mixed solvent wherein.The additive that adopts in the described step 1) is one or more the mixture in polyethylene glycol, polypropylene glycol, glycerine, water, ethanol, acetone, the PVP.Described usefulness is done/wetting phase conversion method knifing, and evaporation time is 5～20 seconds, 25～35 ℃ of evaporating temperatures, envionmental humidity 40%～60%.The coagulating bath of adopting in the described step 4) is that percentage by volume is 5%～60% ethanol water, 25～40 ℃ of coagulation bath temperatures.
The present invention compared with prior art has tangible advantage and beneficial effect.By above technical scheme as can be known, adopt the nano antiseptic material-polysulphone composite microporous filter film of preparation method's preparation of the present invention, in membrane filtration, play sterilization, simultaneously, prevent film surface pollution.
The MF film that is made by the inventive method can be applied to produce the membrane separation plant that carries out purifying of drinking water under water for pharmaceutical purposes and military going up " three the is anti-" condition better, it has prevented the biological pollution that water is produced in the growth of face mycoderm, control, reaches and improves the purpose of producing water quality.
Nano antiseptic material-polysulphone composite microporous filter film of the present invention has the characteristics of the following aspects:
1. the interpolation of hydrophilic nano anti-biotic material has strengthened the hydrophily of compound MF film, promotes the transmission of water in film surface and film, has strengthened the resistant to pollution ability of film.
2. the interpolation of nano material can influence the forming process of film, thereby influence the aperture and the porosity of film, as, the mass percent of casting solution is a polysulfones 8%～12%, pore-foaming agent PVP addition is 10%～15%, the nano anti-biotic material addition is 0.25%～5% of a polysulfones content, can be one or more mixing in the nano anti-biotic materials such as nano titanium oxide, Nano Silver, nanometer zinc or nanometer copper; All the other are solvent, and then average pore size is at 0.1 μ m～0.5 μ m, and porosity owing to the variation of aperture and porosity, makes the permeability rate generation respective change of film, its excursion 50L/m then 82%～87%
2Min～300L/m
2Min (0.1MPa) illustrates that the nano material of certain addition can obtain the diffusion barrier of function admirable.
3. add the mechanical property that nano material can be improved film, the mechanical property of nano antiseptic material-polysulphone composite microporous filter film is compared with the mechanical property of common polysulfone millipore filtering membrane and is enhanced, and is example with embodiment 1, and its maximum stress is from 0.85N/mm
2Bring up to 1.29N/mm
2, fracture strength is then from 0.84N/mm
2Bring up to 1.28N/mm
2
4. compound MF film anti-microbial property is given in the interpolation of nano anti-biotic material.In sterile petri dish, add sterilized meat extract peptone agar medium, make it to cover whole culture dish bottom, evenly coat a certain amount of assorted bacterium bacterium liquid again, concentration is about 10cfu/ml, embodiment 1 compound MF membrane sample is cut into the diaphragm of the about 5mm size of diameter, is put on the culture medium that has solidified, cultivate down for 37 ℃, 24h observes composite membrane bacterial growth situation on every side later on, measures inhibition zone.Measurement result, the compound MF film that has added nano anti-biotic material has tangible antibacterial effect, and the inhibition zone scope is diaphragm periphery 1～2mm, and Zu common polysulfones MF film does not then have antibacterial effect in contrast.
The specific embodiment
Now the present invention will be described in detail with specific embodiment.
Nano antiseptic material-polysulphone composite microporous filter film of the present invention is prepared by the following method: the polysulfones macromolecular material is dried 4～6h down at 120 ℃, the polysulfones of oven dry is dissolved in the selected solvent, add additive again, stir with agitator, obtain the polymer solution of clear, with in advance in certain solvent the scattered nano anti-biotic material of ultrasonic wave under the ultrasonic wave effect, progressively add in the polymer solution, continue to stir 30min, obtain mixing casting solution, leave standstill the above deaeration of 24h, filtration is to remove impurity, then with doing/wetting phase conversion method knifing, immerse film forming in the coagulating bath, diaphragm soaks in pure water more than the 48h, with solvent wherein, additive goes to the greatest extent.
Wherein, the concrete steps of preparation casting solution are: the polysulfones macromolecular material of inherent viscosity 0.55～0.65 is dried 4～6h down at 120 ℃, the polysulfones of oven dry is dissolved in the solvent, add the PVP additive again, stir with agitator, obtain the clear polymer solution, with in advance in certain solvent the scattered nano anti-biotic material of ultrasonic wave under the ultrasonic wave effect, progressively add in the polymer solution, continue to stir 30min, must mix casting solution.Wherein, the mass percent of casting solution is a polysulfones 5%～25%, is preferably 8%～20%; In addition, in casting solution, can also add a certain amount of pore-foaming agent, aperture and pore-size distribution with preliminary control diffusion barrier, addition is 2%～18%, be preferably 5%～15%, pore-foaming agent can be one or more the mixture in the following substances, as polyethylene glycol, polypropylene glycol, glycerine, water, ethanol, acetone, PVP etc.; The nano anti-biotic material addition is 0.1%～5% of a polysulfones content, is preferably 0.25%～2.75%, can be one or more mixing in the nano anti-biotic materials such as nano titanium oxide, Nano Silver, nanometer zinc and nanometer copper; All the other are solvent, and solvent is a kind of in dimethyl formamide, dimethylacetylamide, the N-methyl pyrrolidone or two kinds mixed solvent wherein.
The concrete steps of system film are: mix casting solution and leave standstill the above deaeration of 24h, filtration is to remove impurity, then with doing/wetting phase conversion method knifing, evaporation time 5～20 seconds, 25～35 ℃ of evaporating temperatures, envionmental humidity 40%～60% immerses film forming in the coagulating bath, coagulating bath is that percentage by volume is 5%～60% ethanol water, 25～40 ℃ of coagulation bath temperatures.
The concrete steps of washing are: diaphragm soaks 48h in pure water, change water one time every 5h, so that wherein solvent, additive are gone to the greatest extent.
Following mask body provides several embodiment and comparative example:
Embodiment 1
With the mass percent of oven dry is that 10% polysulfones (is called for short PS, technical grade, Shanghai plastics industry affiliated company dawn chemical plant produces), be dissolved in mass percent and be 65% solvent N, dinethylformamide (is called for short DMF, analyze pure, the Tianjin North Star Hua chemical reagent factory that jumps), add mass percent again and be 12% macromolecule pore-foaming agent PVP and (be called for short PVP, K-30, molecular weight 40,000, analyze pure, U.S.'s import, Shanghai reagent purchasing station packing), stir with agitator, obtain the polymer solution of clear, to be the scattered nano silver antimicrobials that accounts for PS content 2.5% (technical grade, average grain diameter 8nm, Jiangsu Hehai Nanometer Technology Co., Ltd.) in 13% the solvent at mass percent in advance, under the ultrasonic wave effect, progressively add in the polymer solution, continue to stir 30min, must mix casting solution, leave standstill the above deaeration of 24h, filtration is to remove impurity, then with doing/wetting phase conversion method knifing evaporation time 10 seconds, 30 ℃ of evaporating temperatures, envionmental humidity 45%, immerse film forming in the coagulating bath, coagulating bath is that percentage by volume is 10% ethanol water, 28 ℃ of coagulation bath temperatures.Diaphragm soaks 48h in pure water, change water one time every 5h, so that wherein solvent, additive are gone to the greatest extent.The average pore size of the Nano Silver-polysulphone composite microporous filter film of gained is 0.15 μ m, and porosity is 86.2%, and the pure water permeation flux is 70L/m
2Min (0.1MPa), maximum stress 1.29N/mm
2, fracture strength 1.28N/mm
2, antibacterial experiment shows that the inhibition zone scope is diaphragm periphery 1～1.90mm.
Embodiment 2
With mass percent is that to be dissolved in mass percent be in 68% the solvent DMF for 10% PS, add mass percent again and be 12% macromolecule pore-foaming agent PVP, stir with agitator, obtain the polymer solution of clear, to be the scattered nano titanium oxide that accounts for PS content 0.5% (Zhejiang Zhoushan Tomorrow Nanomaterials Co., Ltd in 10% the solvent at mass percent in advance, technical grade, average grain diameter 5nm), under the ultrasonic wave effect, progressively add in the polymer solution, press the same method system film of embodiment 1.The average pore size of the nano titanium oxide-polysulphone composite microporous filter film of gained is 0.17 μ m, and porosity is 86.2%, and the pure water permeation flux is 120L/m
2Min (0.1MPa), maximum stress 1.14N/mm
2, fracture strength 1.14N/mm
2Antibacterial experiment shows, 48W ultra violet lamp 30min, and the inhibition zone scope is diaphragm periphery 0.7～1.74mm.
Comparative example 1
With the mass percent of oven dry is that to be dissolved in mass percent be in 78% solvent DMF for 10% PS, add mass percent again and be 12% macromolecule pore-foaming agent PVP, stir with agitator, obtain the polymer solution of clear, press the same method system film of embodiment 1.The average pore size of the PS MF film of gained is 0.12 μ m, and porosity is 85.3%, and the pure water permeation flux is 50L/m
2Min (0.1MPa), maximum stress 0.85N/mm
2, fracture strength 0.84N/mm
2Antibacterial experiment shows not have antibiotic effect.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified to the equivalent embodiment of equivalent variations, but every technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (9)
1, a kind of nano antiseptic material-polysulphone composite microporous filter film, it is characterized in that: it is made up of with the nano anti-biotic material that mixes the polysulfones that is dissolved in the selected solvent, wherein, the mass percent of polysulfones in mixture is 5%～25%, nano anti-biotic material accounts for 0.1%～5% of polysulfones content, also have 2%～18% additive in the mixture, all the other are solvent.
2, nano antiseptic material-polysulphone composite microporous filter film according to claim 1 is characterized in that described nano anti-biotic material is one or more mixing wherein of nano titanium oxide, Nano Silver, nanometer zinc and nanometer copper.
3, nano antiseptic material-polysulphone composite microporous filter film according to claim 1 and 2 is characterized in that the mass percent of described polysulfones in mixture is preferably 8%～20%.
4, nano antiseptic material-polysulphone composite microporous filter film according to claim 1 and 2 is characterized in that the percentage that described nano anti-biotic material accounts for polysulfones content is preferably 0.25%～2.75%.
5, a kind of method for preparing nano antiseptic material-polysulphone composite microporous filter film as claimed in claim 1 is characterized in that may further comprise the steps:
1) with the oven dry of polysulfones macromolecular material, the polysulfones of drying is dissolved in the selected solvent, adds additive, stir, obtain the polymer solution of clear;
2) will be in advance in certain solvent the scattered nano anti-biotic material of ultrasonic wave under the ultrasonic wave effect, progressively add in the polymer solution, continue to stir, obtain mixing casting solution;
3) standing and defoaming removes by filter impurity;
4) with doing/wetting phase conversion method knifing, immerse film forming in the coagulating bath;
5) diaphragm after the film forming soaks in pure water, and wherein solvent, additive gone to the greatest extent.
6, the method for preparing nano antiseptic material-polysulphone composite microporous filter film according to claim 5 is characterized in that: the solvent that adopts in the described step 1) is a kind of in dimethyl formamide, dimethylacetylamide and the N-methyl pyrrolidone or two kinds mixed solvent wherein.
7, the method for preparing nano antiseptic material-polysulphone composite microporous filter film according to claim 5 is characterized in that: the additive that adopts in the described step 1) is one or more the mixture in polyethylene glycol, polypropylene glycol, glycerine, water, ethanol, acetone and the PVP.
8, according to claim 5, the 6 or 7 described methods that prepare nano antiseptic material-polysulphone composite microporous filter film, it is characterized in that: the usefulness described in the step 3) is done/wetting phase conversion method knifing, its evaporation time is 5～20 seconds, 25～35 ℃ of evaporating temperatures, envionmental humidity 40%～60%.
9, according to claim 5, the 6 or 7 described methods that prepare nano antiseptic material-polysulphone composite microporous filter film, it is characterized in that: the coagulating bath of adopting in the described step 4) is that percentage by volume is 5%～60% ethanol water, 25～40 ℃ of coagulation bath temperatures.
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| CN115093703A (en) * | 2022-06-02 | 2022-09-23 | 湖南美柏生物医药有限公司 | Polymer carrier with nano-pore structure for cell culture and preparation method and application thereof |
| CN115093703B (en) * | 2022-06-02 | 2024-02-02 | 湖南美柏生物医药有限公司 | Polymer carrier with nano-pore structure for cell culture and preparation method and application thereof |
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