CN114377554B - Preparation method of antibacterial polytetrafluoroethylene air filtering membrane - Google Patents
Preparation method of antibacterial polytetrafluoroethylene air filtering membrane Download PDFInfo
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- CN114377554B CN114377554B CN202210027028.9A CN202210027028A CN114377554B CN 114377554 B CN114377554 B CN 114377554B CN 202210027028 A CN202210027028 A CN 202210027028A CN 114377554 B CN114377554 B CN 114377554B
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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
- 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
- B01D71/36—Polytetrafluoroethene
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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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Abstract
The invention discloses a preparation method of a bacteriostatic polytetrafluoroethylene air filtering membrane, which comprises the following steps: dissolving proper amount of Polyethylenimine (PEI) in a certain amountStirring uniformly in ethanol solution at room temperature; pouring the mixture on the surface of a Polytetrafluoroethylene (PTFE) film placed on a vacuum filtration bottle, and standing for a period of time; a certain amount of ferric trichloride (FeCl) 3 ) Mixing ethanol solution and Tannic Acid (TA) ethanol solution with water, pouring the mixture into the surface of a PTFE membrane, standing for a period of time, allowing the mixed solution to permeate the PTFE membrane by a suction filter, washing the PTFE membrane by deionized water, and drying the PTFE membrane in an oven; the dried PTFE film is placed in a neomycin sulfate (NCS) aqueous solution with a certain concentration for 2-24 hours, and then is placed in an oven for drying. The preparation process is simple and convenient, the operation is simple, and the preparation method is nontoxic and environment-friendly; a bacteriostatic polytetrafluoroethylene air filtering membrane has good air permeability, hydrophobicity and antibacterial property.
Description
Technical Field
The invention relates to the technical field of organic films and the field of gas separation, in particular to a preparation method of a polytetrafluoroethylene gas separation film with antibacterial property.
Background
The quality of air is closely related to human health. Among the various factors affecting the air quality, biological contamination by microorganisms such as bacteria and fungi is a non-negligible group. Microbial contamination can cause eye irritation, asthma, allergic dermatitis, allergic pneumonia, and infectious diseases in people, and severe cases can lead to death. Some microorganisms exist in the air in the form of aerosol under certain conditions, and are inhaled by human bodies, so that the human health is endangered. Especially in the present environment, as new coronaries spread worldwide, people need to cope with microbial contamination in the air and avoid virus infection from person to person. So that the antibacterial agent gradually goes into eyes of people along with the development of society.
Antibacterial methods include ultraviolet sterilization, gas sterilization, ultra-high temperature sterilization, etc., but these are not suitable for use in daily life, such as ultraviolet sterilization techniques that use specially designed ultraviolet light with high efficiency, high intensity and long life to destroy bacterial (cell) DNA configuration, resulting in bacterial (cell) mutation or death. However, ultraviolet radiation is harmful to living organisms, and if the irradiation intensity is insufficient, the sterilizing effect cannot be achieved. And gas sterilization refers to sterilization using gaseous sterilizing agents (e.g., ethylene oxide, formaldehyde vapor, etc.). Is the most effective means of killing and removing microbial contamination in the air. The gas sterilization speed is high, the efficiency is high, but the sterilizing agent generally has pungent smell, and meanwhile, the problem of secondary pollution exists, and the rest medicaments are directly discharged into the atmosphere, so that the pollution to the surrounding environment is caused. For ultrahigh temperature sterilization, the sensitivity of microorganisms to high temperature is far greater than that of most other substances, so that the ultrahigh temperature short-time sterilization can effectively kill microorganisms in a short time, but the ultrahigh temperature sterilization has strong limitation and is only suitable for products insensitive to temperature.
So with the development of human material technology science and the urgent need of human beings for improving the living environment of the human beings. Antibacterial materials are therefore a major focus in the field of materials. In summary, it is necessary for a gas separation membrane to have a certain antibacterial property, among organic membranes, polytetrafluoroethylene (PTFE) porous membranes exhibit excellent high heat resistance, hydrophobicity and chemical stability, and because the membrane has a large number of micropores, it has a very high specific surface area, so that it has sufficient air permeability and interception of small particles in the air and even microorganisms, but also because it has a large number of micropores and specific surface area, it is easy for PTFE to scale and contaminate microorganisms, so that the service life thereof is reduced.
Therefore, the PTFE membrane is modified so as to achieve an antibacterial effect without affecting the hydrophobicity and air permeability as much as possible. This is necessary in the daily use of PTFE.
Disclosure of Invention
The invention aims to provide a preparation method of a bacteriostatic polytetrafluoroethylene air filtering membrane.
In order to achieve the aim of the invention, the invention adopts the following technical scheme: a preparation method of an antibacterial polytetrafluoroethylene air filtering membrane is characterized by comprising the following steps of: the method comprises the following steps:
1) Dissolving a proper amount of Polyethylenimine (PEI) in a certain amount of ethanol solution, and uniformly stirring at room temperature; pouring the mixture on the surface of a Polytetrafluoroethylene (PTFE) film placed on a vacuum filtration bottle, and standing for a period of time;
2) A certain amount of ferric trichloride (FeCl) 3 ) Mixing ethanol solution and Tannic Acid (TA) ethanol solution with water, pouring the mixture into the surface of a PTFE membrane, standing for a period of time, allowing the mixed solution to permeate the PTFE membrane by a suction filter, washing the PTFE membrane by deionized water, and drying the PTFE membrane in an oven;
3) The dried PTFE film is placed in a neomycin sulfate (NCS) aqueous solution with a certain concentration for 2-24 hours, and then is placed in an oven for drying.
Preferably, the concentration of the PEI ethanol solution is 1-5 mg/mL.
Preferably, the PTFE film has a size of 0.001 to 0.01m 2 The method comprises the steps of carrying out a first treatment on the surface of the The volume of PEI added is 5-30mL, and the standing time on the PTFE membrane is 30-100 s.
Preferably, the FeCl is added 3 The concentration of the ethanol solution is 0.05-0.15 mg/mL, and the adding volume is 30-120 mL.
Preferably, the concentration of the TA ethanol and water mixed solution is 0.1-0.5 mg/mL, and the ratio of water to ethanol in the mixed solution is 1: 50-100 mL, and the adding volume is 30-120 mL.
Preferably, the TA ethanol solution and FeCl are added 3 After the ethanol and the water solution, the standing time on the membrane is 100 to 300 seconds.
Preferably, after the suction filtration is finished, the filter is rinsed 2 to 5 times with 10 to 100mL of deionized water.
Preferably, after the suction filtration is finished, the mixture is baked in an oven at 30-60 ℃ for 30-90min.
Preferably, the PTFE membrane is placed in an aqueous NCS solution of 0.1-0.5g/L for 2-24 hours.
Compared with the prior art, the invention has the beneficial effects that: the preparation process is simple and convenient, the operation is simple, and the preparation method is nontoxic and environment-friendly; a bacteriostatic polytetrafluoroethylene air filtering membrane has good air permeability, hydrophobicity and antibacterial property.
Drawings
The following is a further detailed description of embodiments of the invention with reference to the drawings
FIG. 1 is a graph showing the antibacterial performance of the air filtration membrane in the example.
Detailed Description
The preparation environment of all initial nanofiltration membranes in the invention is as follows: the temperature is 25 ℃, the humidity is 50% and the pressure is normal.
The following description and drawings are provided to illustrate the present invention and not to limit the general inventive concept, but to provide a further understanding of the present invention, by way of example, specific details are set forth in the following description, not to limit the general inventive concept, but to provide a further understanding of the present invention, including the appended claims, without departing from the spirit and scope of the invention.
Examples 1 to 5:
the method comprises the following specific steps:
a certain amount of PEI was dissolved in ethanol to form a solution with a concentration of 0.2mg/mL, and stirred at room temperature. And poured onto the surface of the PTFE membrane and allowed to stand for 30-100 s. FeCl with the concentration of 0.05-0.15 mg/mL 3 Pouring the ethanol solution and the mixed solution of 0.1-0.5 mg/mL TA ethanol and water into the surface of PTFE at the same time, standing for 100-300 s, starting a suction filter, and mixing PEI ethanol solution and FeCl 3 The ethanol solution, TA ethanol and water mixed solution permeate through the PTFE membrane, the PTFE membrane is washed by deionized water, and the PTFE membrane is dried in an oven at 30-60 ℃ for 30-90min.
As in the previous examples, the concentration of PEI was maintained constant, and TA and FeCl were varied 3 0mg/mL,0.02mg/mL,0.04mg/mL,0.1mg/mL,0.2mg/mL of TA ethanol solution and 0mg/mL,0.005mg/mL,0.01mg/mL,0.025mg/mL,0.05mg/mL of FeCl are added, respectively 3 Ethanol solution. Its performance is as follows
Examples 6 to 8:
the method comprises the following specific steps:
a certain amount of PEI was dissolved in ethanol to form a solution with a concentration of 0.2mg/mL, and stirred at room temperature. And poured onto the surface of a PTFE film placed on a vacuum flask, and left standing for 60 seconds. FeCl with concentration of 0-0.05 mg/mL 3 Pouring the ethanol solution and the mixed solution of 0-0.2 mg/mL TA ethanol and water on the surface of PTFE at the same time, standing for 120s, starting a suction filter, and adding PEI ethanol solution and FeCl 3 The ethanol solution, TA ethanol and water mixed solution permeate through the PTFE membrane, the PTFE membrane is taken out, washed with deionized water, and dried in an oven at 40 ℃ for 30-90min. And immersing the dried PTFE in 0.1g/L NCS solution for 2-24h.
As in the above examples, 0.2mg/mL TA ethanol solution and 0.05mg/mL FeCl are preferred 3 And immersed in 0.1g/L NCS, for comparison, PTFE precursor film (example 6), PTFE+TA/FeCl, respectively 3 PEI film (example 7), PTFE+TA/FeCl 3 PEI+NCS film (example 8) As a plate coating count test of E.coli, sterilized samples were placed in disposable dishes in groups, respectively, and 200. Mu.L of 10 concentration was added dropwise to the center of the samples 6 CFU/mL of E.coli bacterial liquid was added to a blank dish at a concentration of 10. Mu.L 6 The CFU/mL bacterial liquid is used as a blank control group, and then a cover film is clamped by sterile forceps to cover the sample, and the bacterial liquid is spread as much as possible by lightly pressing. Placing in a constant temperature incubator at 37 ℃ for standing cultivation for 18h. After the completion of the culture, 100. Mu.L of the dilution was uniformly spread on LB solid medium, respectively. Culturing in a constant temperature incubator at 37 ℃ for 18 hours, taking out, photographing and recording the colony number.
Antibacterial ratio = (1-experimental group bacterial liquid concentration/blank control group bacterial liquid concentration) ×100%
The performance is as follows:
| examples | Bacterial liquid concentration (CFU/mL) | Antibacterial efficiency (%) |
| Blank group | 1.65×10 9 | / |
| 6 | 9.6×10 8 | 41.82 |
| 7 | 1.02×10 9 | 38.18 |
| 8 | 5.0×10 5 | 99.97 |
Claims (8)
1. A preparation method of an antibacterial polytetrafluoroethylene air filtering membrane is characterized by comprising the following steps of: the method comprises the following steps:
1) Dissolving a proper amount of polyethylenimine PEI in a certain amount of ethanol solution, and uniformly stirring at room temperature to obtain a PEI ethanol solution; pouring the mixture on the surface of a polytetrafluoroethylene film placed on a vacuum filtration bottle, and standing for a period of time;
2) To a certain amount of ferric trichloride FeCl 3 Ethanol dissolutionPouring the solution, ethanol and water mixed solution of tannic acid TA into the surface of a polytetrafluoroethylene film, standing for a period of time, allowing the mixed solution to permeate the polytetrafluoroethylene film by using a suction filter, washing the polytetrafluoroethylene film by using deionized water, and drying the polytetrafluoroethylene film in an oven;
3) And (3) placing the dried polytetrafluoroethylene film in a neomycin sulfate NCS aqueous solution with a certain concentration for 2-24 hours, and then placing the polytetrafluoroethylene film in an oven for drying.
2. The method of claim 1, wherein: the concentration of the PEI ethanol solution is 1-5 mg/mL.
3. The method of claim 2, wherein: the size of the polytetrafluoroethylene film is 0.001-0.01m 2; the volume of the PEI ethanol solution is 5-30mL, and the standing time on the polytetrafluoroethylene film is 30-100 s.
4. The method of claim 1, wherein: the FeCl is added in the step 2) 3 The concentration of the ethanol solution is 0.05-0.15 mg/mL, and the adding volume is 30-120 mL.
5. The method of claim 1, wherein: the concentration of the ethanol and water mixed solution added with TA in the step 2) is 0.1-0.5 mg/mL, and the ratio of water to ethanol in the mixed solution is 1: 50-100 mL, and the adding volume is 30-120 mL.
6. The method of claim 4 or 5, wherein: the step 2) is added with the mixed solution of ethanol and water of TA and FeCl 3 After the ethanol solution, the standing time on the membrane is 100 to 300 seconds.
7. The method of claim 6, wherein: after the suction filtration in the step 2), washing with 10-100 mL deionized water for 2-5 times; baking in a baking oven at 30-60 ℃ for 30-90min.
8. The method of claim 1, wherein: in the step 3), the polytetrafluoroethylene film is placed in an NCS aqueous solution with the concentration of 0.1-0.5g/L for 2-24h.
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| CN202210027028.9A CN114377554B (en) | 2022-01-11 | 2022-01-11 | Preparation method of antibacterial polytetrafluoroethylene air filtering membrane |
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| CN114377554B true CN114377554B (en) | 2023-04-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2990786B2 (en) * | 1990-10-31 | 1999-12-13 | エヌオーケー株式会社 | Antimicrobial membrane |
| CN106823865B (en) * | 2017-02-23 | 2020-04-10 | 天津大学 | Aromatic polyamide composite reverse osmosis membrane grafted with fluorocarbon material and aminoglycoside antibiotic and preparation method thereof |
| CN108310983B (en) * | 2018-02-02 | 2021-02-02 | 山西大学 | Preparation and regeneration method of antibacterial and anti-pollution PVDF ultrafiltration membrane |
| CN112023727B (en) * | 2020-08-14 | 2022-07-12 | 万华化学集团股份有限公司 | Anti-pollution antibacterial reverse osmosis membrane, preparation method and application thereof |
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