CN113181771A - Antibacterial ultrafiltration membrane - Google Patents
Antibacterial ultrafiltration membrane Download PDFInfo
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- CN113181771A CN113181771A CN202110636187.4A CN202110636187A CN113181771A CN 113181771 A CN113181771 A CN 113181771A CN 202110636187 A CN202110636187 A CN 202110636187A CN 113181771 A CN113181771 A CN 113181771A
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- CN
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- Prior art keywords
- ultrafiltration membrane
- mos
- porous ball
- polyether sulfone
- honeycomb
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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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
Abstract
The invention discloses an antibacterial ultrafiltration membrane, which adopts Ce-doped MoS2The polyether sulfone membrane is modified as an antibacterial agent, and the preparation process of the ultrafiltration membrane specifically comprises the following steps: (1) weighing sodium molybdate, thiourea, cerium nitrate and diethylenetriamine, dissolving the sodium molybdate, the thiourea, the cerium nitrate and the diethylenetriamine in a glycerol/deionized water solution, uniformly stirring, transferring the mixture into a polytetrafluoroethylene high-temperature reaction hydrothermal kettle, and carrying out microwave hydrothermal reaction to obtain Ce-doped MoS2A honeycomb-shaped porous ball; (2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, blade-coating the mixture on a glass plate, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball. The preparation process of the inventionSimple, low cost, strong antibacterial property and high industrial use value.
Description
Technical Field
The invention belongs to the technical field of ultrafiltration membranes, and particularly relates to Ce-doped MoS2The honeycomb porous ball is used as an antibacterial agent modified polyethersulfone ultrafiltration membrane.
Background
In recent years, the problem of water pollution is more and more serious, various impurities in wastewater cannot be efficiently adsorbed by simple physical treatment, the treatment effect is not satisfactory, and new ions are easily introduced by complex chemical treatment to cause secondary pollution of a water environment. In recent years, the membrane separation technology is widely applied to the field of water treatment, has the advantages of greenness, high efficiency, energy conservation, convenient operation and the like, can filter impurities, and can avoid secondary chemical pollution. However, microorganisms such as bacteria in the wastewater are easy to breed and propagate on the surface of the ultrafiltration membrane, so that the ultrafiltration membrane is damaged, and the filtering performance of the ultrafiltration membrane is greatly reduced. The method for modifying the membrane by dispersing the antibacterial material in the polymer matrix is concerned at present, and not only can adjust the structure and physicochemical properties of the membrane, such as hydrophilicity, porosity, mechanical stability and the like, but also can improve the antibacterial property of the ultrafiltration membrane.
CN105727751A discloses an application of a high-dispersibility hybrid antibacterial agent in modification of an ultrafiltration membrane, wherein silver nanoparticles are anchored on a graphene sheet layer to form a nano hybrid material, the high-dispersibility hybrid antibacterial agent is added into N, N-dimethylacetamide, N-dimethylformamide or dimethyl sulfoxide, uniform dispersion liquid is obtained through ultrasonic treatment, polyvinylidene fluoride or polyether sulfone is added into the dispersion liquid, the mixture is stirred at the temperature of 55-65 ℃ to obtain uniform membrane casting liquid, standing and defoaming are carried out for 6-12 hours, pure water is used as a gel bath, and a modified ultrafiltration membrane is prepared through an immersion precipitation phase inversion method;
CN109589801A discloses an antibacterial film comprising a base film and an antibacterial layer coated on the upper surface of the base film, wherein the antibacterial layer is a nano molybdenum disulfide layer. The preparation method of the antibacterial film comprises the following steps: (1) preparing nano molybdenum disulfide dispersion liquid; (2) and (3) carrying out suction filtration on the surface of the base film on the nano molybdenum disulfide dispersion solution, and drying to obtain the antibacterial film.
However, the existing ultrafiltration membrane still has the technical problems of poor antibacterial property and the like.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides Ce-doped MoS2The honeycomb porous ball is used as an antibacterial agent modified polyethersulfone ultrafiltration membrane.
An antibacterial ultrafiltration membrane is characterized in that Ce-doped MoS is adopted2The ultrafiltration membrane is used as an antibacterial agent to modify the ultrafiltration membrane, wherein the preparation process of the ultrafiltration membrane specifically comprises the following steps:
(1) weighing sodium molybdate, thiourea, cerium nitrate and diethylenetriamine, dissolving in glycerol/deionized water solution, and stirringHomogenizing, transferring the mixture into a polytetrafluoroethylene high-temperature reaction hydrothermal kettle, and carrying out microwave hydrothermal reaction at 180-220 ℃ and 80-90W for 0.5-1 h to prepare Ce-doped MoS2A honeycomb-shaped porous ball;
(2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, coating the mixture on a glass plate by blade coating, taking deionized water as a gel bath, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball.
Preferably, the molar ratio of sodium molybdate to thiourea to cerium nitrate to diethylenetriamine is 1: (1.1-1.5): (0.05-0.08): (0.2-0.4).
Preferably, Ce-doped MoS2The cellular porous ball has a particle size of 20-40 μm.
Preferably, the stirring time in step (1) is 30-60 min.
The technical effects are as follows:
according to the invention, the molybdenum disulfide antibacterial agent is improved from two aspects of structure and material components, and the honeycomb-pore-shaped microsphere antibacterial agent is obtained by combining a microwave hydrothermal process with diethylenetriamine as a structure regulator, so that the antibacterial material can adsorb and filter micro particles or pathogenic aerosol due to high porosity and specific surface area, the antibacterial active sites are effectively promoted, and higher antibacterial performance can be achieved with fewer materials; in addition, the antibacterial activity of the material is surprisingly found to be further improved by doping the material with Ce.
Drawings
FIG. 1 is an SEM image of the antimicrobial agent of the present application.
Detailed Description
Example 1
(1) Weighing 0.5mmol of sodium molybdate, 0.5mmol of thiourea, 0.025mmol of cerium nitrate and 0.1mmol of diethylenetriamine, dissolving the sodium molybdate, the thiourea and the 0.025mmol of cerium nitrate in 80ml of glycerol/deionized water solution with the volume ratio of 3:1, stirring for 40min, transferring the solution into a polytetrafluoroethylene high-temperature reaction hydrothermal kettle, and carrying out microwave hydrothermal reaction at 180 ℃ and 80W for 0.5h to prepare the Ce-doped MoS2A honeycomb-shaped porous ball;
(2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, coating the mixture on a glass plate by blade coating, taking deionized water as a gel bath, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball.
Example 2
(1) Weighing 0.5mmol of sodium molybdate, 0.5mmol of thiourea, 0.03mmol of cerium nitrate and 0.15mmol of diethylenetriamine, dissolving the sodium molybdate, the thiourea and the 0.03mmol of cerium nitrate in 80ml of glycerol/deionized water solution with the volume ratio of 3:1, stirring for 40min, transferring the solution into a polytetrafluoroethylene high-temperature reaction hydrothermal kettle, and carrying out microwave hydrothermal reaction at 200 ℃ and 80W for 0.5h to prepare the Ce-doped MoS2A honeycomb-shaped porous ball;
(2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, coating the mixture on a glass plate by blade coating, taking deionized water as a gel bath, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball.
Example 3
(1) Weighing 0.5mmol of sodium molybdate, 0.5mmol of thiourea, 0.03mmol of cerium nitrate and 0.15mmol of diethylenetriamine, dissolving the sodium molybdate, the thiourea and the 0.03mmol of cerium nitrate in 80ml of glycerol/deionized water solution with the volume ratio of 3:1, stirring for 40min, transferring the solution into a polytetrafluoroethylene high-temperature reaction hydrothermal kettle, and carrying out microwave hydrothermal reaction for 1h at 290 ℃ and 85W to obtain Ce-doped MoS2A honeycomb-shaped porous ball;
(2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, coating the mixture on a glass plate by blade coating, taking deionized water as a gel bath, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball.
Comparative example 1
(1) 0.5mmol of sodium molybdate, 0.5mmol of thiourea and 0.15mmol of diethylenetriamine are weighed out and dissolved in 80ml of glycerol/deionized water in a volume ratio of 3:1, stirred for 40min and transferred to polytetrafluoro-ethyleneIn an ethylene high-temperature reaction hydrothermal kettle, carrying out microwave hydrothermal reaction for 1h at 290 ℃ and 85W to prepare Ce-doped MoS2A honeycomb-shaped porous ball;
(2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, coating the mixture on a glass plate by blade coating, taking deionized water as a gel bath, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball.
And (3) testing antibacterial performance:
the ultrafiltration membranes of examples 1-3 and comparative example 1 were used as antibacterial materials to test their bacteriostatic effects on escherichia coli and staphylococcus aureus.
Example (bacteriostasis rate) | Staphylococcus aureus | Escherichia coli |
Example 1 | 98.2% | 97.0% |
Example 2 | 97.3% | 97.7% |
Example 3 | 96.7% | 98.9% |
Comparative example 1 | 90.3% | 87.7% |
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (4)
1. An antibacterial ultrafiltration membrane is characterized in that Ce-doped MoS is adopted2The polyether sulfone ultrafiltration membrane is used as an antibacterial agent to modify, wherein the preparation process of the ultrafiltration membrane specifically comprises the following steps:
(1) weighing sodium molybdate, thiourea, cerium nitrate and diethylenetriamine, dissolving the sodium molybdate and the thiourea, the cerium nitrate and the diethylenetriamine in a glycerol/deionized water solution, uniformly stirring, transferring the mixture into a polytetrafluoroethylene high-temperature reaction hydrothermal kettle, and carrying out microwave hydrothermal reaction at 180-220 ℃ and 80-90W for 0.5-1 h to prepare the Ce-doped MoS2A honeycomb-shaped porous ball;
(2) doping Ce with MoS2Uniformly mixing the honeycomb porous ball with N, N-dimethylacetamide and polyether sulfone, coating the mixture on a glass plate by blade coating, taking deionized water as a gel bath, and preparing the Ce-doped MoS by adopting an immersion precipitation phase conversion method2A polyether sulfone ultrafiltration membrane modified by a honeycomb porous ball.
2. The antimicrobial ultrafiltration membrane of claim 1, wherein: the molar ratio of sodium molybdate to thiourea to cerium nitrate to diethylenetriamine is 1: (1.1-1.5): (0.05-0.08): (0.2-0.4).
3. The antimicrobial ultrafiltration membrane of claim 1, wherein: ce doped MoS2The cellular porous ball has a particle size of 20-40 μm.
4. The antimicrobial ultrafiltration membrane of claim 1, wherein: the stirring time in the step (1) is 30-60 min.
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CN202110636187.4A CN113181771A (en) | 2021-06-08 | 2021-06-08 | Antibacterial ultrafiltration membrane |
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CN202110636187.4A CN113181771A (en) | 2021-06-08 | 2021-06-08 | Antibacterial ultrafiltration membrane |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115413673A (en) * | 2022-09-30 | 2022-12-02 | 安徽江淮汽车集团股份有限公司 | Antibacterial agent suitable for thermoplastic plastics and preparation method thereof |
CN115722234A (en) * | 2022-11-15 | 2023-03-03 | 陕西科技大学 | Ce-MoS with photodynamic-enzyme activity 2 /WO 3 Preparation method and application of nano composite antibacterial material |
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2021
- 2021-06-08 CN CN202110636187.4A patent/CN113181771A/en not_active Withdrawn
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115413673A (en) * | 2022-09-30 | 2022-12-02 | 安徽江淮汽车集团股份有限公司 | Antibacterial agent suitable for thermoplastic plastics and preparation method thereof |
CN115722234A (en) * | 2022-11-15 | 2023-03-03 | 陕西科技大学 | Ce-MoS with photodynamic-enzyme activity 2 /WO 3 Preparation method and application of nano composite antibacterial material |
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