CN113509851B - Polyether sulfone ultrafiltration membrane with pure natural green tea extract tea polyphenol as additive and preparation method thereof - Google Patents
Polyether sulfone ultrafiltration membrane with pure natural green tea extract tea polyphenol as additive and preparation method thereof Download PDFInfo
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- CN113509851B CN113509851B CN202110373479.3A CN202110373479A CN113509851B CN 113509851 B CN113509851 B CN 113509851B CN 202110373479 A CN202110373479 A CN 202110373479A CN 113509851 B CN113509851 B CN 113509851B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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Abstract
The invention discloses a polyether sulfone ultrafiltration membrane taking pure natural green tea extract tea polyphenol as an additive and a preparation method thereof, wherein the preparation method comprises the following steps: drying polyether sulfone and polyvinylpyrrolidone, dissolving in N, N-dimethylacetamide, adding tea polyphenol, and uniformly dispersing in an ultrasonic dispersion instrument to prepare a casting solution a; and stirring the prepared membrane casting solution a at normal temperature in air to enable tea polyphenol to fully self-polymerize, standing for defoaming, pouring the membrane casting solution for membrane scraping, standing in air, then placing into a deionized water coagulation bath for membrane forming, and soaking with deionized water to obtain the tea polyphenol modified polyether sulfone ultrafiltration membrane. The invention adopts a phase inversion method to prepare the membrane, uses static pressure difference as a driving force, and uses a pore size sieving theory as a filtering mechanism, so that pollutants in water are intercepted by a tea polyphenol-polyethersulfone ultrafiltration membrane, thereby achieving the purpose of primary water purification; the hydrophilicity of the polyether sulfone is increased, the permeation flux of the membrane is increased, and the retention rate is improved.
Description
Technical Field
The invention relates to the technical field of ultrafiltration membrane preparation, in particular to a polyether sulfone ultrafiltration membrane taking pure natural green tea extract tea polyphenol as an additive and a preparation method thereof.
Background
The ultrafiltration membrane is a pressure-driven membrane with static pressure difference as driving force, the ultrafiltration technology has a wider interception interval (500-. Ultrafiltration techniques are widely used, such as: wastewater treatment, reverse osmosis pretreatment, separation application in food, dairy products, paper making, textile, chemical and biochemical industries, and the like. Currently, the materials widely used as the film matrix include polyamides, polyolefins, polyaryl ethers, polyaryl heterocycles and other organic polymer materials, and the polyether sulfone is a thermoplastic polymer material with excellent comprehensive performance and has excellent heat resistance, mechanical properties, insulating properties and the like.
However, as the common material of the ultrafiltration membrane, the polyethersulfone has low permeation flux, poor interception effect and poor anti-pollution capability in the application process due to the weak hydrophilicity. The hydrophilic modification of the membrane is beneficial to the permeation of water molecules, and a hydration layer can be formed to enhance the anti-fouling performance of the membrane. Therefore, the improvement of the hydrophilic capability of the polyethersulfone membrane is an important mode for improving the flux and the anti-pollution capability of the membrane.
Disclosure of Invention
The invention aims to improve the hydrophilic capacity of a polyether sulfone membrane, and provides a polyether sulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as an additive and a preparation method thereof.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a polyether sulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as an additive takes N, N-dimethylacetamide as a solvent, and comprises the following components in percentage by mass: 16-20% of polyether sulfone, 1-3% of polyvinylpyrrolidone and 0.08-0.32% of tea polyphenol.
Furthermore, in the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as the additive, the mass concentration of the polyethersulfone is 18%.
Furthermore, in the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as an additive, the mass concentration of the polyvinylpyrrolidone is 2%.
Furthermore, in the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as the additive, the mass concentration of the tea polyphenol is 0.1-0.3%.
Further, in the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as the additive, the preparation method comprises the following steps:
(1) drying polyether sulfone and polyvinylpyrrolidone at the temperature of 100-120 ℃ for 10-14 hours, dissolving the polyether sulfone and polyvinylpyrrolidone in N, N-dimethylacetamide at normal temperature, and magnetically stirring to uniformly dissolve the polyether sulfone and polyvinylpyrrolidone;
(2) adding tea polyphenol, carrying out ultrasonic dispersion for 25-35 minutes, stirring for 10-14 hours in air, and defoaming for 2-3 hours to obtain a casting solution a;
(3) pouring the casting solution a onto a glass plate, scraping the film at room temperature, standing in the air for 25-35 seconds, slowly immersing the glass plate coated with the casting solution a into deionized water at room temperature for gel curing to form a film, immersing for 2-4 days, and replacing the deionized water every 11.5-12.5 hours to obtain a PES film;
(4) and (3) carefully taking out the obtained PES membrane, and then hanging and airing the PES membrane in a dustless room-temperature environment to obtain the tea polyphenol-polyethersulfone ultrafiltration membrane.
Furthermore, in the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as the additive, the density of the polyethersulfone in the step (1) is 1.2-1.3g/cm 3.
Furthermore, in the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as an additive, the molecular weight of polyvinylpyrrolidone in the step (1) is 58000.
Further, the polyethersulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as the additive is dried for 12 hours at 110 ℃ by the polyethersulfone and polyvinylpyrrolidone in the step (1).
Further, in the polyether sulfone ultrafiltration membrane using the pure natural green tea extract tea polyphenol as the additive, a proper amount of tea polyphenol is added in the step (2) for ultrasonic dispersion for 30min, air stirring is carried out for 12h, and defoaming is carried out for 2-3 h.
Further, in the polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as an additive, the membrane casting solution a in the step (3) is poured on a glass plate, the membrane is scraped at room temperature, the glass plate coated with the membrane casting solution a is slowly immersed in deionized water at room temperature for 30 seconds to be subjected to gel curing to form a membrane, the membrane is immersed for 3 days, and the deionized water is replaced every 12 hours.
The invention has the beneficial effects that:
the invention adopts a phase inversion method to prepare the membrane, has simple preparation, takes tea polyphenol and polyvinylpyrrolidone as additives, takes polyether sulfone as membrane matrix, takes static pressure difference as driving force, and takes a pore size sieving theory as a filtering mechanism, so that pollutants in water are intercepted by a tea polyphenol-polyether sulfone ultrafiltration membrane, thereby achieving the purpose of primary water purification. The ultrafiltration membrane prepared by the invention realizes the increase of the hydrophilicity of the polyethersulfone by adding the tea polyphenol, increases the permeation flux of the membrane and improves the retention rate.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
FIG. 1 is an electron micrograph of a cross section of a film of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) 18g of polyethersulfone and 2g of polyvinylpyrrolidone, which were dried at 110 ℃ for 12 hours, were dissolved in N, N-dimethylacetamide at room temperature, and the mixture was magnetically stirred.
(2) And adding 0.1g of tea polyphenol into the system, performing ultrasonic dispersion for 30min, stirring for 12h in air to uniformly dissolve the tea polyphenol, and defoaming for 3h to obtain the polyether sulfone casting solution.
(3) Pouring the casting solution on a glass plate, coating the clean glass plate with a glass rod in a room temperature environment with certain relative humidity, standing in the air for 30 seconds, slowly immersing the glass plate of the polyether sulfone casting solution in deionized water at room temperature for gel curing to form a film, immersing for 3 days, and replacing the deionized water every 12 hours to obtain the polyether sulfone film.
(4) And (3) carefully taking out the obtained PES membrane, and then hanging and airing the PES membrane in a dustless room-temperature environment to obtain the tea polyphenol-polyethersulfone ultrafiltration membrane.
Polyether sulfone produced in this exampleThe pure water flux of the ultrafiltration membrane is 213L/m 2 H, (transmembrane pressure 0.1MPa, 28 ℃), Bovine Serum Albumin (BSA) retention of 97.5%.
Membrane retention Performance test
Pure water flux and retention flux, retention rate test:
pure water flux and bovine serum albumin retention rate are tested by using a flux tester, and in the test process, the effective area of the tea polyphenol-polyether sulfone membrane is 0.00077m 2 The testing pressure is 0.1MPa, the testing temperature is room temperature, and the pure water flux of the filtering membrane is tested to be 1h after the pure water is pre-pressed for 30 min. The pure water flux and the retained flux of the filtration membrane were calculated according to the formula J ═ V/At, where J represents the pure water flux (retained flux) (L/m) 2 H), where t is the permeation time, A is the effective membrane area, and V is the permeate volume.
Dissolving 1g of bovine serum albumin in 1L of deionized water, preparing 1g/L of bovine serum albumin solution, collecting protein penetrating fluid according to the method, testing the absorbance of the penetrating fluid at 280nm by using ultraviolet, and calculating the retention rate of the tea polyphenol-polyether sulfone ultrafiltration membrane according to a tested protein standard curve. Calculating according to the formula: r (%) (1-C1/C2) × 100%, C1 is permeate concentration, C2 is feed concentration. The results of the pure water flux and protein rejection tests are shown in the following table:
| pure water flux (L/square meter h) | Protein rejection (%) | |
| Example 1 | 213 | 97.5％ |
Example 2
(1) 18g of polyethersulfone and 2g of polyvinylpyrrolidone, which were dried at 110 ℃ for 12 hours, were dissolved in N, N-dimethylacetamide at room temperature, and the mixture was magnetically stirred.
(2) And then 0.2g of tea polyphenol is added into the system, ultrasonic dispersion is carried out for 30min, air stirring is carried out for 12h, the solution is uniformly dissolved, and deaeration is carried out for 3h, thus obtaining the polyether sulfone casting solution.
(3) Pouring the casting solution on a glass plate, coating the clean glass plate with a glass rod in a room temperature environment with certain relative humidity, standing in the air for 30 seconds, slowly immersing the glass plate of the polyether sulfone casting solution in deionized water at room temperature for gel curing to form a film, immersing for 3 days, and replacing the deionized water every 12 hours to obtain the polyether sulfone film.
(4) And (3) carefully taking out the obtained PES membrane, and then hanging and airing the PES membrane in a dustless room-temperature environment to obtain the tea polyphenol-polyethersulfone ultrafiltration membrane.
The pure water flux of the polyether sulfone ultrafiltration membrane prepared in the example is 279.22L/m 2 H, (transmembrane pressure 0.1MPa, 28S ℃), Bovine Serum Albumin (BSA) retention of 99.7%.
Membrane retention Performance test
Pure water flux and retention flux, retention rate test:
pure water flux and protein retention rate are tested by using a flux tester, and in the testing process, the effective area of the tea polyphenol-polyether sulfone membrane is 0.00077m 2 The testing pressure is 0.1MPa, the testing temperature is room temperature, and the pure water flux of the filtering membrane is tested to be 1h after the pure water is pre-pressed for 30 min. The pure water flux and the retained flux of the filtration membrane were calculated according to the formula J ═ V/At, where J represents the pure water flux (retained flux) (L/m) 2 H), where t is the permeation time, A is the effective membrane area, and V is the permeate volume.
Dissolving 1g of bovine serum albumin in 1L of deionized water, preparing 1g/L of bovine serum albumin solution, collecting protein penetrating fluid according to the method, testing the absorbance of the penetrating fluid at 280nm by using ultraviolet, and calculating the retention rate of the tea polyphenol-polyether sulfone ultrafiltration membrane according to a tested protein standard curve. Calculating according to the formula: r (%) (1-C1/C2) × 100%, C1 is permeate concentration, C2 is feed concentration. The results of the pure water flux and protein rejection tests are shown in the following table:
| pure water flux (L/square meter h) | Protein rejection (%) | |
| Example 2 | 279.22 | 99.7％ |
Comparative example 1 pure water flux experiment of polyethersulfone base membrane modified without tea polyphenol
(1) 18g of polyether sulfone and 2g of polyvinylpyrrolidone which are dried at 110 ℃ for 12 hours are dissolved in N, N-dimethylacetamide at normal temperature, and the mixture is magnetically stirred to be uniformly dissolved.
(2) And defoaming for 3h to obtain the polyether sulfone casting solution.
(3) Pouring the casting solution on a glass plate, coating the clean glass plate with a glass rod in a room temperature environment with certain relative humidity, standing in the air for 30 seconds, slowly immersing the glass plate of the polyether sulfone casting solution in deionized water at room temperature for gel curing to form a film, immersing for 3 days, and replacing the deionized water every 12 hours to obtain the polyether sulfone film.
(4) And (3) carefully taking out the obtained polyethersulfone membrane, and then hanging and airing the polyethersulfone membrane in a dust-free room temperature environment to obtain the tea polyphenol-polyethersulfone ultrafiltration membrane.
The polyethersulfone ultrafiltration membrane prepared in the example is pureThe water flux is 124.67L/m 2 H, (transmembrane pressure 0.1MPa, 28S ℃), Bovine Serum Albumin (BSA) retention of 95%.
Membrane retention Performance test
Pure water flux and retention flux, retention rate test:
and (3) carrying out pure water flux and protein rejection test by using an experimental flux tester, wherein in the test process, the effective area of the polyether sulfone membrane is 0.00077 square meters, the test pressure is 0.1MPa, the test temperature is room temperature, and the pure water flux of the filter membrane is tested for 1h after pure water is prepressed for 30 min. The pure water flux and the retained flux of the filtration membrane were calculated according to the formula J ═ V/At, where J represents the pure water flux (retained flux) (L/m) 2 H), where t is the permeation time, A is the effective membrane area, and V is the permeate volume.
Dissolving 1g of bovine serum albumin in 1L of deionized water, preparing 1g/L of bovine serum albumin solution, collecting protein penetrating fluid according to the method, testing the absorbance of the penetrating fluid at 280nm by using ultraviolet, and calculating the rejection rate of the polyether sulfone ultrafiltration membrane through a tested protein standard curve. Calculating according to the formula: r (%) (1-C1/C2) × 100%, C1 is permeate concentration, C2 is feed concentration. The results of the pure water flux and protein retention tests are given in the following table:
| pure water flux (L/square meter h) | Protein rejection (%) | |
| Comparative example 1 | 124.67 | 95％ |
And (4) conclusion: compared with a comparative experiment, the pure water flux of the tea polyphenol-polyethersulfone ultrafiltration membrane modified by tea polyphenol is improved by about 2 times, and the retention rate is increased.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. A polyether sulfone ultrafiltration membrane taking pure natural green tea extract tea polyphenol as an additive is characterized by taking N, N-dimethylacetamide as a solvent and comprising the following components in percentage by mass: 16-20% of polyether sulfone, 1-3% of polyvinylpyrrolidone and 0.08-0.32% of tea polyphenol;
the preparation method comprises the following steps:
(1) drying polyether sulfone and polyvinylpyrrolidone at the temperature of 100-120 ℃ for 10-14 hours, dissolving the polyether sulfone and polyvinylpyrrolidone in N, N-dimethylacetamide at normal temperature, and magnetically stirring to uniformly dissolve the polyether sulfone and polyvinylpyrrolidone;
(2) adding tea polyphenol, carrying out ultrasonic dispersion for 25-35 minutes, stirring for 10-14 hours in air, and defoaming for 2-3 hours to obtain a casting solution a;
(3) pouring the casting solution a onto a glass plate, scraping the film at room temperature, standing in the air for 25-35 seconds, slowly immersing the glass plate coated with the casting solution a into deionized water at room temperature for gel curing to form a film, immersing for 2-4 days, and replacing the deionized water every 11.5-12.5 hours to obtain a PES film;
(4) and (3) carefully taking out the obtained PES membrane, and then hanging and airing the PES membrane in a dustless room-temperature environment to obtain the tea polyphenol-polyethersulfone ultrafiltration membrane.
2. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: the mass concentration of the polyether sulfone is 18%.
3. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: the mass concentration of the polyvinylpyrrolidone is 2%.
4. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: the mass concentration of the tea polyphenol is 0.1-0.3%.
5. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: in the step (1), the density of the polyether sulfone is 1.2-1.3g/cm 3.
6. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: the molecular weight of polyvinylpyrrolidone in step (1) is 58000.
7. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: in the step (1), the polyether sulfone and the polyvinylpyrrolidone are dried for 12 hours at 110 ℃.
8. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: adding a proper amount of tea polyphenol into the mixture obtained in the step (2), performing ultrasonic dispersion for 30min, stirring for 12h in air, and defoaming for 2-3 h.
9. The polyethersulfone ultrafiltration membrane using pure natural green tea extract tea polyphenol as additive according to claim 1, characterized in that: and (3) pouring the casting solution a onto a glass plate, scraping the film at room temperature, standing in the air for 30 seconds, slowly immersing the glass plate coated with the casting solution a into deionized water at room temperature for gel curing to form a film, immersing for 3 days, and replacing the deionized water every 12 hours.
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