CN112370974A - Preparation method of super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion - Google Patents
Preparation method of super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion Download PDFInfo
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion. Dopamine and tobramycin are reacted on the surface of the polyvinylidene fluoride base membrane and a very thin composite hydrophilic layer is deposited, so that the infiltration characteristic of the membrane is changed essentially, and the super-hydrophilic/underwater super-oleophobic wetting characteristic is presented, so that the anti-fouling performance of the membrane is greatly improved; meanwhile, due to the introduction of tobramycin, the super-hydrophilic separation membrane has excellent antibacterial performance.
Description
Technical Field
The invention belongs to the technical field of environment-friendly materials, and particularly relates to a preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion.
Background
Water resources in the 21 st century are becoming a precious scarce resource, and with the increasing shortage of fresh water resources, nearly 30 billion people around the world face the shortage of fresh water, so that the recycling of water resources becomes an urgent problem. A large amount of oily wastewater is generated in industries such as petrochemical industry, metallurgy, food processing, medicine manufacturing and the like every year, and the resource utilization of the water also becomes a great challenge to human beings.
With the rapid development of membrane separation technology, its application has been spread in various fields such as industry, medical treatment, environment, etc. In the field of oily wastewater treatment, the method not only overcomes the defects of high consumption, easy generation of secondary pollution, large occupied area and the like of the traditional methods such as an adsorption method, a gravity method, a biological method, a flotation method and the like, but also embodies unique high-efficiency separation characteristics on the separation of oil-water mixed liquor. Therefore, membrane separation technology is considered to be one of the most promising technologies for treating oil-containing wastewater.
Membrane fouling is a major problem that prevents the widespread use of membrane technology, and is one of the most challenging of the current separation technologies. In recent years, scientists are inspired by the super-hydrophobic phenomenon of the lotus leaf surface, and materials with special wettability gradually appear in various fields and applications. Although the film with the super-hydrophobic characteristic is a film material capable of efficiently separating oily wastewater, the film can also have the phenomenon of film blockage in application, so that the super-hydrophilic/underwater super-hydrophobic oil type anti-fouling material is produced, and the super-hydrophilic/underwater super-hydrophobic oil type anti-fouling material can prevent oil stains from being attached to the surfaces of film pores by forming a very thin water layer on the surface of the film, so that the service life of the film is greatly prolonged, and the maintenance time is greatly prolonged.
Dopamine is a catechol substance rich in hydrophilic groups, is commonly used for material surface modification, can greatly improve the hydrophilicity of the material surface, and can greatly improve the anti-fouling and antibacterial properties of the material by combining the dopamine with tobramycin antibiotics with antibacterial properties. The invention is based on a dopamine-tobramycin system, simultaneously introduces a strong oxidizing trigger to shorten the reaction time of the dopamine-tobramycin system and the strong oxidizing trigger, combines the strong oxidizing trigger with a membrane separation technology, and can prepare the super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion in a short time.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-efficiency anti-fouling antibacterial separation membrane for treating oily wastewater, which utilizes dopamine and tobramycin to react on the surface of a polyvinylidene fluoride (PVDF) membrane and deposit a very thin composite hydrophilic layer to cause the infiltration characteristic of the membrane to change essentially and present the ultra-hydrophilic/underwater ultra-oleophobic wetting characteristic, thereby greatly improving the anti-fouling performance of the membrane. The separation membrane has excellent oil-water separation efficiency and anti-fouling and antibacterial properties. The preparation method is simple, short in time consumption and capable of realizing large-scale production.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion comprises the following steps:
1) adding tobramycin and a trigger into a dissolved Tris-HCl buffer solution, shaking and oscillating uniformly, adding dopamine hydrochloride, and performing ultrasonic dissolution completely to obtain a mixed solution a;
2) placing the PVDF porous base membrane in a mould, slowly pouring the mixed solution a into the mould, fixing the mould in a constant-temperature oscillation box for reaction, taking out the PVDF porous base membrane after the PVDF porous base membrane and the mixed solution a are fully reacted, and washing the PVDF porous base membrane for a plurality of times by deionized water until the residual solution on the membrane is washed, thus obtaining the efficient anti-fouling antibacterial separation membrane for treating the oily wastewater.
Preferably, the trigger in the step 1) is persulfate and CuSO4/H2O2The persulfate is ammonium persulfate, and the periodate is sodium periodate. The trigger accelerates the self-polymerization process of dopamine to enable the tobramycin and the dopamine to generate codeposition reaction, so that a super-hydrophilic interface is constructed.
Preferably, the concentration of dopamine hydrochloride in the mixed solution a in the step 1) is 1.1 × 10-2mol/L, the concentration of tobramycin is 1.1X 10-2~4.4×10-2mol/L, concentration of trigger is 5.8X 10-3~2.8×10-2 mol/L。
Preferably, the Tris-HCl solution of step 1) has a pH of 8.5.
Preferably, the reaction temperature in the step 2) is within the range of 20-30 ℃.
Preferably, the reaction time in the step 2) is 0.25-1 h.
The invention has the beneficial effects that: based on a dopamine-tobramycin system, the invention also introduces a trigger to shorten the reaction time, so that the dopamine and the tobramycin quickly undergo Michael addition and Schiff base codeposition reaction in a short time, and the super-hydrophilic anti-fouling antibacterial separation membrane suitable for efficiently separating oil-water emulsion can be prepared. The introduction of the dopamine-tobramycin system can not only greatly improve the hydrophilicity of the surface of the membrane, but also greatly improve the anti-fouling and antibacterial properties of the membrane.
Drawings
FIG. 1 is an electron photograph of the PVDF-based membrane and the resulting superhydrophilic antifouling antibacterial separation membrane of example 1;
FIG. 2 is a Fourier infrared spectrum of the PVDF-based membrane and the superhydrophilic anti-fouling antibacterial separation membrane in example 1;
FIG. 3 is a schematic diagram of the reaction of tobramycin with dopamine codeposition;
FIG. 4 is a scanning electron microscope image of the surfaces of the PVDF-based membrane and the superhydrophilic anti-fouling antibacterial separation membrane in example 1;
FIG. 5 is a result of a water contact angle test of the superhydrophilic antifouling antibacterial separation membrane of example 1;
FIG. 6 shows the results of the underwater oil contact angle test of the superhydrophilic antifouling antibacterial separation membrane of example 1;
FIG. 7 is the result of the performance test of the super-hydrophilic anti-fouling antibacterial separation membrane in the oil-water separation in example 1;
FIG. 8 shows the results of 50 cycle performance tests of the superhydrophilic antifouling antibacterial separation membrane in example 1 during oil-water separation;
FIG. 9 shows the antibacterial effect of the superhydrophilic antifouling antibacterial separation membrane of example 1 after soaking in water for 8 days.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion comprises the following steps:
1) adding tobramycin and ammonium persulfate into a dissolved Tris-HCl buffer solution (pH = 8.5), shaking and oscillating uniformly, adding dopamine hydrochloride, and performing ultrasonic dissolution completely to obtain a mixed solution a; the concentration of tobramycin in the mixed solution a is 2.2 multiplied by 10-2mol/L, the concentration of ammonium persulfate is 2.8 multiplied by 10-2mol/L, concentration of dopamine hydrochloride is 1.1 × 10-2 mol/L。
2) And (2) placing the PVDF porous base membrane into a mould, slowly pouring the mixed solution a into the mould, fixing the mould in a constant-temperature oscillation box at 25 ℃ for reaction, taking out after 0.25 h of reaction, washing with deionized water for a plurality of times until residual liquid on the membrane is washed, and thus obtaining the super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion.
As can be seen from FIG. 1, the surface of the modified PVDF film appears as a dark brown coating; from the Fourier infrared spectrum of FIG. 2, it can be clearly seen that the modified PVDF film is 1554 cm-1、1614 cm-1And 3342 cm-1The equal wavenumber has strong vibration peaks, and the corresponding groups are respectively N-H, C = N and O-H, which shows that dopamine and tobramycin are co-deposited on the surface of the PVDF basement membrane through Michael addition and Schiff base reaction, and the reaction schematic diagram is shown in FIG. 3; as can be seen from FIG. 4, after the dopamine and the tobramycin are co-deposited on the surface of the PVDF basement membrane, the pore diameter of the membrane is effectively reduced, and is reduced from 500 nm to 150 nm, so that the oil-water separation efficiency can be effectively improved; as can be seen from FIG. 5, the initial water contact angle of the anti-fouling and antibacterial separation membrane prepared by the method is 22.5 +/-2.1 degrees, and the complete wetting only needs 2.6 seconds; meanwhile, as can be seen from fig. 6: the underwater oil contact angle is 171.3 +/-0.6 degrees. Therefore, the co-deposition of dopamine and tobramycin endows the membrane surface with excellent hydrophilic anti-fouling performance; as can be seen from FIGS. 7 and 8, the flux for separating oil and water under gravity can reach 317.1 + -15.7L·m-2·h-1The separation efficiency of oil/water emulsions such as n-hexane, petroleum ether, dichloromethane and the like is more than 99.92 percent, and the flux and the rejection rate of the membrane are kept stable through 50 times of oil-water circulation separation tests, so that excellent anti-fouling performance is shown; as can be seen from FIG. 9, the super-hydrophilic anti-fouling antibacterial separation membrane prepared by the invention is placed in an Escherichia coli solution for 4 hours, and the antibacterial rate can reach more than 99.9% by using a plate calculation method; in addition, after the super-hydrophilic anti-fouling antibacterial separation membrane is soaked for 8 days, the antibacterial rate still reaches over 99.8 percent, and extremely stable antibacterial performance is shown.
Example 2
A preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion comprises the following steps:
1) adding tobramycin and CuSO to a dissolved Tris-HCl buffer (pH = 8.5)4/H2O2Shaking and oscillating uniformly, adding dopamine hydrochloride, and obtaining a mixed solution a after ultrasonic dissolution is completed; the concentration of tobramycin in the mixed solution a is 1.1 multiplied by 10-2 mol/L，CuSO4/H2O2Has a concentration of 1.1X 10-2mol/L, concentration of dopamine hydrochloride is 1.1 × 10-2 mol/L。
2) Placing the PVDF porous base membrane into a mould, slowly pouring the mixed solution a into the mould, fixing the mould in a constant-temperature oscillation box at 20 ℃ for reaction, taking out after 0.5 h of reaction, washing the membrane for a plurality of times by deionized water until the residual solution on the membrane is washed, and obtaining the super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion.
After the PVDF base film is modified, the initial water contact angle of the anti-fouling and antibacterial separation film prepared by the invention is 23.2 +/-2.6 degrees, and the complete wetting only needs 2.8 seconds; the underwater oil contact angle is 170.9 +/-0.7 degrees. Therefore, the co-deposition of dopamine and tobramycin endows the membrane surface with excellent hydrophilic anti-fouling performance; the flux of oil-water separation under the gravity condition can reach 305.8 +/-14.1 L.m-2·h-1The separation efficiency of the oil/water emulsion such as n-hexane, petroleum ether, dichloromethane and the like is more than 99.94 percent; in addition, the invention preparesThe super-hydrophilic anti-fouling antibacterial separation membrane has excellent antibacterial performance in an antibacterial test, and the antibacterial rate is over 99.9%.
Example 3
A preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion comprises the following steps:
1) adding tobramycin and sodium periodate into a dissolved Tris-HCl buffer solution (pH = 8.5), shaking and oscillating uniformly, adding dopamine hydrochloride, and performing ultrasonic dissolution completely to obtain a mixed solution a; the concentration of tobramycin in the mixed solution a is 4.4 multiplied by 10-2mol/L, the concentration of sodium periodate is 5.8 multiplied by 10-3mol/L, concentration of dopamine hydrochloride is 1.1 × 10-2 mol/L。
2) Placing the PVDF porous base membrane into a mould, slowly pouring the mixed solution a into the mould, fixing the mould in a constant-temperature oscillation box at 25 ℃ for reaction, taking out after 1 h of reaction, washing the membrane for a plurality of times by deionized water until the residual solution on the membrane is washed, and obtaining the super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating the oil-water emulsion.
After the PVDF base film is modified, the initial water contact angle of the anti-fouling and antibacterial separation film prepared by the invention is 23.7 +/-1.9 degrees, and the complete wetting only needs 2.4 seconds; the underwater oil contact angle is 170.4 +/-1.0 degrees. Therefore, the co-deposition of dopamine and tobramycin endows the membrane surface with excellent hydrophilic anti-fouling performance; the flux of oil-water separation under the gravity condition can reach 303.9 +/-14.7 L.m-2·h-1The separation efficiency of the oil/water emulsion such as n-hexane, petroleum ether, dichloromethane and the like is more than 99.95 percent; in addition, the super-hydrophilic anti-fouling antibacterial separation membrane prepared by the invention shows excellent antibacterial performance in an antibacterial test, and the antibacterial rate is up to more than 99.9%.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.
Claims (8)
1. A preparation method of a super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion is characterized by comprising the following steps: the method comprises the following steps:
1) adding tobramycin and a trigger into a dissolved Tris-HCl buffer solution, shaking and oscillating uniformly, adding dopamine hydrochloride, and performing ultrasonic dissolution completely to obtain a mixed solution a;
2) placing a polyvinylidene fluoride porous base membrane in a mould, slowly pouring a mixed solution a into the mould, fixing the mould in a constant-temperature oscillation box for reaction, taking out the polyvinylidene fluoride porous base membrane after the polyvinylidene fluoride porous base membrane is fully reacted with the mixed solution a, washing the membrane for a plurality of times by deionized water until residual liquid on the membrane is washed, and obtaining the super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion.
2. The method of claim 1, wherein: the trigger in the step 1) is persulfate and CuSO4/H2O2And periodate.
3. The method of claim 2, wherein: the persulfate is ammonium persulfate; the periodate is sodium periodate.
4. The method of claim 1, wherein: in the mixed solution a, the concentration of tobramycin is 1.1X 10-2~4.4×10-2mol/L, concentration of trigger is 5.8X 10-3~2.8×10-2mol/L, concentration of dopamine hydrochloride is 1.1 × 10-2 mol/L。
5. The method of claim 1, wherein: the pH value of the Tris-HCl buffer solution in the step 1) is 8.5.
6. The method of claim 1, wherein: the reaction temperature of the constant-temperature oscillation box in the step 2) is 20-30 ℃.
7. The method of claim 1, wherein: the reaction time in the step 2) is 0.25-1 h.
8. A super-hydrophilic anti-fouling antibacterial separation membrane for efficiently separating oil-water emulsion prepared by the preparation method according to any one of claims 1 to 7.
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Application publication date: 20210219 |