CN111437737B - Hydrophilic self-cleaning oil-water separation membrane and preparation method thereof - Google Patents

Hydrophilic self-cleaning oil-water separation membrane and preparation method thereof Download PDF

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CN111437737B
CN111437737B CN202010279291.8A CN202010279291A CN111437737B CN 111437737 B CN111437737 B CN 111437737B CN 202010279291 A CN202010279291 A CN 202010279291A CN 111437737 B CN111437737 B CN 111437737B
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membrane
dopamine
graphene oxide
water separation
quantum dot
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CN111437737A (en
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范加谊
刘贝贝
刘宇欣
赵学志
石进
徐积斌
张春芳
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Jiangnan University
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Jiangnan University
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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
    • 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
    • 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
    • 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
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/34—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling by radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/36—Hydrophilic membranes

Abstract

The invention relates to a hydrophilic self-cleaning oil-water separation membrane and a preparation method thereof, belonging to the technical field of membrane separation. The base membrane of the hydrophilic self-cleaning oil-water separation membrane is a polyolefin porous membrane, and graphene oxide quantum dots are deposited on the surface of the base membrane under the assistance of dopamine and are subjected to condensation reaction with the dopamine to form a graphene oxide quantum dot hydrophilic modification layer. Under the irradiation of visible light, the graphene oxide quantum dots can degrade organic pollutants attached to the surface of the film and efficiently kill bacteria, so that the film has excellent self-cleaning antifouling performance; the membrane is suitable for the rapid separation of various oil-water layered mixtures and oil-in-water emulsions with stable surface activity, and has good pollution resistance and circulation stability.

Description

Hydrophilic self-cleaning oil-water separation membrane and preparation method thereof
Technical Field
The invention relates to a hydrophilic self-cleaning oil-water separation membrane and a preparation method thereof, belonging to the technical field of membrane separation.
Background
The increasing of industrial oily sewage and the frequent occurrence of oil leakage accidents at sea pose great threats to the environment and the health of human beings. How to effectively treat oily sewage, in particular to emulsified oily sewage in complex environment, has become a problem of world attention. The membrane separation technology is a novel high-efficiency separation technology, has the advantages of no phase change and side reaction in the process, no secondary pollution, high separation efficiency, mild operation conditions, low energy consumption and the like, and is widely applied to the fields of seawater desalination, chemical industry, printing and dyeing, environmental protection, food, biochemistry and the like. The use of membrane separation techniques to achieve oil-water separation is considered to be one of the most effective separation means, particularly for emulsified oil-water systems. However, the traditional membrane separation material is very easy to suffer from serious membrane surface pollution in the oil-water separation process, so that the separation flux and the oil-water separation efficiency are reduced sharply, and the development and the application of the membrane separation technology in the field of oil-water separation are severely restricted. Therefore, the development of a novel separation membrane material is a key point for realizing efficient, rapid and stable separation of oil and water, and the pollution problem of the separation membrane material is solved.
The membrane pollution can be effectively solved by carrying out surface modification on the membrane material. Common membrane surface modification methods include adsorption, chemical grafting, coating, surface irradiation, plasma modification, and the like. Graphene is a two-dimensional carbon material with the thickness of only a single atomic layer, has the characteristics of excellent conductivity, mechanical strength, ductility and the like, and shows good application prospects in the fields of fuel cells, supercapacitors, biomedicine, molecular separation and the like. As one member of graphene family, graphene oxide quantum dots not only maintain the original excellent characteristics of graphene materials, but also exhibit some new characteristics due to quantum confinement effect and boundary effect, thereby attracting the wide attention of scientists in various fields. The graphene oxide quantum dots are small in size, contain a large number of hydrophilic groups such as hydroxyl groups, carboxyl groups and the like at the edges, have good hydrophilicity and biocompatibility, and are ideal membrane surface hydrophilic modification materials.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a hydrophilic self-cleaning oil-water separation membrane and a preparation method thereof.
According to the technical scheme, the base membrane is a polyolefin porous membrane, and graphene oxide quantum dots are deposited on the surface of the base membrane under the assistance of dopamine and react to form a graphene oxide quantum dot hydrophilic modification layer; under illumination, the graphene oxide quantum dots can degrade organic pollutants attached to the surface of the membrane and efficiently kill bacteria, so that the membrane has excellent self-cleaning antifouling performance; the membrane is suitable for the rapid separation of various oil-water layered mixtures and oil-in-water emulsions with stable surface activity, and has good pollution resistance and circulation stability.
Further, the base membrane is one of a polyolefin microfiltration membrane or an ultrafiltration membrane, and is made of one of polyethylene, polypropylene, polyvinyl chloride, polyvinylidene fluoride or polyacrylonitrile.
Further, the graphene oxide quantum dots are prepared by pyrolyzing citric acid, namely pyrolyzing citric acid at 200 ℃ for 15min, dialyzing and freeze-drying to obtain the graphene oxide quantum dots with a zero-dimensional nano flake structure, a large amount of carboxyl groups on the surface and a particle size of 1-10 nm.
A preparation method of a hydrophilic self-cleaning oil-water separation membrane comprises the following steps:
(1) modification of dopamine: soaking the polyolefin base membrane in 1-3 g/L, pH value 8.5 dopamine solution for 15-25 min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain a dopamine modified porous base membrane;
(2) quantum dot deposition: immersing the dopamine modified base film prepared in the step (1) into a graphene oxide quantum dot aqueous suspension with the mass concentration of 0.01-2% for 10-30 min, and depositing a graphene oxide quantum dot layer on the surface of the base film by means of dopamine to prepare a quantum dot deposition film;
(3) in-situ crosslinking: and (3) immersing the quantum dot deposition film prepared in the step (2) into a morpholine ethanesulfonic acid MES buffer solution containing 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride EDC and N-hydroxysuccinimide NHS, wherein the pH value is 4-6.5, and after an activation reaction is carried out for 1-10 h at room temperature, the hydrophilic self-cleaning oil-water separation film is prepared.
Further, in the mixed solution in the step (3), the total concentration of EDC and NHS is 0.01-0.1 mol/L, and the molar ratio of EDC to NHS is 1-3: 1.
According to the hydrophilic self-cleaning oil-water separation membrane and the preparation method thereof, on one hand, graphene oxide quantum dots are small in size, the edges of the graphene oxide quantum dots contain a large number of hydrophilic groups such as hydroxyl groups, carboxyl groups and the like, the graphene oxide quantum dots have extremely high hydrophilicity and biocompatibility, the graphene oxide quantum dots are deposited on the surface of a base membrane in an auxiliary mode through dopamine, and a graphene oxide quantum dot hydrophilic layer formed after reaction can effectively inhibit deposition of pollutants on the surface of the membrane; on the other hand, the graphene oxide quantum dots have quantum confinement effect and boundary effect, and can degrade organic pollutants attached to the surface of the membrane and efficiently kill bacteria under illumination, so that the membrane has self-cleaning and anti-fouling performance.
The hydrophilic self-cleaning oil-water separation membrane and the preparation method thereof provided by the invention have the following advantages:
1. the hydrophilic self-cleaning oil-water separation membrane is prepared by using a method of dopamine-assisted deposition and crosslinking, and has the advantages of simple preparation process and good repeatability.
2. According to the invention, the graphene oxide quantum dots are introduced to the surface of the base film, and the hydrophilicity and the anti-pollution performance of the film are obviously improved by utilizing the hydrophilic oxygen-containing functional groups such as rich hydroxyl, carboxyl, epoxy and the like at the edge of the graphene quantum dots.
3. According to the invention, the graphene oxide quantum dots are introduced to the surface of the base film through chemical bond linkage, the graphene oxide quantum dots are not easy to run off in the use process, and the operation stability of the oil-water separation film is good.
4. The oil-water separation membrane prepared by the invention has a self-cleaning function, flux recovery can be performed by simple illumination, the use of a chemical cleaning agent is reduced, and the operation cost of the membrane is effectively reduced.
5. The oil-water separation membrane prepared by the invention has high water permeability and high retention rate, and is suitable for industrial and domestic oily sewage treatment.
Drawings
FIG. 1 is a scanning electron micrograph of the surface of a hydrophilic self-cleaning oil-water separation membrane.
Detailed Description
The following are examples of hydrophilic self-cleaning oil-water separation membranes, but the examples are not to be construed as limiting the invention.
Example 1
(1) Modification of dopamine: soaking the polyvinylidene fluoride ultrafiltration membrane in a dopamine solution with the value of 1g/L, pH of 8.5 for 15min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyvinylidene fluoride ultrafiltration membrane;
(2) quantum dot deposition: immersing the dopamine modified ultrafiltration membrane prepared in the step (1) into a graphene oxide quantum dot water suspension with the mass concentration of 0.01% for 10min, and depositing a graphene oxide quantum dot layer on the surface of the membrane by means of dopamine to prepare a quantum dot deposition membrane;
(3) in-situ crosslinking: and (3) immersing the quantum dot deposition membrane prepared in the step (2) into MES buffer solution containing EDC and NHS, wherein the pH value is 4, the total concentration of EDC and NHS is 0.01mol/L, the molar ratio of EDC to NHS is 1: 1, and after activation reaction is carried out for 10h at room temperature, the hydrophilic self-cleaning oil-water separation membrane is prepared.
Example 2
(1) Modification of dopamine: soaking the polyvinylidene fluoride ultrafiltration membrane in a dopamine solution with the value of 3g/L, pH of 8.5 for 25min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyvinylidene fluoride ultrafiltration membrane;
(2) quantum dot deposition: immersing the dopamine modified ultrafiltration membrane prepared in the step (1) into a graphene oxide quantum dot water suspension with the mass concentration of 1.0% for 10min, and depositing a graphene oxide quantum dot layer on the surface of the membrane by means of dopamine to prepare a quantum dot deposition membrane;
(3) in-situ crosslinking: and (3) immersing the quantum dot deposition film prepared in the step (2) into MES buffer solution containing EDC and NHS, wherein the pH value is 6.5, the total concentration of EDC and NHS is 0.1mol/L, the molar ratio of EDC to NHS is 3:1, and after the activation reaction is carried out for 1h at room temperature, the hydrophilic self-cleaning oil-water separation film is prepared.
Example 3
(1) Modification of dopamine: soaking the polyvinylidene fluoride ultrafiltration membrane in a dopamine solution with the value of 3g/L, pH of 8.5 for 20min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyvinylidene fluoride ultrafiltration membrane;
(2) quantum dot deposition: immersing the dopamine modified ultrafiltration membrane prepared in the step (1) into a graphene oxide quantum dot water suspension liquid with the mass concentration of 2% for 30min, and depositing a graphene oxide quantum dot layer on the surface of the membrane by means of dopamine to prepare a quantum dot deposition membrane;
(3) in-situ crosslinking: and (3) immersing the quantum dot deposition film prepared in the step (2) into MES buffer solution containing EDC and NHS, wherein the pH value is 5.5, the total concentration of EDC and NHS is 0.05mol/L, the molar ratio of EDC to NHS is 1: 1, and after the activation reaction is carried out for 1h at room temperature, the hydrophilic self-cleaning oil-water separation film is prepared.
Example 4
(1) Modification of dopamine: soaking the polyvinylidene fluoride ultrafiltration membrane in a dopamine solution with the value of 3g/L, pH of 8.5 for 25min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyvinylidene fluoride ultrafiltration membrane;
(2) quantum dot deposition: immersing the dopamine modified ultrafiltration membrane prepared in the step (1) into a graphene oxide quantum dot water suspension with the mass concentration of 2% for 15min, and depositing a graphene oxide quantum dot layer on the surface of the membrane by means of dopamine to prepare a quantum dot deposition membrane;
(3) in-situ crosslinking: and (3) immersing the quantum dot deposition membrane prepared in the step (2) into MES buffer solution containing EDC and NHS, wherein the pH value is 5, the total concentration of EDC and NHS is 0.01mol/L, the molar ratio of EDC to NHS is 1: 1, and after the activation reaction is carried out for 1h at room temperature, the hydrophilic self-cleaning oil-water separation membrane is prepared.
Application examples
The hydrophilic self-cleaning oil-water separation membranes prepared in examples 1 to 4 were subjected to comprehensive performance tests to measure the permeation flux (L/m)2h) Contact angle (°), and flux recovery (%), the results are shown in table 1. The scanning electron micrograph of the surface of the hydrophilic self-cleaning oil-water separation membrane is shown in FIG. 1.
TABLE 1
Permeate flux (L/m)2h) Contact angle (°) Flux recovery (%)
Example 1 280 73 64
Example 2 324 64 70
Example 3 397 63 71
Example 4 420 54 77
The above description of embodiments should be taken as illustrative, and it will be readily understood that many variations and combinations of the features set forth above may be made without departing from the spirit and scope of the invention as set forth in the claims, and that such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such variations are intended to be included within the scope of the following claims.

Claims (4)

1. The preparation method of the hydrophilic self-cleaning oil-water separation membrane is characterized by comprising the following specific steps of:
(1) modification of dopamine: soaking the polyolefin base membrane in 1-3 g/L, pH value 8.5 dopamine solution for 15-25 min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain a dopamine-modified porous base membrane;
(2) quantum dot deposition: immersing the dopamine-modified porous base membrane prepared in the step (1) into a graphene oxide quantum dot aqueous suspension with the mass concentration of 0.01-2% for 10-30 min, and depositing a graphene oxide quantum dot layer on the surface of the base membrane to prepare a quantum dot deposition membrane;
the graphene oxide quantum dots are prepared by thermal decomposition of citric acid, have a zero-dimensional nano flake structure, have a particle size of 1-10 nm, and contain carboxyl groups on the surface;
(3) in-situ crosslinking: and (3) immersing the quantum dot deposition film prepared in the step (2) into a morpholine ethanesulfonic acid MES buffer solution containing 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride EDC and N-hydroxysuccinimide NHS, wherein the pH value is 4-6.5, and after an activation reaction is carried out for 1-10 h at room temperature, the hydrophilic self-cleaning oil-water separation film is prepared.
2. The method for preparing a hydrophilic self-cleaning oil-water separation membrane according to claim 1, characterized in that: in the mixed solution in the step (3), the total concentration of EDC and NHS is 0.01-0.1 mol/L, and the molar ratio of EDC to NHS is 1-3: 1.
3. The hydrophilic self-cleaning oil-water separation membrane prepared by the method of claim 1, which is characterized by comprising the following steps: the base membrane of the hydrophilic self-cleaning oil-water separation membrane is a polyolefin porous membrane, and graphene oxide quantum dots are deposited on the surface of the base membrane under the assistance of dopamine and are subjected to condensation reaction with the dopamine to form a graphene oxide quantum dot hydrophilic modification layer.
4. The hydrophilic self-cleaning oil-water separation membrane according to claim 3, characterized in that: the polyolefin porous membrane is specifically a polyolefin microfiltration membrane or a polyolefin ultrafiltration membrane; the polyolefin is polyethylene, polypropylene, polyvinyl chloride, polyvinylidene fluoride or polyacrylonitrile.
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CN112604510B (en) * 2020-12-31 2022-07-15 福州大学 Graphene oxide-carbon quantum dot composite hydrophilic oleophobic membrane
CN116603401B (en) * 2023-06-14 2024-02-27 贵州省材料产业技术研究院 Visible light driven catalytic coupling nano enzyme light cleaning film and preparation method thereof

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