CN110124527B - Method for preparing high-flux graphene oxide quantum dot composite nanofiltration membrane through dopamine-assisted deposition - Google Patents
Method for preparing high-flux graphene oxide quantum dot composite nanofiltration membrane through dopamine-assisted deposition Download PDFInfo
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- CN110124527B CN110124527B CN201910469237.7A CN201910469237A CN110124527B CN 110124527 B CN110124527 B CN 110124527B CN 201910469237 A CN201910469237 A CN 201910469237A CN 110124527 B CN110124527 B CN 110124527B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
Abstract
The invention relates to a method for preparing a high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition, and belongs to the technical field of membrane separation. The method comprises the steps of using a polyacrylonitrile ultrafiltration membrane as a base membrane, firstly carrying out carboxylation modification in alkali liquor, then immersing the polyacrylonitrile ultrafiltration membrane into a dopamine solution for base membrane modification to form a poly-dopamine layer, then immersing the poly-dopamine layer into a graphene oxide quantum dot solution, carrying out assisted deposition of a graphene oxide quantum dot layer on the surface of the base membrane by means of the poly-dopamine layer, and finally carrying out in-situ crosslinking in a crosslinking agent solution to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane. The high-flux graphene oxide quantum dot composite nanofiltration membrane is prepared by a method of firstly carrying out dopamine coating and then carrying out interfacial polymerization, and the preparation method is novel in preparation process, simple and excellent in operation stability.
Description
Technical Field
The invention relates to a method for preparing a high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition, and belongs to the technical field of membrane separation.
Background
With the increasing world population and the increasing water pollution problem, the global total amount of fresh water begins to decline, and water resource shortage becomes a global concern. In order to alleviate the global water crisis, people have conducted extensive research and exploration on economic and effective seawater desalination and water treatment technologies. Nanofiltration has received wide attention in the fields of desalination, wastewater treatment, and the like. However, due to the inherent limitations of conventional nanofiltration membranes, the preparation of nanofiltration membranes with high flux while maintaining good rejection remains a challenging task. Ultra-thin nanofiltration membranes reduce mass transfer resistance and concentration polarization, increase water flux, and smaller nanoparticles reduce membrane surface roughness and enhance permeability. So that the construction of an ultrathin nano-particle nanofiltration membrane is very important.
Graphene oxide membranes have received a great deal of attention in the fields of water purification and desalination due to their unique layer-by-layer stacking structure. Graphene oxide quantum dots with smaller sheet sizes can provide a shorter path for water molecules to penetrate through the graphene oxide film than larger graphene oxide sheets. The edges of the graphene oxide quantum dots contain more hydrophilic groups such as carboxyl, hydroxyl, epoxy and the like, so that the hydrophilicity of the surface of the film is greatly improved, and water molecules easily penetrate through the surface of the film. In addition, the distribution of the graphene oxide quantum dots on the surface layer is more uniform, so that the stretching of the graphene oxide quantum dots on the surface layer is smaller, a smoother surface is obtained, and the antifouling performance of the graphene oxide quantum dots is improved. These excellent characteristics make graphene oxide quantum dots excellent separation membrane materials. However, the extremely small sheet size and inorganic nature of graphene oxide quantum dots makes it technically challenging to form ultra-thin defect-free composite nanofiltration membranes.
Disclosure of Invention
The invention aims to overcome the defects and provides a method for preparing a high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition.
The technical scheme includes that a polyacrylonitrile ultrafiltration membrane is used as a base membrane, firstly, carboxylation modification is carried out in alkali liquor, then, the base membrane is immersed in a dopamine solution for base membrane modification to form a poly-dopamine layer, then, the poly-dopamine layer is immersed in a graphene oxide quantum dot solution, the poly-dopamine layer is used for assisting in depositing a graphene oxide quantum dot layer on the surface of the base membrane, and finally, in-situ crosslinking is carried out in a cross-linking agent solution, so that the high-flux graphene oxide quantum dot composite nanofiltration membrane is obtained.
Further, the method comprises the following specific steps:
(1) pretreatment of a base film: soaking a polyacrylonitrile ultrafiltration membrane in 1-3 mol/L sodium hydroxide aqueous solution for 14-24 h, taking out, washing with deionized water, and soaking for 20-24 h to obtain a carboxylated polyacrylonitrile ultrafiltration membrane;
(2) modification of dopamine: soaking the carboxylated polyacrylonitrile ultrafiltration membrane obtained in the step (1) in a dopamine solution with the value of 1-3 g/L, pH being 8.5 for 15-25 min, self-assembling to form a polydopamine modification layer, taking out, washing with water and obtaining the dopamine modified polyacrylonitrile ultrafiltration membrane;
(3) and (3) depositing graphene oxide quantum dots: immersing the dopamine modified polyacrylonitrile ultrafiltration membrane prepared in the step (2) into 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 a base membrane by means of dopamine to prepare a composite membrane;
(4) in-situ crosslinking: and (4) immersing the composite membrane obtained in the step (3) into a cross-linking agent solution with the mass concentration of 0.01-0.5% for 5-10 min, adjusting the reaction temperature, and performing in-situ cross-linking to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane.
Further, the aperture of the polyacrylonitrile ultrafiltration basement membrane in the step (1) is 5-80 nm.
Further, the thickness of the polydopamine layer in the step (2) is 5-50 nm.
Further, the dopamine solution in the step (2) is prepared by dissolving dopamine in a tris buffer solution, wherein the concentration of the buffer solution is 10 mmol/L.
Further, the thickness of the graphene oxide quantum dot layer in the step (3) is 15-150 nm.
Further, the graphene oxide quantum dots in the step (3) are prepared by a citric acid pyrolysis method, the particle size is 1-5 nm, and the number of layers is 1-40.
Further, the specific preparation process of the graphene oxide quantum dots is as follows: adding 5-10 g of citric acid into a 250mL round-bottom flask, heating to 200 ℃ through a heating jacket, and keeping for 15-20 min. The resulting liquid was immediately added dropwise to 250mL of a 1.0mol/L NaOH solution under vigorous magnetic stirring. The solution was further neutralized to pH 7.0, and the dialyzed solution was freeze-dried to obtain graphene oxide quantum dots.
Further, the cross-linking agent in the step (4) is aromatic acyl chloride.
Further, the crosslinking agent in the step (4) is one or a combination of more of trimesoyl chloride, phthaloyl chloride, 5-isocyanic isophthaloyl dichloride, 1, 3, 5-trimethyloyl chloride cyclohexane and biphenyl tetracoyl chloride.
Further, the crosslinking reaction temperature in the step (4) is 5-50 ℃.
According to the method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane through dopamine-assisted deposition, on one hand, the size of the graphene oxide quantum dot is small, the graphene oxide quantum dot is deposited in an assisted manner to form more water channels in an interfacial polymerization layer, and the graphene oxide quantum dot is uniformly accumulated on the surface of the membrane, so that the surface is smoother, water can pass through the surface, and the anti-fouling performance is improved; on the other hand, the super-hydrophilicity of the graphene oxide quantum dots can improve the surface hydrophilicity of the membrane, so that the water flux and the anti-pollution performance are improved; on the other hand, the thickness of the polydopamine layer and the graphene oxide quantum dots can be effectively controlled according to different deposition time and concentration, and the graphene oxide quantum dots are uniformly accumulated on the surface of the membrane, so that the defect-free high-flux graphene oxide quantum dot nanofiltration membrane is formed. In addition, the in-situ crosslinking of the graphene oxide quantum dots can inhibit the graphene oxide quantum dots from swelling in water or in a high-humidity environment, so that the performance stability of the composite nanofiltration membrane is improved.
The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition has the following advantages:
1. the high-flux anti-fouling composite nanofiltration membrane is prepared by a method of firstly preparing the polydopamine adsorption layer and then carrying out interfacial polymerization, and the preparation method is rapid and simple to operate.
2. According to the method, the graphene oxide quantum dots are introduced to the surface of the nanofiltration membrane, and the high-flux anti-fouling nanofiltration membrane is prepared by utilizing the hydrophilic hydroxyl, carboxyl and zero-dimensional structures on the edges of the graphene oxide quantum dots.
3. The graphene oxide quantum dots exist in the nanofiltration membrane through chemical bonds, have high stability, and cannot fall off after long-time operation in water.
4. According to the invention, a polydopamine layer is introduced on the porous carrier to generate stronger adsorption capacity, so that graphene oxide quantum dots are effectively captured from an ultra-dilute solution to form uniform accumulation, the thicknesses of the polydopamine layer and the graphene oxide quantum dot layer can be effectively controlled, and the ultra-thin defect-free nanofiltration membrane is easily formed after polymerization.
Detailed Description
The following is an example of preparation of the high-throughput graphene oxide quantum dot composite nanofiltration membrane, but the example does not limit the present invention.
Example 1
(1) Pretreatment of a base film: soaking the polyacrylonitrile ultrafiltration membrane in 1mol/L sodium hydroxide aqueous solution for 24h, taking out, washing with deionized water, and soaking for 24h to obtain a carboxylated polyacrylonitrile ultrafiltration membrane;
(2) modification of dopamine: soaking the carboxylated polyacrylonitrile ultrafiltration membrane obtained in the step (1) in a dopamine solution with the value of 3g/L, pH of 8.5 for 15min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyacrylonitrile ultrafiltration membrane;
(3) and (3) depositing graphene oxide quantum dots: immersing the dopamine modified polyacrylonitrile ultrafiltration membrane prepared in the step (2) into a graphene oxide quantum dot water suspension with the mass concentration of 0.5% for 10min, and depositing a graphene oxide quantum dot layer on the surface of a base membrane by means of dopamine to prepare a composite membrane;
(4) in-situ crosslinking: and (4) immersing the composite membrane obtained in the step (3) into a n-hexane solution with the mass concentration of 0.02% of phthaloyl chloride for 5min, adjusting the reaction temperature, and performing in-situ crosslinking to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane.
The separation performance test results of the prepared high-flux graphene oxide quantum dot composite nanofiltration membrane are specifically shown in table 1.
Example 2
(1) Pretreatment of a base film: soaking the polyacrylonitrile ultrafiltration membrane in 3mol/L sodium hydroxide aqueous solution for 14h, taking out, washing with deionized water, and soaking for 20h to obtain a carboxylated polyacrylonitrile ultrafiltration membrane;
(2) modification of dopamine: soaking the carboxylated polyacrylonitrile ultrafiltration membrane obtained in the step (1) in a dopamine solution with the value of 2g/L, pH of 8.5 for 20min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyacrylonitrile ultrafiltration membrane;
(3) and (3) depositing graphene oxide quantum dots: immersing the dopamine modified polyacrylonitrile ultrafiltration membrane prepared in the step (2) into a graphene oxide quantum dot water suspension liquid with the mass concentration of 1% for 15min, and depositing a graphene oxide quantum dot layer on the surface of a base membrane by means of dopamine to prepare a composite membrane;
(4) in-situ crosslinking: and (4) immersing the composite membrane obtained in the step (3) into a normal hexane solution with the mass concentration of 0.1% trimesoyl chloride for 5min, adjusting the reaction temperature, and performing in-situ crosslinking to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane.
The separation performance test results of the prepared high-flux graphene oxide quantum dot composite nanofiltration membrane are specifically shown in table 1.
Example 3
(1) Pretreatment of a base film: soaking the polyacrylonitrile ultrafiltration membrane in 1mol/L sodium hydroxide aqueous solution for 20h, taking out, washing with deionized water, and soaking for 22h to obtain a carboxylated polyacrylonitrile ultrafiltration membrane;
(2) modification of dopamine: soaking the carboxylated polyacrylonitrile ultrafiltration membrane obtained in the step (1) in a dopamine solution with the value of 1g/L, pH of 8.5 for 20min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyacrylonitrile ultrafiltration membrane;
(3) and (3) depositing graphene oxide quantum dots: immersing the dopamine modified polyacrylonitrile ultrafiltration membrane prepared in the step (2) into a graphene oxide quantum dot water suspension liquid with the mass concentration of 2% for 10min, and depositing a graphene oxide quantum dot layer on the surface of a base membrane by means of dopamine to prepare a composite membrane;
(4) in-situ crosslinking: and (4) immersing the composite membrane obtained in the step (3) into a normal hexane solution with the mass concentration of 0.05% trimesoyl chloride for 7min, adjusting the reaction temperature, and performing in-situ crosslinking to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane.
The separation performance test results of the prepared high-flux graphene oxide quantum dot composite nanofiltration membrane are specifically shown in table 1.
Example 4
(1) Pretreatment of a base film: soaking the polyacrylonitrile ultrafiltration membrane in 1mol/L sodium hydroxide aqueous solution for 14h, taking out, washing with deionized water, and soaking for 20h to obtain a carboxylated polyacrylonitrile ultrafiltration membrane;
(2) modification of dopamine: soaking the carboxylated polyacrylonitrile ultrafiltration membrane obtained in the step (1) in a dopamine solution with the value of 2g/L, pH of 8.5 for 15min, self-assembling to form a polydopamine modification layer, taking out and washing to obtain the dopamine modified polyacrylonitrile ultrafiltration membrane;
(3) and (3) depositing graphene oxide quantum dots: immersing the dopamine modified polyacrylonitrile ultrafiltration membrane prepared in the step (2) into a graphene oxide quantum dot water suspension liquid with the mass concentration of 0.05% for 30min, and depositing a graphene oxide quantum dot layer on the surface of a base membrane by means of dopamine to prepare a composite membrane;
(4) in-situ crosslinking: and (4) immersing the composite membrane obtained in the step (3) into a normal hexane solution of 0.08% of biphenyltetracarbonyl for 7min, adjusting the reaction temperature, and performing in-situ crosslinking to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane.
The separation performance test results of the prepared high-flux graphene oxide quantum dot composite nanofiltration membrane are specifically shown in table 1.
TABLE 1
Note: testing under pure water for 3h, and changing to Na2SO4The solution is tested for 2 hours, then the test solution is changed to 100mg/L BSA solution with pH 7 for testing for 4 hours, the tested nanofiltration membrane is washed with clear water for 4 hours, the washed membrane is repeated the first two steps again, and pure water flux and sodium sulfate interception are tested.
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 (8)
1. A method for preparing a high-flux graphene oxide quantum dot composite nanofiltration membrane through dopamine-assisted deposition is characterized by comprising the following steps: the method comprises the following steps of taking a polyacrylonitrile ultrafiltration membrane as a base membrane, firstly carrying out carboxylation modification in alkali liquor, then immersing the polyacrylonitrile ultrafiltration membrane into a dopamine solution for base membrane modification to form a poly-dopamine layer, then immersing the poly-dopamine layer into a graphene oxide quantum dot solution, carrying out assisted deposition of a graphene oxide quantum dot layer on the surface of the base membrane by means of the poly-dopamine layer, and finally carrying out in-situ crosslinking in a crosslinking agent solution to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane;
the method comprises the following specific steps:
(1) pretreatment of a base film: soaking a polyacrylonitrile ultrafiltration membrane in 1-3 mol/L sodium hydroxide aqueous solution for 14-24 h, taking out, washing with deionized water, and soaking for 20-24 h to obtain a carboxylated polyacrylonitrile ultrafiltration membrane;
(2) modification of dopamine: soaking the carboxylated polyacrylonitrile ultrafiltration membrane obtained in the step (1) in a dopamine solution with the value of 1-3 g/L, pH being 8.5 for 15-25 min, self-assembling to form a polydopamine modification layer, taking out, washing with water and obtaining the dopamine modified polyacrylonitrile ultrafiltration membrane;
(3) and (3) depositing graphene oxide quantum dots: immersing the dopamine modified polyacrylonitrile ultrafiltration membrane prepared in the step (2) into 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 a base membrane by means of dopamine to prepare a composite membrane;
(4) in-situ crosslinking: and (4) immersing the composite membrane obtained in the step (3) into a cross-linking agent solution with the mass concentration of 0.01-0.5% for 5-10 min, adjusting the reaction temperature, and performing in-situ cross-linking to obtain the high-flux graphene oxide quantum dot composite nanofiltration membrane.
2. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 1, which is characterized in that: the aperture of the polyacrylonitrile ultrafiltration basement membrane in the step (1) is 5-80 nm.
3. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 1, which is characterized in that: and (3) the thickness of the polydopamine layer in the step (2) is 5-50 nm.
4. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 1, which is characterized in that: and (3) the thickness of the graphene oxide quantum dot layer in the step (3) is 15-150 nm.
5. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 1, which is characterized in that: the particle size of the graphene oxide quantum dots in the step (3) is 1-5 nm, and the number of layers is 1-40.
6. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 1, which is characterized in that: and (4) the cross-linking agent is aromatic acyl chloride.
7. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 6, which is characterized in that: the cross-linking agent in the step (4) is one or a combination of more of trimesoyl chloride, phthaloyl chloride, 5-isocyanic isophthaloyl dichloride, 1, 3, 5-trimethyloyl chloride cyclohexane and biphenyl tetracarbonyl.
8. The method for preparing the high-flux graphene oxide quantum dot composite nanofiltration membrane by dopamine-assisted deposition as claimed in claim 1, which is characterized in that: and (4) the crosslinking reaction temperature is 5-50 ℃.
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| CN111214964A (en) * | 2020-01-15 | 2020-06-02 | 上海翊科精密挤出技术有限公司 | Surface modified oxygenator membrane and preparation method thereof |
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| CN113797772A (en) * | 2020-06-12 | 2021-12-17 | 三达膜科技（厦门）有限公司 | Graphene oxide modified polydopamine composite nanofiltration membrane and preparation method thereof |
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