CN113926315A - Rapid preparation method and application of efficient oil-water separation membrane - Google Patents
Rapid preparation method and application of efficient oil-water separation membrane Download PDFInfo
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- CN113926315A CN113926315A CN202111409336.XA CN202111409336A CN113926315A CN 113926315 A CN113926315 A CN 113926315A CN 202111409336 A CN202111409336 A CN 202111409336A CN 113926315 A CN113926315 A CN 113926315A
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- B01D67/0002—Organic membrane manufacture
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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
- B01D61/38—Liquid-membrane separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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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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- 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
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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 rapid preparation method and application of an efficient oil-water separation membrane, and belongs to the field of material surface modification. The preparation method comprises the following steps: (1) carrying out deoiling, decontamination and cleaning on the surface of the solid net film; (2) weighing hydrophobic polymer materials, dissolving the hydrophobic polymer materials in a solvent, magnetically stirring the mixture for 6-8 hours at room temperature to obtain uniform modified solution, uniformly coating the uniform modified solution on a pretreated solid net film, and drying the solid net film. According to the invention, the construction of the micro-nano structure on the surface of the solid net film and the surface hydrophobic modification are combined into the same system, so that the integral hydrophobic oleophylic effect of the material is improved, the material is cheap and easy to obtain, the preparation process is simple and quick, and the preparation process does not involve hazardous reagents such as toxic, strong-corrosivity and strong-oxidation reducing reagents and the like, so that the preparation method is suitable for large-scale industrial production; the oil-water separation mesh membrane can realize the efficient separation of oil-water mixtures, has good mechanical properties, can well realize self-supporting, and can be freely cut into required shapes during application.
Description
Technical Field
The invention relates to the technical field of material surface modification, in particular to a rapid preparation method and application of an efficient oil-water separation membrane.
Background
Along with the development of industry and the change of life style of people, the discharge of industrial oily wastewater and domestic oily sewage is increasing day by day, and the healthy life of people is harmed. Therefore, the oil-water separation technology is gradually gaining attention and has become a technical challenge related to all mankind.
At present, various oil-water separation technologies are widely researched and developed, including a sol-gel method, an etching method, an electrochemical method, a plasma treatment method and the like, which all have good effects, but have the defects of complex process and high production cost to different degrees, and are not beneficial to industrial production. The oil-water separation mesh membrane with special wettability designed and prepared based on the surface modification technology has the remarkable characteristics of simple preparation process, low material cost, high separation efficiency and the like, and can be applied to the field of industrial production.
On the other hand, most of the oil-water separation net membranes of the prior invention have long membrane preparation time and certain dangerousness in relation to dangerous reagents or preparation processes, which causes great troubles for large-scale industrial production. Therefore, the search for a safer and more efficient preparation method of the oil-water separation membrane has very important significance for better implementation of the oil-water separation membrane to industrial production.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for safely and efficiently preparing an oil-water separation mesh membrane with high separation efficiency. The preparation process adopted by the invention is simple, the membrane can be quickly prepared, the material cost is low, hazardous reagents such as toxic, strong-corrosivity and strong-oxidation-reduction reagents are not involved in the preparation process, and the high-efficiency oil-water separation net membrane with strong operability can be safely and efficiently obtained.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides a rapid preparation method of a high-efficiency oil-water separation membrane, which comprises the following steps: (1) cleaning the solid net film with acetone, ethanol and ultrapure water respectively for 20min under ultrasonic condition to remove oil stain on the surface, and drying for later use; wherein the solid net film is made of a metal phosphor copper net, a brass net, a red copper net, an aluminum net, a stainless steel net, an iron net, or a non-metal polypropylene net, a nylon fiber fabric net, a polyester net, a non-woven fabric or a polyvinyl chloride net;
(2) weighing a hydrophobic polymer material, dissolving the hydrophobic polymer material in a solvent, magnetically stirring the solution at room temperature for 6-8 hours to obtain a modified solution uniformly dissolved, uniformly coating the modified solution on a pretreated solid net membrane, and drying the solid net membrane to obtain the oil-water separation net membrane; wherein, the hydrophobic polymer material can be one or more of polyvinylidene fluoride, polyvinylidene fluoride copolymerized hexafluoropropylene, polytetrafluoroethylene, polypropylene, polyethylene and polystyrene; the solvent can be any one or mixture of acetone, N-methyl pyrrolidone, N-dimethyl acetamide and N, N-dimethyl formamide;
furthermore, the mesh number of the solid net is 200-1200 meshes, preferably 300-600 meshes, and specifically 350 meshes, 450 meshes, 550 meshes or 350-550 meshes;
preferably, the concentration of the modification solution is 2 to 40 wt%, preferably 6 to 18 wt%, and specifically may be 7 wt%, 9 wt%, 11 wt%, or 7 to 18 wt%, and the balance is a solvent;
further, the step (2) of coating the pretreated solid mesh membrane comprises the following specific steps: coating the solid net film with a modifying solution by one or more of brushing, knife coating, rolling, dipping or spraying, wherein the amount of the modifying solution is 0.03-0.08ml/cm relative to the area of the solid net film2。
In the step (2), the drying temperature is 15-130 ℃, preferably 40-60 ℃, and specifically 45 ℃, 50 ℃ and 55 ℃.
The oil-water separation mesh membrane prepared by the invention is obtained by coating a hydrophobic polymer modified material on the surface of a solid mesh membrane, and after the hydrophobic polymer is coated on a smooth solid mesh membrane and dried, on one hand, the surface of the solid mesh membrane becomes rough, and on the other hand, a network structure with certain roughness is formed in gaps of the solid mesh membrane, so that the construction of the rough structure on the surface of the solid mesh membrane is realized. Due to the construction of the rough surface structure and the coating of the low surface energy substance, the hydrophobic oil-water separator has excellent hydrophobic oleophylic performance and can be applied to the separation of oil-water mixtures.
In the application, when oil-water separation is carried out, water is blocked outside, and oil phase can be quickly infiltrated and passes through the omentum; the separated oil-water can be mixture of dichloromethane, chloroform, dichloroethane, brominated hydrocarbon and water.
Compared with the prior art, the invention has the following beneficial effects:
1. the oil-water separation mesh membrane disclosed by the invention is simple in preparation process, can be used for quickly preparing the membrane, is cheap and easily available in raw materials, is safe and efficient in preparation process, and is suitable for large-scale industrial production and application.
2. The oil-water separation net film can realize the autonomous and efficient separation of various oil-water mixtures, saves a large amount of time and labor, and has obvious economic benefit.
3. The finished separation membrane has good mechanical property, can well realize self-supporting, and can be freely designed and cut into a required shape according to requirements during application.
4. The surface of the oil-water separation membrane is inert, and the oil-water separation membrane has a development prospect in the field of analysis and detection.
Drawings
FIG. 1 is a scanning electron microscope photograph of the surface topography of the oil-water separation mesh film prepared in example 1 of the present invention;
FIG. 2 is a photograph showing contact angles of water droplets and oil droplets in the air of the oil-water separation mesh membrane prepared in example 1 of the present invention;
FIG. 3 is a photograph showing the device and separation effect of the oil-water separation net membrane prepared by the present invention for oil-water separation experiment.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
In the present invention, the materials and reagents used are not specifically described, and are commercially available.
The invention provides a rapid preparation method and application of an efficient oil-water separation membrane, and the specific embodiment is as follows.
Example 1
A rapid preparation method of a high-efficiency oil-water separation membrane comprises the following steps:
(1) respectively cleaning a 400-mesh phosphorus copper net for 20min by using acetone, ethanol and ultrapure water under an ultrasonic condition to remove oil stains on the surface, and drying at 60 ℃ for later use;
(2) weighing 0.8g of polyvinylidene fluoride, dissolving the polyvinylidene fluoride in 10mLN, N-dimethylformamide, and magnetically stirring for 8 hours at room temperature to obtain a uniformly dissolved polyvinylidene fluoride modified solution;
(3) cutting a phosphor-copper net film into a size of 5cm x 5cm, extruding 1.5ml of modified solution to one side of the net film by a needle tube, uniformly scraping the modified solution by a scraper, repeatedly scraping the turned surface of the net film once (without adding the modified solution), and drying at 50 ℃ to obtain the oil-water separation net film.
Scanning electron micrographs of the surface topography of the oil-water separation mesh film prepared in this example are shown in fig. 1, and the contact angle of the oil-water separation mesh film prepared in this example measured in air to a 5 μ L water droplet was 166 ° and the contact angle to dichloromethane was 0 ° (as shown in fig. 2).
An oil-water separation experiment was performed on the oil-water separation mesh membrane prepared in this example using the experimental apparatus shown in fig. 3. The obtained oil-water separation mesh membrane is fixed in a device, 100ml of dichloromethane/water (methyl orange dyeing) mixed solution with the volume ratio of 1:1 is poured into an upper filter cup, dichloromethane rapidly infiltrates and passes through the mesh membrane, and water is blocked above the mesh membrane, so that the purpose of oil-water separation is achieved.
Example 2
A rapid preparation method of a high-efficiency oil-water separation membrane comprises the following steps:
(1) cleaning a 500-mesh stainless steel net with acetone, ethanol and ultrapure water respectively for 20min under an ultrasonic condition to remove oil stains on the surface, and drying at 60 ℃ for later use;
(2) weighing 0.6g of polyvinylidene fluoride and 0.32g of polyvinylidene fluoride copolymerized hexafluoropropylene, dissolving the polyvinylidene fluoride and the polyvinylidene fluoride copolymerized hexafluoropropylene in a mixed solution of 6mLN, N-dimethylformamide and 4mL of acetone, and magnetically stirring for 8 hours at room temperature to obtain a uniformly dissolved polyvinylidene fluoride and polyvinylidene fluoride copolymerized hexafluoropropylene modified solution;
(3) cutting the stainless steel mesh membrane into a size of 5cm x 5cm, extruding 1ml of modified solution from a needle tube to one side of the net membrane, uniformly scraping the modified solution with a scraper, repeatedly scraping the turned surface of the net membrane once (without adding the modified solution), and drying at 60 ℃ to obtain the oil-water separation net membrane.
The contact angle of the oil-water separation membrane prepared in this example with 5. mu.L of a water droplet was measured in air to be 151 ℃ and the contact angle with chloroform to be 0 ℃.
An oil-water separation experiment was performed on the oil-water separation mesh membrane prepared in this example using the experimental apparatus shown in fig. 3. Fixing the obtained oil-water separation mesh membrane in a device, pouring 100ml of chloroform/water (methyl orange dyeing) mixed solution with the volume ratio of 1:1 into an upper filter cup, quickly infiltrating the chloroform and passing through the mesh membrane, and blocking water above the mesh membrane, thereby achieving the purpose of oil-water separation.
Example 3
A rapid preparation method of a high-efficiency oil-water separation membrane comprises the following steps:
(1) respectively cleaning a 450-mesh nylon net with acetone, ethanol and ultrapure water for 20min under an ultrasonic condition to remove oil stains on the surface, and drying at 60 ℃ for later use;
(2) weighing 0.72g of polyvinylidene fluoride copolymerized hexafluoropropylene, dissolving in 10mL of N, N-dimethylformamide, and magnetically stirring for 8 hours at room temperature to obtain a uniformly dissolved polyvinylidene fluoride copolymerized hexafluoropropylene modified solution;
(3) cutting a nylon net film into 5cm by 5cm, extruding 1.2ml of modified solution to one side of the net film, uniformly brushing the modified solution with a brush, repeatedly brushing the turned surface of the net film once (without adding the modified solution), and drying at 50 ℃ to obtain the oil-water separation net film.
The contact angle of the oil-water separation mesh membrane prepared in this example measured in air to a 5. mu.L water drop was 153 °, and the contact angle to chloroform was 0 °.
An oil-water separation experiment was performed on the oil-water separation mesh membrane prepared in this example using the experimental apparatus shown in fig. 3. The obtained oil-water separation mesh membrane is fixed in a device, 100ml of chloroform/water (methyl orange dyeing) mixed solution with the volume ratio of 1:1 is poured into an upper filter cup, the chloroform rapidly infiltrates and passes through the mesh membrane, and the water is blocked above the mesh membrane, so that the purpose of oil-water separation is achieved.
Example 4
A rapid preparation method of a high-efficiency oil-water separation membrane comprises the following steps:
(1) cleaning a 200-mesh polypropylene net with acetone, ethanol and ultrapure water respectively for 20min under an ultrasonic condition to remove oil stains on the surface, and drying at 60 ℃ for later use;
(2) weighing 0.2g of polyethylene, dissolving the polyethylene in 10 mLN-methyl pyrrolidone, and magnetically stirring for 6 hours at room temperature to obtain a uniformly dissolved polyethylene modified solution;
(3) cutting the polypropylene net film into 5 cm-5 cm size, taking 5ml of modified solution, immersing the polypropylene net film in the polyethylene solution for 1min, taking out and drying at 130 ℃ to obtain the oil-water separation net film.
The contact angle of the oil-water separation membrane prepared in this example with 5. mu.L of a water drop was measured in air at 156 ℃ and the contact angle with dichloroethane at 0 ℃.
Example 5
A rapid preparation method of a high-efficiency oil-water separation membrane comprises the following steps:
(1) cleaning a 1200-mesh brass net with acetone, ethanol and ultrapure water respectively for 20min under an ultrasonic condition to remove oil stains on the surface, and drying at 60 ℃ for later use;
(2) weighing 2.25g of polytetrafluoroethylene and 3g of polystyrene, dissolving in 10mL of acetone, and magnetically stirring for 7 hours at room temperature to obtain a uniformly dissolved polytetrafluoroethylene and polystyrene mixed modified solution;
(3) cutting a brass net film into the size of 5cm by 5cm, putting the modified solution into a spray gun, uniformly spraying the two surfaces of the suspended net film, wherein the amount of the modified solution consumed by each net film is 1.3mL, and drying at 80 ℃ to obtain the oil-water separation net film.
The contact angle of the oil-water separation mesh membrane prepared in this example to a 5. mu.L water drop was measured in air at 164 ℃ and the contact angle to dichloroethane at 0 ℃.
To further illustrate the beneficial effects of the present application, a comparative example was constructed as follows, using example 1 as an example only, for reasons of space.
Comparative example 1
In this comparative example, the treated 400 mesh phosphocopper mesh was replaced with filter paper, and the rest of the conditions were the same as in example 1.
The contact angle of the oil-water separation mesh membrane prepared in this example to a 5. mu.L water droplet was measured in air at 92 ℃ and the contact angle to chloroform at 0 ℃.
An oil-water separation experiment was performed on the oil-water separation mesh membrane prepared in this example using the experimental apparatus shown in fig. 3. The oil-water separation mesh membrane obtained above is fixed in a device, 100ml of mixed solution of chloroform/water (methyl orange dyeing) with the volume ratio of 1:1 is poured into an upper filter cup, the chloroform can infiltrate and pass through the mesh membrane, but part of water can also pass through the mesh membrane, and the rest water is blocked above the mesh membrane, so that the oil-water separation effect is poor.
Comparative example 2
A preparation method of an oil-water separation membrane comprises the following steps:
(1) respectively cleaning a 400-mesh phosphorus copper net for 20min by using acetone, ethanol and ultrapure water under an ultrasonic condition to remove oil stains on the surface, and drying at 60 ℃ for later use;
(2) weighing 0.8g of polyvinylidene fluoride and 1.5 parts of silicon dioxide (10-50 microns) and adding the mixture into 10mLN, N-dimethylformamide, and magnetically stirring the mixture for 8 hours at room temperature to obtain modified liquid;
(3) and (3) uniformly blade-coating the modified liquid on the phosphor-copper screen treated in the step (1), and drying at 50 ℃.
The contact angle of the oil-water separation membrane prepared in this example with 5. mu.L of a water droplet was measured in air at 112 ℃ and with chloroform at 0 ℃.
An oil-water separation experiment was performed on the oil-water separation mesh membrane prepared in this example using the experimental apparatus shown in fig. 3. The oil-water separation mesh membrane obtained above was fixed in a device, and 100ml of a chloroform/water (methyl orange-dyed) mixed solution at a volume ratio of 1:1 was poured into the upper filter cup, and chloroform was able to pass through the mesh membrane only slowly, and water was blocked above the mesh membrane, and although the purpose of oil-water separation could be achieved, the separation speed was slow.
In conclusion, the oil-water separation mesh membrane prepared by the invention is obtained by coating a hydrophobic polymer modified material on the surface of a solid mesh membrane, and has excellent hydrophobic and oleophilic properties due to the construction of a surface rough structure and the coating of a low-surface-energy substance, so that the oil-water separation mesh membrane can be applied to oil-water mixture separation.
The foregoing is a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and are intended to be within the scope of the invention.
Claims (10)
1. A rapid preparation method of a high-efficiency oil-water separation membrane is characterized by comprising the following steps:
(1) ultrasonically cleaning the solid net film for 20min by using acetone, ethanol and ultrapure water respectively to remove oil stains on the surface, and drying for later use;
(2) weighing a proper amount of hydrophobic polymer material, dissolving the hydrophobic polymer material in a solvent, stirring the solution at room temperature for 6-8 hours to obtain a uniform modified solution, coating the modified solution on a pretreated solid net film, and drying the solid net film to obtain the oil-water separation net film, wherein the oil-water separation net film has a contact angle of more than 150 degrees to water drops.
2. The method for rapidly preparing an efficient oil-water separation membrane according to claim 1, wherein the solid net membrane is a phosphor-copper net, a brass net, a red copper net, an aluminum net, a stainless steel net or an iron net made of metal.
3. The method for rapidly preparing a high-efficiency oil-water separation membrane according to claim 1, wherein the solid net membrane is a non-metallic nylon fiber fabric net, a polypropylene net, a polyester net, a non-woven fabric or a polyvinyl chloride net.
4. The method for rapidly preparing the high-efficiency oil-water separation membrane according to claim 2 or 3, wherein the mesh number of the solid membrane is 200-1200 meshes.
5. The method for rapidly preparing the high-efficiency oil-water separation membrane according to claim 4, wherein the hydrophobic polymer material is one or more of polyvinylidene fluoride, polyvinylidene fluoride-co-hexafluoropropylene, polytetrafluoroethylene, polypropylene, polyethylene, polystyrene and polymethyl methacrylate.
6. The method for rapidly preparing the high-efficiency oil-water separation membrane according to claim 5, wherein the solvent is any one or more of acetone, N-methylpyrrolidone, N-dimethylacetamide and N, N-dimethylformamide.
7. The method for rapidly preparing a high efficiency oil-water separation membrane according to claim 6, wherein the concentration of the hydrophobic polymer material in the modified solution is 2 to 40 wt%.
8. The method for rapidly preparing the high-efficiency oil-water separation membrane according to claim 7, wherein the step (2) of coating the membrane on the pretreated solid net membrane comprises the following specific steps: coating the solid net film with a modifying solution by one or more of brushing, knife coating, rolling, dipping or spraying, wherein the amount of the modifying solution is 0.03-0.08ml/cm relative to the area of the solid net film2。
9. The method for rapidly preparing the high-efficiency oil-water separation membrane according to claim 8, wherein in the step (1), the drying temperature is 15-130 ℃;
in the step (2), the drying temperature is 15-130 ℃.
10. The application of the high-efficiency oil-water separation membrane in oil-water separation is characterized in that the high-efficiency oil-water separation membrane is prepared by the method of any one of claims 1 to 9; the oil phase in the oil-water mixture is one or more of dichloromethane, chloroform, dichloroethane and brominated hydrocarbon.
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| CN114395938A (en) * | 2021-09-22 | 2022-04-26 | 中国科学院长春应用化学研究所 | Starch-based hydrophobic paper, and preparation method and application thereof |
| CN114713038A (en) * | 2022-03-30 | 2022-07-08 | 深圳维度新材料有限公司 | Micro-nano fiber membrane and preparation method and application thereof |
| CN115445246A (en) * | 2022-08-24 | 2022-12-09 | 电子科技大学 | High-performance surface-modified oil-water separation membrane and preparation method and application thereof |
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| CN115445246B (en) * | 2022-08-24 | 2023-10-20 | 电子科技大学 | High-performance surface-modified oil-water separation membrane and preparation method and application thereof |
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