CN110772996A - Preparation method of novel three-dimensional solar energy photo-thermal oil-water separator - Google Patents
Preparation method of novel three-dimensional solar energy photo-thermal oil-water separator Download PDFInfo
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- CN110772996A CN110772996A CN201911086898.8A CN201911086898A CN110772996A CN 110772996 A CN110772996 A CN 110772996A CN 201911086898 A CN201911086898 A CN 201911086898A CN 110772996 A CN110772996 A CN 110772996A
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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
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/366—Apparatus therefor
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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
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/364—Membrane distillation
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- 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
- B01D67/0039—Inorganic membrane manufacture
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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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/22—Thermal or heat-resistance properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
Abstract
The invention discloses a preparation method of a novel three-dimensional solar photo-thermal oil-water separator, which comprises the following preparation steps: cutting the foam Cu into rectangles, and respectively cleaning the rectangles with hydrochloric acid, absolute ethyl alcohol, acetone and deionized water for later use; preparing a mixed aqueous solution of sodium hydroxide and ammonium persulfate, soaking the cleaned foam Cu in the mixed aqueous solution, taking out the foam Cu, cleaning the foam Cu by using deionized water, soaking the foam Cu in sodium sulfide, taking out the foam Cu, bending the foam Cu into an inverted U-shaped form, and placing the inverted U-shaped Cu into a mold
xS/foam Cu vertically penetrates through the supportable substrate to obtain the Cu with the three-dimensional hierarchical structure
xAnd S, compounding the photo-thermal film. Three-dimensional hierarchical structure Cu prepared by the method
xThe S composite photo-thermal film has low cost and light absorption energyThe composite copper-based sulfide material has strong force and high photo-thermal conversion efficiency, greatly reduces the manufacturing cost of devices and improves the stability of the devices; the photo-thermal efficiency is high, the separation performance is good, any electric drive is not needed, and the cost performance is high.
Description
Technical Field
The invention relates to the technical field of membrane separation, in particular to a preparation method of a novel three-dimensional solar photo-thermal oil-water separator.
Background
Water is one of the most important resources for public health and social development. However, the shortage of fresh water has become one of the important problems of social concern. In order to solve this problem, a new water treatment technology that can recover fresh water from wastewater or seawater is urgently required. In recent years, solar distillation technology has received great attention in the fields of seawater desalination and sewage treatment due to its carbon dioxide zero emission feature. The working principle is as follows: the photothermal membrane is placed on the water surface, the solar energy is absorbed and converted into heat energy, the generation of water vapor from the gas-liquid interface is accelerated through the heat energy, and finally, the fresh water is obtained through condensation. Over the past few years, many solar water evaporation films have been manufactured based on various types of materials, such as: carbon-based materials, metals, metal oxides/carbides, and polymers. However, these photo-thermal films still show significant disadvantages, and they are susceptible to oil contamination during oil-water separation, resulting in a significant drop in fresh water extraction efficiency. Therefore, the development of a novel efficient oil-resistant photo-thermal conversion film is of great significance.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a preparation method of a novel three-dimensional solar energy photo-thermal oil-water separator.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that: a preparation method of a novel three-dimensional solar energy photo-thermal oil-water separator comprises the following preparation steps,
(1) cutting the foam Cu into rectangles, and respectively cleaning the rectangles with hydrochloric acid, absolute ethyl alcohol, acetone and deionized water for later use;
(2) preparing a mixed aqueous solution of sodium hydroxide and ammonium persulfate, soaking the cleaned foam Cu in the mixed aqueous solution for a period of time, taking out the foam Cu, and cleaning the foam Cu with deionized water to obtain Cu (OH) with a hierarchical structure
2Foamed Cu;
(3) soaking the foamy copper obtained in the step (2) in sodium sulfide for a period of time, and taking out to obtain Cu with a hierarchical structure
xS/foam Cu;
(4) bending the foamy copper obtained in the step (3) into an inverted U shape to obtain a high-efficiency oil-stain-resistant three-dimensional hierarchical structure evaporation film;
(5) subjecting the inverted U-shaped Cu obtained in the step (4)
xS/foam Cu vertically penetrates through the supportable substrate to obtain the Cu with the three-dimensional hierarchical structure
xS composite photo-thermal film, namely a solar photo-thermal oil-water separator with a three-dimensional structure.
Further, in the step (1), the pore diameter of the foam Cu is 100PPI, the concentration of hydrochloric acid is 1mol/L, and 200mL of absolute ethyl alcohol and acetone are both used.
Further, in the step (2), the concentration ratio of the sodium hydroxide to the ammonium persulfate is 20:1, the total volume of the mixed solution is 250mL, and the soaking time of the foam Cu is 1 hour.
Further, in the step (3), the concentration of sodium sulfide is 1mM-9mM, and the soaking time is 4 hours, wherein the change of the concentration of sodium sulfide is used for adjusting the chemical composition.
Furthermore, the regulation and control of the water delivery depth and the evaporation area are realized by controlling the lengths of the two ends and the width of the top surface of the inverted U-shaped structure in the step (4).
Further, the inverted U-shaped evaporation membrane is erected by the support substrate in the step (5), the evaporation membrane is prevented from being completely immersed in the solution, a three-dimensional evaporation structure is formed, and the immersion depth and the upper end evaporation area of the evaporation membrane are adjusted through the support substrate, so that the water delivery rate and the evaporation rate are controlled.
Further, the material of the support substrate in the step (5) is foam or flat plate which has stable structure, can be perforated and has floating property or physical support property.
Further, the support substrate is made of polystyrene foam or aluminum plate.
The invention has the beneficial effects that:
(1) the method of the invention obtains the Cu with the three-dimensional hierarchical structure
xThe S composite photo-thermal membrane replaces the traditional artificially synthesized porous organic separation membrane material with complex preparation process and poor tolerance.
(2) Three-dimensional hierarchical structure Cu prepared by the method
xThe S composite photo-thermal film adopts a composite copper-based sulfide material with low cost, strong light absorption capacity and high photo-thermal conversion efficiency to replace the traditional plasma noble metal particles, such as: gold, platinum and the like as light absorption and conversion materials greatly reduce the manufacturing cost of the device and improve the stability of the device.
(3) The solar oil-water separation membrane obtained by the invention has high photo-thermal efficiency, good separation performance, no need of any electric drive and high cost performance.
(4) The preparation process is simple, easy to popularize and easy to realize large-scale preparation.
Drawings
FIG. 1 is a structural object diagram of a three-dimensional solar photo-thermal oil-water separator manufactured by the invention;
FIG. 2 is a scanning electron micrograph of a hierarchical CuxS/foam Cu structure;
FIG. 3 is a contact plus measurement diagram of a hierarchical CuxS/foam Cu structure;
FIG. 4 is an optical micrograph before/after separation of an oil-water solution.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
With the attached drawings 1-4, the technical scheme adopted by the invention is as follows: a preparation method of a novel three-dimensional solar energy photo-thermal oil-water separator comprises the following preparation steps,
(1) cutting foamed Cu with the pore diameter of about 100PPI into a rectangle of 3cm multiplied by 10cm, and respectively washing with 1mol/L hydrochloric acid, 200mL absolute ethyl alcohol, 200mL acetone and 200mL deionized water for later use;
(2) preparing 250mL of mixed aqueous solution of sodium hydroxide and ammonium persulfate with the concentration ratio of 20:1, soaking the cleaned foam Cu in the mixed aqueous solution for 1 hour, taking out the foam Cu, and cleaning the foam Cu with deionized water to obtain Cu (OH) with a hierarchical structure
2Foamed Cu;
(3) the Cu (OH) obtained in (2)
2Soaking foamed Cu in 1-9 mM sodium sulfide solution for 4 hr, taking out, washing with deionized water to obtain Cu with hierarchical structure
xS/foam Cu, wherein the chemical composition can be adjusted by changing the concentration of sodium sulfide;
(4) the Cu obtained in (3)
xBending the S/foam Cu into an inverted U shape to obtain a high-efficiency and oil-stain-resistant evaporation film with a three-dimensional hierarchical structure;
(5) the inverted U-shaped Cu obtained in the step (4)
xThe S/foam Cu vertically penetrates through the supportable substrate, and the simple evaporator with the three-dimensional structure can be obtained, for example, the support substrate used in the figure 1 is polystyrene foam.
As can be seen from FIG. 2, the foam Cu surface treated by the preparation method of the present invention is full of hairy hierarchical structure CuxS nanorod material, and the nanorod surface presents obvious rough structure, which not only helps to improve the light scattering of incident sunlight, but also increases the evaporation area, and improves the photo-thermal conversion efficiency and the water evaporation rate.
FIG. 3 is a graph of contact angle measurement, and Cu can be seen
xS/foamThe Cu photothermal film can rapidly absorb water in the air, has super-hydrophilic characteristics, has obvious blocking effect on oil drops in the water, and has excellent underwater super-oleophobic characteristics. The super-hydrophilic and underwater super-oleophobic characteristics enable the prepared three-dimensional inverted U-shaped evaporation membrane structure to only transport water to the evaporation layer from two ends, and oil stains are blocked in oil-water mixing at the bottom, so that good oil stain resistance is achieved.
Fig. 4 is an optical photograph and a micrograph of the oil-water mixture treated by the present invention before/after separation, and it can be seen that the separated solution is clear and oil drops before separation are not observed under a microscope, which illustrates the feasibility of oil-water separation by the present invention.
Based on the three-dimensional porous structure of the Cu foam and the flexible and bendable characteristic thereof, the method skillfully designs the Cu foam into a three-dimensional inverted U-shaped three-dimensional structure, and grows the hierarchical structure Cu with the super-hydrophilic and underwater super-oleophobic characteristics on the surface of the porous framework in situ
xS composite photo-thermal material, and realizes the preparation of novel, high-efficiency and oil stain-resistant photo-thermal film. The Cu substrate selected by the invention is low in price, simple in preparation process and suitable for large-scale production; prepared hierarchical structure Cu
xThe S composite photo-thermal material can obviously increase the evaporation surface area, not only has a strong light capture effect, but also has high-efficiency photo-thermal conversion performance; the designed three-dimensional evaporation structure can increase the evaporation area, effectively isolate an evaporation layer from an oil stain layer and realize a long-acting oil stain prevention effect.
The present invention and the embodiments thereof have been described above, but the description is not limited to the embodiments, but only one of the embodiments of the present invention, and the actual embodiments are not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of a novel three-dimensional solar photo-thermal oil-water separator is characterized by comprising the following steps: comprises the following preparation steps of the following steps of,
(1) cutting the foam Cu into rectangles, and respectively cleaning the rectangles with hydrochloric acid, absolute ethyl alcohol, acetone and deionized water for later use;
(2) preparing a mixed aqueous solution of sodium hydroxide and ammonium persulfate, soaking the cleaned foam Cu in the mixed aqueous solution for a period of time, taking out the foam Cu, and cleaning the foam Cu with deionized water to obtain Cu (OH) with a hierarchical structure
2Foamed Cu;
(3) soaking the foamy copper obtained in the step (2) in sodium sulfide for a period of time, and taking out to obtain Cu with a hierarchical structure
xS/foam Cu;
(4) bending the foamy copper obtained in the step (3) into an inverted U shape to obtain a high-efficiency oil-stain-resistant three-dimensional hierarchical structure evaporation film;
(5) subjecting the inverted U-shaped Cu obtained in the step (4)
xS/foam Cu vertically penetrates through the supportable substrate to obtain the Cu with the three-dimensional hierarchical structure
xS composite photo-thermal film, namely a solar photo-thermal oil-water separator with a three-dimensional structure.
2. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 1, characterized by comprising the following steps: in the step (1), the pore diameter of the foam Cu is 100PPI, the concentration of hydrochloric acid is 1mol/L, and the absolute ethyl alcohol and the acetone are both 200 mL.
3. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 1, characterized by comprising the following steps: in the step (2), the concentration ratio of the sodium hydroxide to the ammonium persulfate is 20:1, the total volume of the mixed solution is 250mL, and the soaking time of the foam Cu is 1 hour.
4. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 1, characterized by comprising the following steps: the concentration of sodium sulfide in the step (3) is 1mM-9mM, and the soaking time is 4 hours, wherein the change of the concentration of sodium sulfide is used for adjusting the chemical composition.
5. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 1, characterized by comprising the following steps: and (4) regulating and controlling the water delivery depth and the evaporation area by controlling the lengths of two ends and the width of the top surface of the inverted U-shaped structure.
6. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 1, characterized by comprising the following steps: and (5) erecting the inverted U-shaped evaporation film by the support substrate in the step (5), preventing the evaporation film from being completely immersed in the solution, forming a three-dimensional evaporation structure, and adjusting the immersion depth and the upper end evaporation area of the evaporation film by the support substrate so as to control the water delivery rate and the evaporation rate.
7. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 1, characterized by comprising the following steps: the material of the support substrate in the step (5) is foam or flat plate which has stable structure, can be perforated and has floating property or physical support property.
8. The preparation method of the novel three-dimensional solar photo-thermal oil-water separator according to claim 7, characterized in that: the support substrate is made of polystyrene foam or aluminum plate.
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| CN111573780A (en) * | 2020-04-09 | 2020-08-25 | 中国科学院宁波材料技术与工程研究所 | Photothermal membrane distiller, preparation method and application thereof, and water treatment equipment |
| CN112968657A (en) * | 2021-02-05 | 2021-06-15 | 浙江工商大学 | Photo-thermal coupling system and application |
| CN113860410A (en) * | 2021-09-30 | 2021-12-31 | 海南大学 | Full-angle solar efficient driving water evaporation bionic material and preparation method thereof |
| CN114014393A (en) * | 2021-10-15 | 2022-02-08 | 宁波大学科学技术学院 | High-efficient light and heat distiller |
| CN115159607A (en) * | 2022-06-16 | 2022-10-11 | 湖北美辰环保股份有限公司 | Solar evaporation and salt crystal collection device with separated illuminated surface and evaporation surface |
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