CN115746383A - Composite membrane material, preparation method thereof and solar evaporator - Google Patents
Composite membrane material, preparation method thereof and solar evaporator Download PDFInfo
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- CN115746383A CN115746383A CN202211330248.5A CN202211330248A CN115746383A CN 115746383 A CN115746383 A CN 115746383A CN 202211330248 A CN202211330248 A CN 202211330248A CN 115746383 A CN115746383 A CN 115746383A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/138—Water desalination using renewable energy
- Y02A20/142—Solar thermal; Photovoltaics
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The application provides a composite film material, a preparation method thereof and a solar evaporator, wherein the composite film material comprises a water transport layer and a light absorption layer from bottom to top, the light absorption layer is attached to one surface of the water transport layer, the water transport layer is provided with a first pore structure, the light absorption layer is provided with a second pore structure, the first pore structure is communicated with the second pore structure, and the pore diameter of the first pore structure is larger than that of the second pore structure. The first pore structure of the water transport layer and the second pore structure of the light absorption layer form a multi-level pore structure with reduced gradient, so that the capillary action is strong, and the water transport capacity of the composite membrane material is improved; the second pore structure of the light absorption layer is used as a water channel, so that the contact area between seawater and the light absorption layer can be increased, the heat exchange effect is enhanced, and the energy utilization rate of photothermal conversion is improved; the second pore structure of the light absorption layer can also be used as a salt ion exchange channel in seawater, so that high-concentration salt after water evaporation can be quickly diluted in the pore channel of the second pore structure, and the salt crystallization problem of an evaporation interface is relieved.
Description
Technical Field
The application belongs to the technical field of composite membrane materials, and particularly relates to a composite membrane material, a preparation method thereof and a solar evaporator.
Background
Fresh water resources are one of the indispensable conditions for human survival. Although the water coverage area on earth is as high as 70%, the fresh water resource which can be really utilized by us only occupies 2.53% of the total water quantity. Moreover, with the discharge of industrial wastewater and domestic sewage, the problem of fresh water pollution makes water wasteland increasingly serious. To solve the water shortage, the simplest method is to convert the seawater with rich reserves into fresh water, except for protecting the existing fresh water resource from being polluted. The traditional seawater desalination technology is generally high in cost and energy consumption and is difficult to realize in some areas with energy shortage. Therefore, a green, efficient and sustainable desalination technology is needed to alleviate the above-mentioned crisis.
The solar seawater desalination technology utilizes solar energy to distill seawater to remove salt to obtain fresh water, has no additional energy consumption and environmental pollution, and becomes an important way for solving the problem of waster water. The core of solar seawater desalination is the structural design of a solar evaporator based on the idea of 'interface heating', however, the currently designed solar evaporator has a low water evaporation rate and a short service life. Therefore, how to develop a solar evaporator with high water yield and long service life is always the focus and focus of research on the premise of ensuring high-efficiency utilization of solar energy.
The light absorber is the most key component in the solar evaporator, and fundamentally determines the seawater desalination performance of the device. MoS 2 As a typical semiconductor material, the MoS sheet has high light absorption rate and light-heat conversion efficiency in the solar spectrum range due to adjustable band gap (the forbidden band width of the MoS sheet changes from an indirect band gap of 1.3eV to a direct band gap of 1.9eV along with reduction of the number of layers), and in addition, the MoS sheet is formed by 2D sheets 2 The constructed 3D stereo structure is largeIncrease the light absorption area, therefore, moS 2 Has great advantages as a light absorber.
Up to now, researchers have succeeded in constructing MoS 2 /SWNT，MoS 2 Chitosan polymers, moS 2 /GO，MoS 2 MoS such as polyurethane 2 Based on solar evaporators, however, these MoS' s 2 The base solar evaporator still faces the problems of low energy utilization of the photothermal conversion and serious salt deposition.
Disclosure of Invention
Based on this, it is an object of the present application to provide a composite film material to solve the existing MoS in the prior art 2 The base solar evaporators still face the technical problems of low energy utilization of photothermal conversion and serious salt deposition.
Still another object of the present application is to provide a method for preparing the above composite film material.
It is a further object of the present application to provide a solar evaporator.
In order to achieve the purpose, the technical scheme adopted by the application is as follows:
the utility model provides a composite membrane material for desalination handles sea water, and composite membrane material is supreme by lower including water transportation layer and light-absorption layer, and the light-absorption layer is attached to the one side on water transportation layer, and water transportation layer has first pore structure, and the light-absorption layer has second pore structure, and first pore structure and second pore structure communicate each other, and the aperture of first pore structure is greater than the aperture of second pore structure.
Optionally, the first pore structure penetrates through the water transport layer, and the pore diameter of the first pore structure is 90 μm-105 μm; and/or the presence of a gas in the gas,
the pore diameter of the second pore structure is 400nm-550nm.
Optionally, the light absorbing layer includes a hydrophilic carbon layer attached to one side of the water transport layer, the hydrophilic carbon layer being formed by stacking sheet-shaped hydrophilic carbon materials, the second pore structure being formed in the hydrophilic carbon layer, the hydrophilic carbon layer further having mesopores, the pore diameter of the mesopores being smaller than the pore diameter of the second pore structure; and/or the presence of a gas in the gas,
the water transport layer has a porosity of 30% to 50%.
Optionally, the pore size of the mesopores is 5-13nm; and/or the presence of a gas in the gas,
the second pore structure penetrates through the hydrophilic carbon layer, and the porosity of the hydrophilic carbon layer is 40% -60%.
Optionally, the light absorbing layer includes a hydrophobic layer, the hydrophobic layer is attached to a surface of the hydrophilic carbon layer away from the water transport layer, the hydrophobic layer has an evaporation channel, and two ends of the second pore structure are respectively communicated with the first pore structure and the evaporation channel; and/or;
the hydrophobic layer contains molybdenum disulfide, the evaporation channel runs through the hydrophobic layer, and the porosity of the hydrophobic layer is 40% -60%.
Optionally, the water transport layer has a thickness of 0.5cm to 1cm; and/or the presence of a gas in the gas,
the hydrophilic carbon layer has a thickness of 80 μm to 100 μm, and the hydrophobic layer has a thickness of 80 μm to 100 μm.
And the preparation method of the composite membrane material comprises the following steps:
curing the semi-solidified polymer hydrogel to obtain a cured polymer hydrogel;
coating a light absorption material containing a flaky nano raw material on one surface of the solidified polymer hydrogel to form a light absorption material layer, so as to obtain an initial product;
performing liquid nitrogen freezing treatment on the primary product to enable water in the polymer hydrogel to form ice crystals, controlling the size of the ice crystals for forming the first pore structure by adjusting freezing time, and performing freeze drying treatment to sublimate the ice crystals in the polymer hydrogel to form the water transport layer with the first pore structure; and (3) stacking the flaky nano raw materials in the light absorption material layer by adjusting the freeze drying treatment time to form a light absorption layer with a second pore structure, so as to obtain the composite film material.
Alternatively, the method of preparing a semi-solidified polymer hydrogel comprises the steps of:
mixing PVA and glutaraldehyde, and then dropwise adding a dilute hydrochloric acid solution to perform a crosslinking reaction to form semi-solidified polymer hydrogel; the mass ratio of the PVA to the hydrogen chloride in the glutaraldehyde and hydrochloric acid diluted solution is (10-12): (0.5-1.0): (0.4-0.5); and/or the presence of a gas in the gas,
the freezing time of the liquid nitrogen freezing treatment is 1-5min; the freeze drying treatment time is 24-48 hours.
Alternatively, the light absorbing layer includes a hydrophilic carbon layer formed by stacking sheet-shaped hydrophilic carbon materials, and the method for preparing the sheet-shaped hydrophilic carbon materials includes the steps of:
mixing deionized water, absolute ethyl alcohol and a graphene oxide material in a stirring state at the stirring speed of 300-700rpm to obtain a mixture A;
keeping stirring state, and sequentially adding a surfactant, mesitylene and dopamine hydrochloride into the mixture A to obtain a mixture B;
keeping stirring, adding strong ammonia water into the mixture B, and stirring for 2-5 hours to gradually change the solution from colorless to brown and finally to black to obtain a mixture C, wherein the mixture C contains black solids;
adding absolute ethyl alcohol into the mixture C for dilution, and then carrying out solid-liquid separation treatment to obtain a black intermediate product;
freeze-drying the intermediate product to obtain an initial product;
carbonizing the primary product at 800-900 ℃ in a nitrogen atmosphere to obtain a flaky hydrophilic carbon material; and/or the presence of a gas in the gas,
the light absorbing layer comprises a hydrophilic carbon layer and a hydrophobic layer, and the method for forming the light absorbing material layer by coating the light absorbing material on one surface of the cured polymer hydrogel comprises the following steps:
coating a hydrophilic carbon material on one surface of the solidified polymer hydrogel to form a hydrophilic carbon material layer;
and coating the hydrophobic material on the surface of the hydrophilic carbon material layer to form a hydrophobic material layer, so as to obtain an initial product.
And a solar evaporator comprising the above composite film material.
Compared with the prior art, the beneficial effect that this application provided includes:
1. the light absorption layer in the composite film material is used for absorbing sunlight and converting the sunlight into heat so as to evaporate water in seawater; the first pore structure of the water transport layer of the composite membrane material and the second pore structure of the light absorption layer form a multi-level pore structure with reduced gradient, the pore diameter is reduced layer by layer from bottom to top, the capillary action is strong, the water transport capacity of the composite membrane material is favorably improved, and seawater can be rapidly pumped to an evaporation interface; meanwhile, the light absorption layer absorbs solar energy and converts the solar energy into heat energy, seawater is heated in the light absorption layer, and the second pore structure of the light absorption layer is used as a water channel, so that the contact area between the seawater and the light absorption layer can be increased, the heat exchange effect is enhanced, the energy utilization rate of photo-thermal conversion is improved, and the water evaporation rate is increased; the second pore structure of the light absorption layer can also be used as a salt ion exchange channel in seawater, so that high-concentration salt after water evaporation can be quickly diluted in a pore channel of the second pore structure, and the problem of salt crystallization at an evaporation interface is relieved;
2. according to the preparation method of the composite membrane material, water in the polymer hydrogel is frozen and frozen, and then the ice is sublimated to form a larger pore channel; the light absorption material does not contain moisture or contains little moisture, so that the light absorption material cannot be frozen in the freezing treatment process, the material particles are compact, and a second pore structure smaller than the first pore structure can be formed;
3. the application provides a composite film material can be applied to solar evaporator, as solar energy sea water desalination membrane, and light and heat conversion's energy utilization is high, the water evaporation is fast, and is difficult for the salt deposition in composite film material, has improved solar evaporator's economic benefits.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a schematic structural view of a composite membrane material of example 1 of the present application;
FIG. 2 is an electron microscope scanning image of a cross section of the composite film material of example 1 of the present application;
FIG. 3 is an electron microscope scanning image of the surface of the composite film material of example 1 of the present application;
FIG. 4 is an electron microscope scanning image of the hydrophobic layer of the composite film material in example 1 of the present application;
FIG. 5 is a diagram showing the distribution of elements in the composite film material of example 1 of the present application;
FIG. 6 is a schematic diagram of the application of the composite membrane material of example 1 of the present application;
FIG. 7 is an infrared thermography of the composite membrane material and pure water desalination process of seawater according to example 1 of the present application;
FIG. 8 is a temperature-time curve of the composite membrane material in the process of desalinating seawater according to embodiment 1 of the present application;
fig. 9 is a curve of the change in weight of seawater in a container during desalination treatment of seawater by using the composite membrane material in example 1 of the present application.
Description of the drawings reference numbers:
1. a composite membrane material;
10. a water transport layer; 20. a light absorbing layer; 22. a hydrophilic carbon layer; 23. a hydrophobic layer.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application clearer, the present application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
It should be noted that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
The embodiment of the application provides a composite membrane material, composite membrane material is by supreme water transportation layer and the light-absorption layer of including down, and the light-absorption layer is attached to the one side on water transportation layer, and water transportation layer has first pore structure, and the light-absorption layer has second pore structure, and first pore structure and second pore structure communicate each other, and the aperture of first pore structure is greater than the aperture of second pore structure.
The light absorption layer in the composite film material provided by the embodiment of the application is used for absorbing sunlight and converting the sunlight into heat so as to evaporate water in seawater. The first pore structure of the water transport layer of the composite membrane material and the second pore structure of the light absorption layer form a multi-level pore structure with reduced gradient, the pore diameter is reduced layer by layer from bottom to top, the capillary action is strong, the water transport capacity of the composite membrane material is favorably improved, and seawater can be rapidly pumped to an evaporation interface; meanwhile, the light absorption layer absorbs solar energy and converts the solar energy into heat energy, seawater is heated in the light absorption layer, and a second hole structure of the light absorption layer is used as a water channel, so that the contact area between the seawater and the light absorption layer can be increased, the heat exchange effect is enhanced, the energy utilization rate of photo-thermal conversion is improved, and the water evaporation rate is increased; the second pore structure of the light absorption layer can also be used as a salt ion exchange channel in seawater, so that high-concentration salt after water evaporation can be quickly diluted in the pore channel of the second pore structure, and the problem of salt crystallization at an evaporation interface is relieved.
Optionally, the first pore structure penetrates through the water transport layer, the pore diameter of the first pore structure is 90-105 μm, seawater to be treated can be sucked, water can be stored in the first pore structure, concentration difference is formed between the seawater in the first pore structure and the seawater in the second pore structure, high-concentration salt evaporated from the water in the second pore structure can be diluted, and the salt crystallization problem is reduced.
Optionally, the water transport layer has a porosity of 30% to 50% such that the water transport layer has sufficient channels to transport seawater in coordination with the evaporation rate of the light absorbing layer.
Optionally, the water transport layer has a thickness of 0.5cm to 1cm.
Optionally, the pore diameter of the second pore structure is 400nm-550nm, the second pore structure is smaller than the first pore structure, and forms capillary action with the first pore structure, and the seawater is absorbed to the light absorption layer for heating evaporation, the pore diameter range is matched with the first pore structure with the pore diameter of 90 μm-105 μm, the water transmission capacity is better, the water transmission rate and the evaporation rate are balanced, and high-concentration salt can perform salt ion exchange in the first pore structure and the second pore structure, so that salt crystallization is relieved.
Optionally, the light absorbing layer includes a hydrophilic carbon layer attached to one side of the water transport layer, the hydrophilic carbon layer is formed by stacking sheet-shaped hydrophilic carbon materials, the second pore structure is formed on the hydrophilic carbon layer, and the hydrophilic carbon layer further has mesopores having a pore diameter smaller than that of the second pore structure.
It can be understood that, the second pore structure and the mesopores are not distributed layer by layer or distributed up and down, but are mixed and distributed in the hydrophilic carbon layer, the second pore structure is formed by the gaps between the stacked sheet-shaped hydrophilic carbon materials, the mesopores are the pores of the carbon sheet, the second pore structure is communicated with the mesopores, the second pore structure and the mesopores are respectively communicated with the first pore structure, and one end of the second pore structure and one end of the mesopores are respectively communicated with the outside of the light absorption layer, so as to volatilize the evaporated water vapor to the outside. Generally, the pore size of the mesopores is much smaller than the pore size of the second pore structure. The hydrophilic carbon layer can be regarded as the combination of transition layer and evaporation layer, utilizes its hydrophilicity to increase the water transport ability of composite membrane material, makes sea water can deposit in the second pore structure and the mesopore of hydrophilic carbon layer to heat evaporation in second pore structure and mesopore.
When the hydrophilic carbon layer also has mesopores, the first pore structure, the second pore structure and the mesopores form a multilevel pore structure with the reduced gradient of the pore diameter, and the multilevel pore structure is a communicating pore with an open microstructure. Furthermore, the mesopores can also serve as salt ion exchange sites, so that salt ions are rapidly transported into the channels of the larger second pore structure and the first pore structure, and the salt ion concentration is redistributed, which is critical for preventing salt accumulation in the composite membrane material.
According to experiments, the pore diameter of the mesopores is 5-13nm.
Optionally, the porosity of the hydrophilic carbon layer is 40% to 60%, where the porosity is a percentage of a pore volume of the hydrophilic carbon layer including the second pore structure and mesopores together with a total volume of the hydrophilic carbon layer in a natural state, and the porosity can ensure light absorption efficiency and can improve transmission capacity and water storage capacity of the hydrophilic carbon layer and provide sufficient space for salt ion exchange.
Optionally, the thickness of the hydrophilic carbon layer is 80 μm to 100 μm, so that the hydrophilic carbon layer forms a second pore structure with enough length in the vertical direction and the reverse direction to form a capillary tube, and seawater is driven to flow from the water transport layer to the light absorption layer.
Optionally, the light absorbing layer includes a hydrophobic layer, the hydrophobic layer is attached to a surface of the hydrophilic carbon layer away from the water transport layer, the hydrophobic layer has an evaporation channel, and two ends of the second pore structure are respectively communicated with the first pore structure and the evaporation channel. The hydrophobic layer and the hydrophilic carbon layer absorb sunlight at the same time and convert the sunlight into heat energy, seawater in the second pore structure and the mesopores is heated and evaporated, and steam flows out from the evaporation channel to complete seawater desalination. The hydrophobic layer is used as the surface layer of the light absorption layer, and seawater can hardly be transmitted to the hydrophobic layer due to the hydrophobicity of the hydrophobic layer, so that salt ions can be inhibited from crystallizing on the surface of the composite membrane material, and the service life is prolonged.
Optionally, the evaporation channel penetrates through the hydrophobic layer, and the porosity of the hydrophobic layer is 40% -60%, where the porosity is a percentage of the volume of the evaporation channel in the hydrophobic layer to the total volume of the hydrophobic layer in a natural state, so as to increase a specific surface area of water evaporation.
Optionally, the hydrophobic layer comprises molybdenum disulfide (MoS) 2 )，MoS 2 Has higher light absorption rate and light-heat conversion efficiency in the solar spectrum range, moS 2 Has great advantages as a light absorbing material.
Optionally, the thickness of the hydrophobic layer is 80 μm to 100 μm, which can effectively inhibit crystallization of the hydrophobic layer of the salt ions and ensure that water vapor can be evaporated from the evaporation channel.
Optionally, the light absorbing layer has a total porosity of 40% to 60%.
The embodiment of the application also provides a preparation method of the composite membrane material, which comprises the following steps:
s10: and (3) curing the semi-solidified polymer hydrogel to obtain the cured polymer hydrogel.
The polymer hydrogel has wider gaps among molecules, can contain more water, and is easy to form a pore canal with larger pore diameter after subsequent freezing and drying for sublimating water.
In some embodiments, the polymer hydrogel is prepared from a dilute solution of PVA, glutaraldehyde and hydrochloric acid, and the preparation method comprises the following steps:
mixing PVA and glutaraldehyde, and then dropwise adding a dilute hydrochloric acid solution to perform a crosslinking reaction to form a semi-solidified polymer hydrogel.
PVA, glutaraldehyde and hydrochloric acid are crosslinked to form a polymer network structure, and partial water in the raw materials is wrapped in the polymer network structure to form the semi-solidified polymer hydrogel.
In some embodiments, after obtaining the semi-solidified polymer hydrogel, the semi-solidified polymer hydrogel is added into a mold and left to solidify, so as to obtain the polymer hydrogel with a preset shape.
Optionally, the mass ratio of the hydrogen chloride in the PVA, the glutaraldehyde and the hydrochloric acid is (10-12): (0.5-1.0): (0.4-0.5), the polymerization degree of the polymer is controlled by controlling the content of hydrogen chloride in PVA, glutaraldehyde and hydrochloric acid, and the formation state of the polymer hydrogel is regulated.
S20: and coating the light absorption material containing the flaky nano raw materials on one surface of the cured polymer hydrogel to form a light absorption material layer, thereby obtaining an initial product.
In some implementations, the light absorbing layer includes a hydrophilic carbon layer and a hydrophobic layer, and the light absorbing material includes a hydrophilic carbon material and a hydrophobic material in a sheet form, and step S20 includes the steps of:
and S21, coating a hydrophilic carbon material on one surface of the solidified polymer hydrogel to form a hydrophilic carbon material layer.
During the coating process, the hydrophilic carbon material is incorporated into the surface of the polymer hydrogel and is tightly bound to the polymer hydrogel due to the softness of the polymer hydrogel.
S22: and coating the hydrophobic material on the surface of the hydrophilic carbon material layer to form a hydrophobic material layer, so as to obtain an initial product.
Alternatively, the hydrophilic carbon material is a sheet-shaped hydrophilic carbon material, and in one aspect, the preparation method of the sheet-shaped hydrophilic carbon material includes the steps of:
mixing deionized water, absolute ethyl alcohol and a graphene oxide material in a stirring state at the stirring speed of 300-700rpm to obtain a mixture A;
keeping stirring, and sequentially adding a surfactant, mesitylene and dopamine hydrochloride into the mixture A to obtain a mixture B;
keeping stirring, adding strong ammonia water into the mixture B, and stirring for 2-5 hours to gradually change the solution from colorless to brown and finally to black to obtain a mixture C, wherein the mixture C contains black solids;
adding absolute ethyl alcohol into the mixture C for dilution, and then carrying out solid-liquid separation treatment to obtain a black intermediate product;
freeze-drying the intermediate product to obtain an initial product;
and carbonizing the primary product at 800-900 ℃ in a nitrogen atmosphere to obtain the flaky hydrophilic carbon material.
The stirring speed of the steps is 300-700rpm, namely the stirring speed of the multilayer reaction is kept similar or the same. Through multilayer reaction, the stirring speed during the reaction and the reaction time after adding strong ammonia water are controlled to control the sheet size of the obtained hydrophilic carbon material, and the stacking state of the hydrophilic carbon material is further controlled to control the aperture size formed by the second pore structure during subsequent freeze drying.
S30: freezing the initial product to form ice crystals in the water in the polymer hydrogel, controlling the size of the ice crystals for forming a first pore structure by adjusting the freezing time, and then carrying out freeze-drying treatment to sublimate the ice crystals in the polymer hydrogel to form a water transport layer with the first pore structure; and (3) stacking the flaky nano raw materials in the light absorption material layer by adjusting the freeze drying treatment time to form a light absorption layer with a second pore structure, so as to obtain the composite film material.
Optionally, the freezing time of the liquid nitrogen freezing treatment is 1-5min; the freeze-drying treatment time is 24-48 hours, so that a first pore structure with the pore diameter of 90-105 μm can be obtained, and the freeze-drying treatment time is favorable for forming a second pore structure with the pore diameter of 400-550 nm.
The composite membrane material preparation method of this application embodiment freezes the water in through the polymer aquogel and freezes, and then with the ice sublimation, forms great pore, and the light absorbing material is because not containing moisture or moisture is few, can not freeze in the freezing treatment process, and it is inseparable to compare between the material granule, can form the second pore structure that is less than first pore structure, and the composite membrane material preparation method of this application embodiment simple process, and the energy consumption is low, is fit for large-scale production.
When PVA hydrogel is prepared by adopting polymerization reaction of PVA, glutaraldehyde and hydrochloric acid, and the light absorption layer comprises a hydrophilic carbon layer and a hydrophobic layer, when the PVA hydrogel is frozen and frozen, water in the PVA hydrogel, the hydrophilic carbon material layer and the hydrophobic material layer is frozen and then sublimated to respectively form a first pore structure, a second pore structure and a hydrophobic channel, and the size and the porosity of the pore diameter are controlled by the preparation conditions of the PVA hydrogel, the hydrophilic carbon material and the hydrophobic material, such as the proportion of raw material components and reaction conditions.
The composite film material provided by the embodiment of the application can be applied to a solar evaporator and used as a solar seawater desalination film, the energy utilization rate of photo-thermal conversion is high, the water evaporation speed is high, salt is not easy to form in the composite film material, and the economic benefit of the solar evaporator is improved.
The following is illustrated by way of example.
Example 1
As shown in fig. 1, the composite membrane material 1 of the present embodiment includes a water transport layer 10 and a light absorption layer 20 from bottom to top, the light absorption layer 20 includes a hydrophilic carbon layer 22 and a hydrophobic layer 23, two sides of the hydrophilic carbon layer 22 are respectively connected to the water transport layer 10 and the hydrophobic layer 23, the water transport layer 10 is made of a PVA hydrogel material, the hydrophilic carbon layer 22 is made of a mesoporous carbon material, the hydrophobic layer 23 is made of a molybdenum disulfide nanosheet, the thickness of the water transport layer 10 is 0.8cm, and the thicknesses of the hydrophilic carbon layer 22 and the hydrophobic layer 23 are respectively 100 μm.
(1) The preparation method of the PVA hydrogel comprises the following steps:
dissolving 10g of PVA powder in 90g of deionized water to obtain a PVA aqueous solution with the mass fraction of 10%;
fully stirring and mixing 100mL of 10% PVA aqueous solution and 1mL of glutaraldehyde solution (the mass fraction is 50%) for 30min, and then dropwise adding 10mL of dilute hydrochloric acid solution (1.2 mol/L) to obtain semi-solidified PVA hydrogel;
and (3) continuously stirring for 2min, transferring the semi-solidified PVA hydrogel into a circular mould with the diameter of 60mm and the depth of 20mm, and standing and curing to obtain the PVA hydrogel.
(2) The preparation method of the mesoporous carbon material comprises the following steps:
magnetically stirring and mixing 50mL of deionized water, 50mL of absolute ethyl alcohol and 0.5g of graphene oxide material in a round-bottom flask at the rotating speed of 350rpm to obtain a mixture A;
adding 0.5g of surfactant F127, 2mL of mesitylene and 1g of dopamine hydrochloride into the mixture A in sequence, and continuing stirring for 30min to obtain a mixture B;
adding 1mL of concentrated ammonia water into the mixture B, continuously stirring for 120min, gradually changing the solution from colorless to brown, and finally changing the solution to black to obtain a mixture C;
after the reaction is finished, adding 100mL of absolute ethyl alcohol into the mixture C to dilute the reaction solution, then separating out a black product through high-speed centrifugation (the rotating speed is more than 12000 rpm), and freeze-drying to obtain a freeze-dried sample;
freeze-dried samples were heated at a heating rate of 1 ℃/min under N 2 Keeping 800 ℃ in the atmosphere for carbonization to obtain the flaky mesoporous carbon material.
(3)MoS 2 The preparation method of the nano sheet comprises the following steps:
mixing the block MoS 2 Mixing a conductive agent (Super P) and a polyvinylidene fluoride (PVDF) binder in a weight ratio of 80;
coating the slurry on a copper foil, and drying for 12 hours at 100 ℃ under vacuum to obtain a positive electrode material;
mixing 1.0M LiPF 4 The lithium sheet is used as an electrolyte, the lithium sheet is used as a counter electrode, the glass fiber paper is used as a diaphragm, and a half cell is assembled in a glove box filled with argon;
discharging the half-cell at a current density of 0.1C (1c=167mah/g) to a cut-off voltage of 0.9V;
disassembling the half-cell in a glove box, taking out the positive pole piece, and cleaning for 3 times by using a dimethyl carbonate solvent;
placing the cleaned positive pole piece in a beaker, adding 10mL of deionized water (18.2M omega. Cm), and performing ultrasonic dispersion;
adding 0.05g of iodoacetamide glycol aqueous solution, and continuously performing ultrasonic dispersion for 2min to obtain a mixed solution;
standing the mixed solution for 12h, taking the upper suspension for centrifugal separation at the rotation speed of 4000rpm for 15min, taking the precipitate, washing the precipitate with deionized water for 4-6 times, and increasing the centrifugal rotation speed to 9000rpm to obtain MoS 2 Nanosheets;
mixing MoS 2 And (5) drying the nanosheets in a freeze drying oven for later use.
The preparation method of the composite membrane material 1 of the embodiment comprises the following steps:
s1, after the PVA hydrogel is solidified for 90min, a layer of mesoporous carbon material with the mass of 10mg is uniformly coated on the surface of the PVA hydrogel.
S2, after continuously curing for 30min, uniformly coating a layer of MoS on the surface of the mesoporous carbon material 2 The nanosheet material, 15mg in mass, yielded membrane material a.
S3, continuously solidifying the membrane material A for 30min, and then quickly freezing the membrane material A under the condition of liquid nitrogen for 1min to obtain a membrane material B;
and S4, drying the frozen membrane material B in a freeze drying box for 24 hours to obtain the composite membrane containing the gradient pores.
The composite film material prepared in example 1 was subjected to a microscopic morphology test and an element distribution test, electron microscope scanning images of the cross section and the surface of the composite film material are shown in fig. 2 and 3, respectively, and electron microscope scanning of the hydrophobic layer is shown in fig. 4, which indicates that the pores in the composite film material are continuously distributed and communicated with each other.
FIG. 5 is the distribution diagram of the elements of the composite film material, and it can be seen that Mo and S are uniformly dispersed in the surface layer of the device, N, O and C are uniformly dispersed in the hydrophilic carbon layer and the hydrophobic layer structure, and O is derived from the oxygen-containing functional group in PVA hydrogel.
Fig. 6 is an example of applying the composite membrane material of example 1 to desalination of sea water, where the composite membrane material is placed on the sea water surface, the water transport layer is immersed in the sea water, the hydrophobic layer is exposed on the sea water surface, and the sea water is naturally absorbed by the composite membrane material to perform desalination of sea water.
The process of desalination of sea water by the composite film material of example 1 was observed by using infrared thermal image, as shown in fig. 7, and pure water was used as a control group, and it was found from the infrared thermal image that the surface temperature of the composite film material increased from the initial 27 ℃ to 42 ℃ within 10 minutes by about 50%, while the surface temperature of pure water did not change much, which indicates that the light-absorbing layer in the composite film material of example 1 has high photothermal conversion efficiency.
The temperature-time change of the composite membrane material in the implementation process is shown in fig. 8, the weight-time change of water is shown in fig. 9, it can be seen from fig. 8 that the surface temperature of the composite membrane material does not rise any more after 10min of solar irradiation, the monitoring is continued for 50min, the temperature is not lowered, which indicates that the photothermal conversion continues to occur at the moment, a large amount of water is evaporated, and it can also be seen from the weight change graph of water shown in fig. 9, it can be seen from fig. 9 that the gradient pore composite membrane material has a high water evaporation rate in the seawater desalination process, which can reach 2.1kg/m 2 /h。
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A composite membrane material is used for desalinating seawater, and is characterized in that: the composite membrane material comprises a water transport layer and a light absorption layer from bottom to top, wherein the light absorption layer is attached to one surface of the water transport layer, the water transport layer is provided with a first pore structure, the light absorption layer is provided with a second pore structure, the first pore structure is communicated with the second pore structure, and the pore diameter of the first pore structure is larger than that of the second pore structure.
2. The composite film material of claim 1, wherein: the first pore structure penetrates through the water transport layer, and the pore diameter of the first pore structure is 90-105 μm; and/or the presence of a gas in the gas,
the pore diameter of the second pore structure is 400nm-550nm.
3. A composite film material according to claim 1 or claim 2, wherein: the light absorbing layer comprises a hydrophilic carbon layer attached to one side of the water transport layer, the hydrophilic carbon layer is formed by stacking sheet-shaped hydrophilic carbon materials, the second pore structure is formed in the hydrophilic carbon layer, and the hydrophilic carbon layer further has mesopores, the pore diameter of the mesopores is smaller than that of the second pore structure; and/or the presence of a gas in the atmosphere,
the porosity of the water transport layer is 30% -50%.
4. The composite film material of claim 3, wherein: the aperture of the mesopores is 5-13nm; and/or the presence of a gas in the gas,
the second pore structure penetrates through the hydrophilic carbon layer, and the porosity of the hydrophilic carbon layer is 40% -60%.
5. The composite film material of claim 3, wherein: the light absorption layer comprises a hydrophobic layer, the hydrophobic layer is attached to one surface, far away from the water transport layer, of the hydrophilic carbon layer, the hydrophobic layer is provided with an evaporation channel, and two ends of the second pore structure are respectively communicated with the first pore structure and the evaporation channel; and/or;
the hydrophobic layer contains molybdenum disulfide, the evaporation channel penetrates through the hydrophobic layer, and the porosity of the hydrophobic layer is 40% -60%.
6. The composite film material of claim 5, wherein: the thickness of the water transport layer is 0.5cm-1cm; and/or the presence of a gas in the gas,
the thickness of the hydrophilic carbon layer is 80-100 μm, and the thickness of the hydrophobic layer is 80-100 μm.
7. A preparation method of a composite film material is characterized by comprising the following steps: for the preparation of the composite film material of any of claims 1 to 6, the preparation method comprising the steps of:
curing the semi-solidified polymer hydrogel to obtain a cured polymer hydrogel;
coating a light absorption material containing a flaky nano raw material on one surface of the solidified polymer hydrogel to form a light absorption material layer, so as to obtain an initial product;
performing liquid nitrogen freezing treatment on the primary product to enable water in the polymer hydrogel to form ice crystals, controlling the size of the ice crystals for forming the first pore structure by adjusting freezing time, and performing freeze drying treatment to sublimate the ice crystals in the polymer hydrogel to form the water transport layer with the first pore structure; and stacking the flaky nano raw materials in the light absorption material layer by adjusting the freeze drying treatment time to form the light absorption layer with the second pore structure, thereby obtaining the composite film material.
8. The method for preparing a composite film material according to claim 7, wherein: the preparation method of the semi-solidified polymer hydrogel comprises the following steps:
mixing PVA and glutaraldehyde, and then dropwise adding a dilute hydrochloric acid solution to perform a crosslinking reaction to form the semi-solidified polymer hydrogel; the mass ratio of the PVA to the glutaraldehyde to the hydrogen chloride in the dilute hydrochloric acid solution is (10-12): (0.5-1.0): (0.4-0.5); and/or the presence of a gas in the gas,
the freezing time of the liquid nitrogen freezing treatment is 1-5min; the freeze drying treatment time is 24-48 hours.
9. The method for preparing a composite film material according to claim 7, wherein: the light absorbing layer includes a hydrophilic carbon layer formed by stacking sheet-shaped hydrophilic carbon materials, and the method for preparing the sheet-shaped hydrophilic carbon materials includes the steps of:
mixing deionized water, absolute ethyl alcohol and a graphene oxide material in a stirring state at the stirring speed of 300-700rpm to obtain a mixture A;
keeping stirring state, and sequentially adding a surfactant, mesitylene and dopamine hydrochloride into the mixture A to obtain a mixture B;
keeping stirring, adding strong ammonia water into the mixture B, and stirring for 2-5 hours to gradually change the solution from colorless to brown and finally to black to obtain a mixture C, wherein the mixture C contains black solids;
adding absolute ethyl alcohol into the mixture C for dilution, and then carrying out solid-liquid separation treatment to obtain a black intermediate product;
freeze-drying the intermediate product to obtain an initial product;
carbonizing the primary product at 800-900 ℃ in a nitrogen atmosphere to obtain a flaky hydrophilic carbon material; and/or the presence of a gas in the gas,
the light absorbing layer comprises a hydrophilic carbon layer and a hydrophobic layer, and a light absorbing material is coated on one surface of the solidified polymer hydrogel to form the light absorbing material layer, wherein the method comprises the following steps:
coating a hydrophilic carbon material on one surface of the solidified polymer hydrogel to form a hydrophilic carbon material layer;
and coating a hydrophobic material on the surface of the hydrophilic carbon material layer to form a hydrophobic material layer, thus obtaining the initial product.
10. A solar evaporator, characterized by: comprising the composite film material of any one of claims 1 to 6.
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| US20220220008A1 (en) * | 2021-01-11 | 2022-07-14 | City University Of Hong Kong | A composite material and a water purifying system |
| CN114870412A (en) * | 2022-04-02 | 2022-08-09 | 深圳大学 | Solar evaporator and preparation method and application thereof |
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| CN114870412A (en) * | 2022-04-02 | 2022-08-09 | 深圳大学 | Solar evaporator and preparation method and application thereof |
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