CN115746383B - Composite film material, preparation method thereof and solar evaporator - Google Patents
Composite film material, preparation method thereof and solar evaporator Download PDFInfo
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- CN115746383B CN115746383B CN202211330248.5A CN202211330248A CN115746383B CN 115746383 B CN115746383 B CN 115746383B CN 202211330248 A CN202211330248 A CN 202211330248A CN 115746383 B CN115746383 B CN 115746383B
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Classifications
-
- 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 membrane material and a preparation method thereof and a solar evaporator, wherein the composite membrane material comprises a water transportation layer and a light absorption layer from bottom to top, the light absorption layer is attached to one surface of the water transportation layer, the water transportation layer is provided with a first hole structure, the light absorption layer is provided with a second hole structure, the first hole structure and the second hole structure are mutually communicated, and the aperture of the first hole structure is larger than that of the second hole structure. The first pore structure of the water transport layer and the second pore structure of the light absorption layer form a gradient-reduced multi-level pore structure, so that the water transport layer has strong capillary action and is beneficial to improving the water transport capacity of the composite membrane material; the second hole structure of the light absorption layer is used as a water channel, so that the contact area of the seawater and the light absorption layer can be increased, the heat exchange effect is enhanced, and the energy utilization rate of photo-thermal 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 rapidly diluted in pore channels 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 the earth is up to 70%, the fresh water resource which can be really utilized by us only accounts for 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 waste increasingly serious. In order to solve the water waste, besides protecting the current fresh water resources from being polluted, the simplest method is to convert the seawater with rich reserves into fresh water. The traditional sea water desalination technology is high in cost and high in energy consumption, and is difficult to realize in some areas with energy shortage. Thus, there is a need for a green, efficient, sustainable desalination technique that alleviates the above-mentioned crisis.
The solar sea water desalting technology uses solar distilled sea water to remove salt to obtain fresh water, has no additional energy consumption and environmental pollution, and becomes an important way for knowing the problem of water waste. The core of solar sea water desalination is the structural design of a solar evaporator based on the idea of 'interfacial heating', however, the solar evaporator designed at present has lower water evaporation rate and generally shorter service life. Therefore, on the premise of ensuring efficient utilization of solar energy, development of a solar evaporator with high water yield and long service life is always an important point and a hot spot of research.
The absorber is used as the most critical component in the solar evaporator, and the seawater desalination performance of the device is fundamentally determined. MoS (MoS) 2 As a typical semiconductor material, the band gap is adjustable (the band gap width is changed from an indirect band gap of 1.3eV to a direct band gap of 1.9eV along with the reduction of the layer number), the semiconductor material has higher light absorptivity and light-heat conversion efficiency in the solar spectrum range, and in addition, the semiconductor material is formed by 2D sheet MoS 2 The 3D structure greatly increases the light absorption area, so MoS 2 Has great advantages as a light absorber.
Up to now, researchers have successfully constructed MoS 2 /SWNT，MoS 2 Chitosan polymer, moS 2 /GO，MoS 2 MoS such as polyurethane 2 Basic solar evaporators, however, these MoS 2 The base solar energy evaporator still faces the problems of low energy utilization rate of photo-thermal conversion and serious salt formation.
Disclosure of Invention
Based on this, it is an object of the present application to provide a composite membrane material to solve the MoS existing in the prior art 2 The base solar evaporator still faces the technical problems of low energy utilization rate of photo-thermal conversion and serious salt formation.
It is a further object of the present application to provide a method for preparing the above composite membrane material.
It is a further object of the present application to provide a solar evaporator.
In order to achieve the above purpose, the technical scheme adopted in the application is as follows:
a composite membrane material is used for desalting sea water, the composite membrane material comprises a water transportation layer and a light absorption layer from bottom to top, the light absorption layer is attached to one surface of the water transportation layer, the water transportation 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.
Optionally, 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 number of the groups of groups,
the pore diameter of the second pore structure is 400nm-550nm.
Optionally, the light absorbing layer includes a hydrophilic carbon layer, the hydrophilic carbon layer is attached to one surface 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, the hydrophilic carbon layer also has mesopores, and the pore diameter of the mesopores is smaller than that of the second pore structure; and/or the number of the groups of groups,
the porosity of the water transport layer is 30% -50%.
Optionally, the pore diameter of the mesoporous is 5-13nm; and/or the number of the groups of groups,
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 comprises a hydrophobic layer, the hydrophobic layer is attached to one surface of the hydrophilic carbon layer far away from the water transport 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%.
Optionally, the thickness of the water transport layer is 0.5cm to 1cm; and/or the number of the groups of groups,
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:
solidifying the semi-solidified polymer hydrogel to obtain solidified polymer hydrogel;
coating a light-absorbing material containing a flaky nano raw material on one surface of the cured polymer hydrogel to form a light-absorbing material layer, so as to obtain a primary product;
performing liquid nitrogen freezing treatment on the initial product to enable water in the polymer hydrogel to form ice crystals, controlling the size of the ice crystals for forming a first pore structure by adjusting the 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) by adjusting the freeze drying treatment time, stacking the flaky nano raw materials in the light absorbing material layer by layer to form the light absorbing layer with a second pore structure, thereby obtaining the composite film material.
Optionally, the method for preparing the semi-solid polymer hydrogel comprises the following steps:
mixing PVA and glutaraldehyde, then dropwise adding dilute hydrochloric acid solution, and performing a crosslinking reaction to form semi-solid polymer hydrogel; the mass ratio of the PVA to 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 number of the groups of groups,
the freezing time of the liquid nitrogen freezing treatment is 1-5min; the freeze drying treatment time is 24-48 hours.
Optionally, the light absorbing layer includes a hydrophilic carbon layer formed by stacking a sheet-shaped hydrophilic carbon material, and the preparation method of the sheet-shaped hydrophilic carbon material includes the following steps:
mixing deionized water, absolute ethyl alcohol and graphene oxide materials in a stirring state, wherein the stirring speed is 300-700rpm, so as to obtain a mixture A;
sequentially adding a surfactant, mesitylene and dopamine hydrochloride into the mixture A while maintaining a stirring state to obtain a mixture B;
adding concentrated ammonia water into the mixture B under stirring for 2-5 hours, gradually changing the solution from colorless to brown and finally to black to obtain a mixture C containing 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 a primary product;
carbonizing the initial product in nitrogen atmosphere at 800-900 ℃ to obtain a flaky hydrophilic carbon material; and/or the number of the groups of groups,
the light absorbing layer comprises a hydrophilic carbon layer and a hydrophobic layer, the light absorbing material is coated on one surface of the solidified polymer hydrogel, and the method for forming the light absorbing material layer comprises the following steps:
coating a hydrophilic carbon material on one surface of the cured 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, thereby obtaining a primary product.
And a solar evaporator comprising the 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, converting the sunlight into heat and evaporating water in the seawater; the first pore structure of the water transport layer and the second pore structure of the light absorption layer of the composite membrane material form a gradient-reduced multi-level pore structure, the pore diameters are reduced layer by layer from bottom to top, the capillary action is strong, the water transport capacity of the composite membrane material is 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, the second hole structure of the light absorption layer is used as a water channel, so that the contact area of 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 rapidly diluted in pore channels of the second pore structure, and the salt crystallization problem of 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 ice is sublimated to form a larger pore canal; the light absorbing material does not contain water or has little water, can not freeze in the freezing treatment process, has compact material particles, can form a second pore structure smaller than the first pore structure, and the preparation method of the composite membrane material has simple process and low energy consumption, and is suitable for large-scale production;
3. the composite film material can be applied to a solar evaporator, is used as a solar sea water desalination film, has high energy utilization rate of photo-thermal conversion and high water evaporation speed, is not easy to form salt in the composite film material, and improves the economic benefit of the solar evaporator.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a schematic structural diagram of a composite membrane material according to example 1 of the present application;
FIG. 2 is an electron microscope scan of a cross section of a composite film material according to example 1 of the present application;
FIG. 3 is an electron microscope scan of the surface of the composite film material of example 1 of the present application;
FIG. 4 is an electron microscope scan of the hydrophobic layer of the composite film material of example 1 of the present application;
FIG. 5 is an elemental distribution diagram of a composite membrane material of example 1 of the present application;
FIG. 6 is a schematic illustration of the application of the composite membrane material of example 1 of the present application;
FIG. 7 is an infrared thermogram of the seawater desalination process using the composite membrane material and pure water of example 1 of the present application;
FIG. 8 is a graph showing the temperature-time variation of the desalination process of seawater by using the composite membrane material of example 1 of the present application;
fig. 9 is a graph showing the weight change of seawater in a container during desalination of seawater by using the composite membrane material of example 1 of the present application.
The reference numerals:
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 schemes and beneficial effects to be solved by the present application more clear, 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 for purposes of illustration only and are not intended to limit the present application.
It should be noted that the terms "first," "second," and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implying a number of technical features being indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The embodiment of the application provides a composite membrane material, and composite membrane material is by supreme water transport layer and the light-absorbing layer of including down, and the light-absorbing layer is attached to the one side on water transport layer, and water transport layer has first pore structure, and the light-absorbing layer has second pore structure, and first pore structure communicates with each other with the second pore structure, 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 and the second pore structure of the light absorption layer of the composite membrane material form a gradient-reduced multi-level pore structure, the pore diameters are reduced layer by layer from bottom to top, the capillary action is strong, the water transport capacity of the composite membrane material is 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, the second hole structure of the light absorption layer is used as a water channel, so that the contact area of 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 rapidly diluted in pore channels of the second pore structure, and the salt crystallization problem of an evaporation interface is relieved.
Optionally, the first pore structure penetrates through the water transport layer, the aperture 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 after water evaporation in the second pore structure is diluted, and 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 combination with the evaporation rate of the light absorbing layer.
Alternatively, the thickness of the water transport layer is 0.5cm to 1cm.
Optionally, the aperture 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, the seawater is absorbed to the light absorption layer for heating and evaporating, the aperture range is matched with the first pore structure with the aperture of 90-105 μm, the water transmission capacity is better, the water transmission rate and the evaporation rate are balanced, and the 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, the hydrophilic carbon layer is 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, the hydrophilic carbon layer further has mesopores, and the pore diameter of the mesopores is 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 up and down, but are mixed and distributed in the hydrophilic carbon layer, the second pore structure is formed by gaps between the sheet-shaped hydrophilic carbon material stacks, the mesopores are pores of the carbon sheet, the second pore structure and the mesopores are mutually communicated, the second pore structure and the mesopores are respectively mutually communicated with the first pore structure, and one ends of the second pore structure and the mesopores are respectively communicated with the outside of the light absorption layer so as to volatilize the evaporated water vapor to the outside. In general, the pore size of the mesopores is much smaller than that of the second pore structure. The hydrophilic carbon layer can be regarded as the combination of the transition layer and the evaporation layer, and the hydrophilicity of the hydrophilic carbon layer is utilized to increase the water transmission capacity of the composite membrane material, so that seawater can be stored in the second pore structure and the mesopores of the hydrophilic carbon layer, and the seawater is heated and evaporated in the second pore structure and the mesopores.
When the hydrophilic carbon layer is also provided with mesopores, the first pore structure, the second pore structure and the mesopores form a multistage pore structure with reduced pore diameter gradient, and the multistage pore structure is a communication hole with an open microstructure. In addition, 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 the key to prevent salt accumulation in the composite membrane material.
According to experiments, the pore diameter of the mesoporous is 5-13nm.
Optionally, the porosity of the hydrophilic carbon layer is 40% -60%, where the porosity refers to the percentage of the total volume of the hydrophilic carbon layer and the pore volume of the hydrophilic carbon layer including the second pore structure and the mesopores, so that the light absorption efficiency can be ensured, and meanwhile, the transmission capacity and the water storage capacity of the hydrophilic carbon layer can be improved, and enough space is provided for salt ion exchange.
Alternatively, the hydrophilic carbon layer has a thickness of 80 μm to 100 μm, so that the hydrophilic carbon layer forms a second pore structure of a sufficient length in a vertical direction to form capillaries for driving seawater to flow from the water transport layer to the light absorbing 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 and convert the sunlight into heat energy, the second pore structure and the sea water in the mesopores are heated and evaporated, and the steam flows out of the evaporation channel to complete the desalination of the sea water. The hydrophobic layer is used as the surface layer of the light absorption layer, and due to the hydrophobicity of the hydrophobic layer, seawater can hardly be transmitted to the 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, the porosity of the hydrophobic layer is 40% -60%, the porosity refers to the percentage of the volume of the evaporation channel in the hydrophobic layer to the total volume of the hydrophobic layer in a natural state, and the specific surface area of water evaporation is improved.
Optionally, the hydrophobic layer comprises molybdenum disulfide (MoS 2 )，MoS 2 Has higher light absorptivity and light-heat conversion efficiency in the solar spectrum range, moS 2 Has great advantages as light absorbing material.
Alternatively, the thickness of the hydrophobic layer is 80 μm to 100 μm, which can effectively inhibit crystallization of the hydrophobic layer of salt ions and ensure that water vapor can be evaporated from the evaporation channel.
Optionally, the total porosity of the light absorbing layer is 40% -60%.
The embodiment of the application also provides a preparation method of the composite membrane material, which comprises the following steps:
s10: and curing the semi-solidified polymer hydrogel to obtain the cured polymer hydrogel.
The gaps among molecules of the polymer hydrogel are wider, can contain more moisture, and can easily form pore channels with larger pore diameters after subsequent freezing and drying of sublimated moisture.
In some embodiments, the polymer hydrogel is made using a dilute solution of PVA, glutaraldehyde and hydrochloric acid, and the method of making the same comprises the steps of:
PVA and glutaraldehyde are mixed, and then hydrochloric acid diluted solution is added dropwise for crosslinking reaction to form semi-solid polymer hydrogel.
PVA, glutaraldehyde and hydrochloric acid are crosslinked to form a polymer network structure, and part of water in the raw materials is wrapped in the polymer network structure to form semi-solid polymer hydrogel.
In some embodiments, after the semi-solid polymer hydrogel is obtained, the semi-solid polymer hydrogel is added into a mold, and is allowed to stand and solidify to obtain the polymer hydrogel with the preset shape.
Optionally, the mass ratio of hydrogen chloride in PVA, glutaraldehyde and 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 further regulated.
S20: and coating the light-absorbing material containing the flaky nano raw materials on one surface of the solidified polymer hydrogel to form a light-absorbing material layer, thus obtaining a primary product.
In some implementations, the light absorbing layer includes a hydrophilic carbon layer and a hydrophobic layer, and then the light absorbing material includes a sheet-shaped hydrophilic carbon material and a hydrophobic material, and step S20 includes the steps of:
and S21, coating a hydrophilic carbon material on one surface of the cured polymer hydrogel to form a hydrophilic carbon material layer.
In the coating process, the hydrophilic carbon material is doped on the surface of the polymer hydrogel and is tightly combined with the polymer hydrogel due to the fact that the polymer hydrogel is softer.
S22: and coating a hydrophobic material on the surface of the hydrophilic carbon material layer to form a hydrophobic material layer, thereby obtaining a primary product.
Alternatively, the hydrophilic carbon material is a sheet-like hydrophilic carbon material, and in one embodiment, the method of preparing the sheet-like hydrophilic carbon material includes the steps of:
mixing deionized water, absolute ethyl alcohol and graphene oxide materials in a stirring state, wherein the stirring speed is 300-700rpm, so as to obtain a mixture A;
sequentially adding a surfactant, mesitylene and dopamine hydrochloride into the mixture A while maintaining a stirring state to obtain a mixture B;
adding concentrated ammonia water into the mixture B under stirring for 2-5 hours, gradually changing the solution from colorless to brown and finally to black to obtain a mixture C containing 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 a primary product;
carbonizing the initial product in nitrogen atmosphere at 800-900 deg.c to obtain sheet hydrophilic carbon material.
The stirring speed of the steps is 300-700rpm, namely the stirring speed of the multi-layer reaction is kept similar or the same. Through the multi-layer reaction, the stirring speed during the reaction and the reaction time after adding the strong ammonia water are controlled to control the sheet-shaped size of the obtained hydrophilic carbon material, and the stacking state of the hydrophilic carbon material is further controlled to control the pore size formed by the second pore structure during the 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 performing 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) by adjusting the freeze drying treatment time, stacking the flaky nano raw materials in the light absorbing material layer by layer to form the light absorbing layer with a second pore structure, thereby obtaining 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, and the first pore structure with the pore diameter of 90-105 μm can be obtained, and the freeze drying treatment time is favorable for forming the second pore structure with the pore diameter of 400-550 nm.
According to the preparation method of the composite membrane material, moisture in the polymer hydrogel is frozen and frozen, ice is sublimated to form a larger pore canal, the light absorbing material does not contain moisture or has little moisture, the light absorbing material cannot freeze in the freezing treatment process, the material particles are compact, a second pore structure smaller than the first pore structure can be formed, and the preparation method of the composite membrane material is simple in process, low in energy consumption and suitable for large-scale production.
When PVA, glutaraldehyde and hydrochloric acid are adopted for polymerization reaction to prepare PVA hydrogel, when the light absorption layer comprises a hydrophilic carbon layer and a hydrophobic layer, water in the PVA hydrogel, the hydrophilic carbon material layer and the hydrophobic material layer is frozen and frozen, and then sublimated to form a first pore structure, a second pore structure and a hydrophobic channel respectively, and pore size and porosity are controlled through preparation conditions of the PVA hydrogel, the hydrophilic carbon material and the hydrophobic material, such as 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, is used as a solar sea water desalination film, has high energy utilization rate of photo-thermal conversion and high water evaporation speed, is not easy to form salt in the composite film material, and improves the economic benefit of the solar evaporator.
The following is illustrated by examples.
Example 1
As shown in fig. 1, the composite membrane material 1 of the present embodiment includes a water transporting layer 10 and a light absorbing layer 20 from bottom to top, the light absorbing layer 20 includes a hydrophilic carbon layer 22 and a hydrophobic layer 23, both sides of the hydrophilic carbon layer 22 are respectively connected with the water transporting layer 10 and the hydrophobic layer 23, the water transporting layer 10 is made of PVA hydrogel material, the hydrophilic carbon layer 22 is made of mesoporous carbon material, the hydrophobic layer 23 is made of molybdenum disulfide nanosheets, the thickness of the water transporting layer 10 is 0.8cm, and the thicknesses of the hydrophilic carbon layer 22 and the hydrophobic layer 23 are 100 μm, respectively.
(1) PVA hydrogel preparation method:
10g of PVA powder is dissolved in 90g of deionized water to obtain a PVA aqueous solution with the mass fraction of 10%;
100mL of PVA aqueous solution with the mass fraction of 10% and 1mL of glutaraldehyde solution (with the mass fraction of 50%) are fully stirred and mixed for 30min, and then 10mL of hydrochloric acid dilute solution (1.2 mol/L) is added dropwise to obtain semi-solid PVA hydrogel;
after stirring for 2min, the PVA hydrogel in a semi-solidified state is transferred into a round mold with the diameter of 60mm and the depth of 20mm, and is subjected to standing and solidification, so that the PVA hydrogel is obtained.
(2) The preparation method of the mesoporous carbon material comprises the following steps:
50mL of deionized water, 50mL of absolute ethyl alcohol and 0.5g of graphene oxide material are magnetically stirred and mixed in a round-bottomed flask at a rotating speed of 350rpm to obtain a mixture A;
sequentially adding 0.5g of surfactant F127, 2mL of mesitylene and 1g of dopamine hydrochloride into the mixture A, and continuously 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 into black to obtain a mixture C;
after the reaction is finished, 100mL of absolute ethyl alcohol is added into the mixture C to dilute the reaction solution, then a black product is separated out through high-speed centrifugation (the rotating speed is more than 12000 rpm), and freeze-drying is carried out, so that a freeze-dried sample is obtained;
freeze-dried samples were incubated at a rate of 1℃per minute at N 2 Carbonizing at 800 ℃ in the atmosphere to obtain the flaky mesoporous carbon material.
(3)MoS 2 The preparation method of the nano-sheet comprises the following steps:
blocky MoS 2 Mixing a conductive agent (Super P) and a polyvinylidene fluoride (PVDF) binder in a weight ratio of 80:10:10 in N, N-dimethylformamide, and uniformly forming slurry by ultrasonic;
coating the slurry on a copper foil, and drying the copper foil for 12 hours at 100 ℃ in vacuum to obtain a positive electrode material;
1.0M LiPF 4 The method comprises the steps of (1) using a lithium sheet as a counter electrode, glass fiber paper as a diaphragm, and assembling a half cell in a glove box filled with argon;
discharging the half cell to a cut-off voltage of 0.9V at a current density of 0.1C (1c=167 mAh/g);
disassembling the half cell in a glove box, taking out the positive electrode plate, and cleaning for 3 times by using a dimethyl carbonate solvent;
placing the cleaned positive electrode plate into 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, centrifuging the upper suspension at 4000rpm for 15min, collecting precipitate, washing with deionized water for 4-6 times, and centrifuging at 9000rpm to obtain MoS 2 A nanosheet;
MoS is carried out 2 The nano-sheets are placed in a freeze drying box for drying for standby.
The preparation method of the composite membrane material 1 comprises the following steps:
s1, after curing the PVA hydrogel for 90min, uniformly coating a layer of mesoporous carbon material on the surface of the PVA hydrogel, wherein the mass of the PVA hydrogel is 10mg.
S2, after the continuous solidification for 30min, uniformly coating a layer of MoS on the surface of the mesoporous carbon material 2 The mass of the nano sheet material is 15mg, and the film material A is obtained.
S3, continuously solidifying the film material A for 30min, and then rapidly freezing under the condition of liquid nitrogen for 1min to obtain a film material B;
s4, placing the frozen membrane material B in a freeze drying box for drying for 24 hours to obtain the composite membrane containing the gradient holes.
The microscopic morphology test and the element distribution test are carried out on the composite membrane material prepared in the embodiment 1, the section and the surface scanning electron microscope of the composite membrane material are respectively shown in fig. 2 and 3, the scanning electron microscope of the hydrophobic layer is shown in fig. 4, and the pore channels in the composite membrane material are continuously distributed and mutually communicated.
Fig. 5 is an element distribution diagram 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 elements are uniformly dispersed in the hydrophilic carbon layer and the hydrophobic layer structure, and O is derived from an oxygen-containing functional group in the PVA hydrogel.
Fig. 6 shows an example of the application of the composite membrane material of example 1 to desalination of sea water, in which the composite membrane material is placed on the sea water surface, the water transport layer is immersed in sea water, the water drainage layer is exposed to the sea water surface, and sea water is naturally sucked by the composite membrane material, and the sea water desalination treatment is performed.
As shown in fig. 7, pure water was used as a control group when the composite film material of example 1 was observed by infrared thermal imaging, the surface temperature of the composite film material increased from the initial 27 ℃ to 42 ℃ by about 50% within 10 minutes, and the surface temperature of the pure water did not change much, which indicated that the light-absorbing layer in the composite film material of example 1 had a high light-heat conversion efficiency.
The temperature-time change of the composite film material in the implementation process is shown in fig. 8, the weight-time change of water is shown in fig. 9, and as can be seen from fig. 8, the surface temperature of the composite film material is not increased after 10min of sunlight irradiation, the surface temperature is continuously monitored for 50min, the temperature is not reduced, the light-heat conversion continuously occurs, a large amount of water is evaporated, and the weight of water can be also obtainedAs can be demonstrated by the change chart shown in FIG. 9, the gradient pore composite membrane material has higher water evaporation rate in the sea water desalination process, which can reach 2.1kg/m 2 /h。
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (7)
1. A composite membrane material is used for desalinating seawater and is characterized in that: the composite membrane material comprises a water transportation layer and a light absorption layer from bottom to top, wherein the light absorption layer is attached to one surface of the water transportation layer, the water transportation layer is provided with a first pore structure, the light absorption layer is provided with a second pore structure, the first pore structure and the second pore structure are communicated with each other, and the pore diameter of the first pore structure is larger than that of the second pore structure;
the light absorption layer comprises a hydrophilic carbon layer, the hydrophilic carbon layer is attached to one surface of the water transport layer, the hydrophilic carbon layer is prepared by hydrophilic modification of graphene oxide materials, and the hydrophilic carbon layer is formed by stacking flaky hydrophilic carbon materials; the second pore structure is formed in the hydrophilic carbon layer, and the hydrophilic carbon layer is also provided with mesopores, wherein the pore diameter of the mesopores is smaller than that of the second pore structure;
the light absorption layer comprises a hydrophobic layer, the hydrophobic layer is attached to one surface of the hydrophilic carbon layer, which is far away from the water transportation 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;
the hydrophobic layer contains molybdenum disulfide, the evaporation channel penetrates through the hydrophobic layer, and the porosity of the hydrophobic layer is 40% -60%.
2. The composite membrane 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 mu m; and/or the number of the groups of groups,
the aperture of the second pore structure is 400nm-550nm.
3. The composite membrane material of claim 1 or 2, wherein: the porosity of the water transport layer is 30% -50%.
4. A composite membrane material according to claim 3, wherein: the pore diameter of the mesoporous is 5-13nm; and/or the number of the groups of groups,
the second pore structure penetrates through the hydrophilic carbon layer, and the porosity of the hydrophilic carbon layer is 40% -60%.
5. The composite membrane material of claim 1, wherein: the thickness of the water transport layer is 0.5cm-1cm; and/or the number of the groups of groups,
the thickness of the hydrophilic carbon layer is 80-100 μm, and the thickness of the hydrophobic layer is 80-100 μm.
6. A preparation method of a composite membrane material is characterized by comprising the following steps: a process for preparing the composite film material of any one of claims 1 to 5, the preparation process comprising the steps of:
mixing PVA and glutaraldehyde, then dropwise adding dilute hydrochloric acid solution, and performing a crosslinking reaction to form semi-solid polymer hydrogel; the mass ratio of the PVA to glutaraldehyde to the hydrogen chloride in the dilute hydrochloric acid solution is (10-12): (0.5-1.0): (0.4-0.5);
curing the semi-solid polymer hydrogel to obtain cured polymer hydrogel;
coating a light-absorbing material containing a flaky nano raw material on one surface of the cured polymer hydrogel to form a light-absorbing material layer, so as to obtain a primary product;
performing liquid nitrogen freezing treatment on the initial product for 1-5min 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 the freezing time, and performing freeze drying treatment for 24-48 h to sublimate the ice crystals in the polymer hydrogel to form the water transport layer with the first pore structure; the sheet nanometer raw materials in the light absorption material layer are stacked layer by adjusting the freeze drying treatment time, so that the light absorption layer with the second pore structure is formed, and the composite membrane material is obtained;
the light absorbing layer comprises a hydrophilic carbon layer, the hydrophilic carbon layer is formed by stacking sheet-shaped hydrophilic carbon materials, and the preparation method of the sheet-shaped hydrophilic carbon materials comprises the following steps:
mixing deionized water, absolute ethyl alcohol and graphene oxide materials in a stirring state, wherein the stirring speed is 300-700rpm, so as to obtain a mixture A;
sequentially adding a surfactant, mesitylene and dopamine hydrochloride into the mixture A while maintaining a stirring state to obtain a mixture B;
adding concentrated ammonia water into the mixture B under stirring for 2-5 hours, gradually changing 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 a primary product;
carbonizing the initial product in nitrogen atmosphere at 800-900 ℃ to obtain a flaky hydrophilic carbon material; and/or the number of the groups of groups,
the light absorbing layer comprises a hydrophilic carbon layer and a hydrophobic layer, a light absorbing material is coated on one surface of the cured polymer hydrogel, and the method for forming the light absorbing material layer comprises the following steps of:
coating a hydrophilic carbon material on one surface of the cured 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, thereby obtaining the initial product.
7. A solar evaporator, characterized in that: a composite membrane material comprising any one of claims 1 to 5.
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