CN106809897B - Preparation method of graphene photothermal conversion material for seawater desalination and water purification treatment - Google Patents
Preparation method of graphene photothermal conversion material for seawater desalination and water purification treatment Download PDFInfo
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- CN106809897B CN106809897B CN201510853944.8A CN201510853944A CN106809897B CN 106809897 B CN106809897 B CN 106809897B CN 201510853944 A CN201510853944 A CN 201510853944A CN 106809897 B CN106809897 B CN 106809897B
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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
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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
- Y02A20/138—Water desalination using renewable energy
- Y02A20/142—Solar thermal; Photovoltaics
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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
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention relates to the field of water treatment materials, in particular to a preparation method of a graphene photothermal conversion material for seawater desalination and water purification treatment. Preparing graphene powder, a polymer material with a chain-like molecular structure and a solvent into slurry according to a proportion, adding the slurry into a mold, drying and carrying out heat treatment to carbonize organic substances in the material, and obtaining a graphene foam material with good mechanical strength; and carrying out hydrophilization treatment on one side of the bottom surface of the graphene film to prepare the graphene photothermal conversion material for distillation purification and desalination treatment of sewage and seawater. The material utilizes the black body structure and high heat conduction property of graphene foam, and can efficiently convert sunlight into heat; the capillary action of the foam structure is utilized to continuously convey water and reduce the evaporation potential barrier, thereby realizing the rapid distillation and desalination of seawater. The graphene foam material can be used for preparing a portable high-efficiency seawater desalination and sewage purification device, and the requirement of quickly preparing clean fresh water on the sea and outdoors is met.
Description
Technical Field
The invention relates to the field of water treatment materials, in particular to a preparation method of a graphene photothermal conversion material for seawater desalination and water purification treatment.
Background
Fresh water is one of the basic substances on which human society relies to survive and develop. China is lack of water resources and occupies 108 th place in the world. China is long in coastline, and islands, coastal saline-alkali areas and inland bitter regions belong to regions lack of fresh water. People in these areas develop various conditions due to long-term drinking of water that does not meet hygienic standards, directly affecting their physical health and local economic construction. Therefore, the problem of insufficient fresh water supply is a serious problem in China. An advantageous approach to increase the supply of fresh water is to desalinate seawater or brackish water in close proximity, particularly in remote areas where water usage is dispersed. There are many methods for desalinating seawater or brackish water, but conventional methods, such as: distillation, ion exchange, dialysis, reverse osmosis, refrigeration, and the like consume large amounts of fuel and electricity. It is reported that energy consumption for seawater desalination is about 1.3 million tons in terms of crude oil every year around the world, and there are also serious air pollution, greenhouse effect, and other problems. Therefore, it is of great practical significance to seek other cleaner and more sustainable methods for desalination of sea water. Wherein, the seawater desalination is carried out by utilizing solar energy, and the device has wide application prospect.
At present, the adopted solar seawater desalination technology is mainly divided into two types: firstly, utilize solar energy to carry out photovoltaic power generation, then utilize electric energy drive reverse osmosis unit to desalt, because photovoltaic power generation's conversion efficiency itself is just very low, and energy consumption and the life-span problem that reverse osmosis unit itself exists make its development restricted. Secondly, the heat effect of solar energy is utilized, and the seawater is heated by a heat collecting device to be distilled and desalinated; because of low energy utilization rate, the working temperature is usually very low, and the evaporation efficiency is not high; to improve the efficiency, a large-scale heat collecting device needs to be built to heat the seawater, which undoubtedly increases the use and maintenance cost of the technology; the problems of equipment corrosion and pipeline blockage caused by high salinity of seawater also become technical obstacles which are difficult to overcome in the popularization and the use of large-scale equipment. Therefore, the development of the current technology is leading to how to more efficiently utilize solar energy and optimize the structure of the device, thereby reducing the use and maintenance cost and prolonging the service life.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene photothermal conversion material for seawater desalination and water purification treatment, which is used for obtaining a graphene porous foam material with high-efficiency photothermal conversion capacity, floating on the surface of seawater and sewage and placing the graphene porous foam material in the sun for solarization, can quickly convert water into vapor, and then simply condensing the vapor to prepare drinkable pure fresh water.
The technical scheme of the invention is as follows:
a preparation method of a graphene photothermal conversion material for seawater desalination and water purification treatment comprises the steps of preparing graphene powder, a polymer material with a chain-shaped molecular structure and a solvent into slurry, adding the slurry into a mold, drying and carrying out heat treatment to carbonize organic substances in the material, and obtaining a graphene foam material with good mechanical strength; and carrying out hydrophilization treatment on one side of the bottom surface of the graphene film to prepare the graphene photothermal conversion material for distillation purification and desalination treatment of sewage and seawater.
According to the preparation method of the graphene photothermal conversion material for seawater desalination and water purification treatment, the graphene material is eigen-state graphene or graphene derivatives prepared by various methods; the thickness of the lamella of the eigenstate graphene or graphene derivative is that the number of carbon atom layers is less than 10, and the lamella diameter/thickness ratio of the lamella is more than 10.
According to the preparation method of the graphene photothermal conversion material for seawater desalination and water purification treatment, the graphene derivative comprises modified graphene, graphene oxide, a flaky graphene structure grafted or coated with other molecular chain segments, and one of defective or doped graphene.
The preparation method of the graphene photothermal conversion material for seawater desalination and water purification treatment comprises the following steps: graphene powder or liquid phase dispersion prepared by taking graphite as a raw material through expansion stripping, graphene prepared by taking a gaseous carbon source as a raw material through chemical vapor deposition or physical vapor deposition, and graphene powder or liquid phase dispersion formed by crushing or dispersing, or powder or liquid phase dispersion formed by gathering graphene-like two-dimensional sheet materials formed by chemical polymerization of small molecular substances.
The graphene photothermal conversion material for seawater desalination and water purification treatment is prepared by using a polymer with a chain molecular structure, wherein the polymer comprises sucrose, cellulose and a derivative thereof, and one of thermoplastic and thermosetting resin materials, and the used solvent is a good solvent corresponding to the polymer material due to different polymer materials.
According to the preparation method of the graphene photothermal conversion material for seawater desalination and water purification treatment, in slurry prepared from graphene and a polymer material, the proportion range of solid matters is 0.1-50% by weight, wherein the proportion range of graphene and the polymer material is 1000: 1-1: 100 by weight.
According to the preparation method of the graphene photothermal conversion material for seawater desalination and water purification, the shape of a mold for graphene slurry molding is not particularly limited, and the graphene photothermal conversion material can be subjected to heat treatment at 300-1000 ℃ without deformation or damage.
According to the preparation method of the graphene photothermal conversion material for seawater desalination and water purification treatment, the graphene slurry is added into a mold and then is dried and sintered, wherein the preparation method comprises the following two processes: the drying temperature is 50-250 ℃ and the drying time is 10 minutes-12 hours; the sintering temperature is 300-1000 ℃, and the sintering time is 10 minutes-12 hours.
According to the preparation method of the graphene photothermal conversion material for seawater desalination and water purification treatment, the hydrophilization treatment of the bottom surface of the sintered foam material is realized by adopting a chemical oxidation method, an oxygen plasma treatment method or coating a hydrophilic polymer coating.
The design principle of the invention is as follows:
the graphene foam material prepared by the invention is microscopically a macroscopic black body material formed by disordered stacking of graphene nano sheets, when light irradiates the material, the light is not reflected outwards, but is finally and completely converted into heat inside a pore structure of the material through continuous reflection and refraction, and the heat is absorbed by the material. The photo-thermal conversion mode can utilize the light effect and the heat effect of solar energy to the maximum extent at the same time, and graphene foam in the air can be heated to a very high temperature (150-200 ℃) quickly under the illumination condition.
Due to its very low density (-0.3 g/cm)3) The graphene foam can float on the water surface, and due to the capillary action of micro channels in the graphene foam, water can permeate into the graphene foam and be attached to the surface of a graphene nanosheet in the form of a micro liquid film; due to the fact that the graphene has extremely high thermal conductivity, when the graphene foam is heated by illumination, heat can be quickly conducted into pores to heat water; because water in the micropore structure exists in the form of an ultrathin liquid film and the acting force between graphene and water molecules is weak, the energy barrier to be overcome by water film evaporation is greatly reduced, and therefore, water in the pores of graphene foam can be quickly converted into low-temperature water vapor to overflow; simultaneously, the liquid is soaked due to the siphon actionThe water outside the foam is continuously sucked into the foam and the above cycle is repeated until the water in the container is completely evaporated.
In the actual preparation process, a polymer and graphene composite sintering method is utilized, so that the mechanical strength of graphene foam is improved, and meanwhile, a surface layer with super-hydrophobicity and a super-microporous structure is formed on the surface of the graphene foam, the phenomenon of micropore blockage caused by the fact that ions in water are diffused into the foam material to be separated out can be prevented, and the continuous transmission and evaporation of water are guaranteed; however, since the superhydrophobic surface is not favorable for wetting the foam material with water in an initial state, a contact surface of the foam material and water needs to be subjected to hydrophilization treatment, and the hydrophilization treatment can be realized by adopting surface chemical oxidation, oxygen plasma treatment or a method of coating a hydrophilic polymer layer.
The invention has the following beneficial effects:
1. under the condition of sufficient sunlight, the ambient temperature is within the range of 10-50 ℃, the water evaporation rate obtained by using the graphene foam is more than 1000 times of the natural evaporation rate of the water surface with the same area, and is more than 5 times of the efficiency of the current commercial heat collection type solar water evaporation device.
2. Due to the extremely high thermal conductivity and hydrophobicity of the graphene, the utilization rate of heat generated by evaporating water by utilizing graphene foam is extremely high, the initial temperature of formed water vapor is only 50-60 ℃, and condensation is facilitated.
3. The device for manufacturing the desalination and water purification device by utilizing the graphene foam has the advantages of simple structure, convenience in use, low cost, easiness in manufacturing small-sized portable equipment, no consumption of electric energy or other energy sources and convenience in use.
4. The graphene foam material can be repeatedly used and is convenient to clean, and micro-pores cannot be blocked due to salt precipitation, so that the graphene foam material can be applied to seawater desalination and distillation purification of sewage.
Drawings
FIG. 1 is a schematic cross-sectional microstructure of a graphene foam photothermal conversion material prepared in example 1.
FIG. 2 shows scanning electron microscope microscopic microstructures of the upper surface (a, b) and the lower surface (c, d) of the graphene foam photothermal conversion material prepared in example 1.
Detailed Description
In the specific implementation process, graphene powder, a polymer material with a chain-like molecular structure and a solvent are prepared into slurry according to a proportion, the slurry is added into a mold for drying and heat treatment, organic substances in the material are carbonized, and the graphene foam material with good mechanical strength is obtained, wherein the mechanical strength range of the graphene foam material is tensile strength: 0.5 to 5 MPa; the elastic modulus is 30-50 MPa; and carrying out hydrophilization treatment on one side of the bottom surface of the graphene foam material to prepare the graphene photothermal conversion material for sewage and seawater distillation purification and desalination treatment. Wherein the content of the first and second substances,
the graphene material can be eigen-state graphene, modified graphene or graphene oxide prepared by various methods; the intrinsic graphene or graphene derivative is characterized in that the thickness of a sheet layer is that the number of carbon atom layers is less than 10, and the optimized number of layers is 1-5; the sheet layer thickness/diameter ratio is greater than 10, and the optimized sheet thickness/diameter ratio distribution is 1000-5000; the graphene derivative mainly comprises graphene oxide, a sheet-like graphene structure grafted or coated with other molecular chain segments, defective or doped graphene and the like, and the carbon layer structure of the graphene derivative meets the structural characteristics described above.
The preparation method of the eigenstate graphene or the graphene derivative comprises the following three methods: the graphene powder or liquid phase dispersion is prepared by taking graphite as a raw material through expansion stripping, the graphene powder or liquid phase dispersion is formed by crushing or dispersing graphene prepared by taking a gaseous carbon source as a raw material through Chemical Vapor Deposition (CVD) or Physical Vapor Deposition (PVD), or the graphene-like two-dimensional sheet material formed by chemical polymerization of a small molecular substance is aggregated to form the powder or liquid phase dispersion.
Polymers having a chain-like molecular structure include, but are not limited to, the following: sucrose, cellulose and its derivatives, thermoplastic and thermosetting resin materials (such as polyvinyl alcohol, polyethylene, polypropylene, epoxy resin, phenolic resin, aldehyde ketone resin, etc.); the solvent used is a good solvent corresponding to the polymer material.
In the slurry prepared from the graphene and the polymer material, the proportion range of the solid matter is 0.1-50% by weight, and the preferable proportion is 1-10%; wherein the ratio of the graphene to the polymer material is 1000: 1-1: 100 by weight, and the preferable ratio is 50: 1-1: 1; the shape of the mold for graphene slurry molding is not particularly limited, but the mold is required to withstand heat treatment at 300-1000 ℃ without deformation or damage; after the graphene slurry is added into a mold, two processes of drying and sintering are required, wherein the drying temperature is different according to different solvents, generally ranges from 50 ℃ to 250 ℃, the time ranges from 10 minutes to 12 hours, and the preferable time range is 1 hour to 2 hours; the sintering temperature is 300-1000 ℃, the preferred temperature is 600-800 ℃, the time is 10 minutes-12 hours, and the preferred time is 3-5 hours; the hydrophilization treatment of the bottom surface of the foam after sintering can be carried out by chemical oxidation, oxygen plasma treatment or by applying a hydrophilic polymer coating (e.g., polyvinyl alcohol, hydroxyethyl cellulose, etc.).
The process is described in detail below with specific examples.
Example 1
Mixing 50g of graphene powder, 15g of polyvinyl alcohol and 1kg of water, then preparing the mixture into uniform slurry by utilizing high-speed shearing emulsification, carrying out high-speed centrifugation on the slurry, and collecting lower-layer slurry, wherein the solid content (weight ratio) of the lower-layer slurry is 8.7%; pouring the slurry into a bottom area of 225cm2Spreading in square stainless steel mold (15cm × 15cm) to form cake with thickness of about 2 cm; and standing the material cake and the die for 12 hours at room temperature, then putting the material cake and the die into a forced air drying oven, heating the material cake to 80 ℃, drying the material cake for 4 hours, then taking the material out, putting the material into a muffle furnace, heating the material to 550 ℃, and preserving the heat for 5 hours to completely carbonize the polyvinyl alcohol in the material. And cooling to room temperature, and taking out the black foam material in the mold to obtain the graphene foam material with good mechanical strength. Preparing polyvinyl alcohol into a uniform aqueous solution with the concentration of 5 wt%, and brushing the polyvinyl alcohol solution on the bottom of a mold in the sintering process of the graphene foam material by using a brushAnd (3) coating the side of the graphene composite foam material for 1-2 times, naturally airing, and then performing crosslinking treatment on the side of the graphene composite foam material by using borax to prepare the graphene composite foam material for photothermal conversion of fresh water and purified water.
The schematic diagram of the cross-sectional microstructure of the graphene foam material is shown in the attached drawing 1, the microstructure of the upper surface and the microstructure of the lower surface of the graphene foam material are shown in the attached drawing 2, and the upper surface (shown in the attached drawings 2a-b) of the graphene foam material has obvious macropore (the aperture is larger than 0.1 micrometer and smaller than or equal to 10 micrometers) and mesopore (the aperture is 1-100 nanometers) structures and is mainly used for absorbing light rays and evaporating moisture; the lower surface (fig. 2c-d) is mainly provided with a micropore (the pore diameter is more than or equal to 0.1 nanometer and less than 1 nanometer) structure, and is mainly used for filtering salt and impurities in water and only allowing water molecules to permeate.
Example 2
Mixing 20g of graphene powder, 10g of hydroxyethyl cellulose and 800g of ethanol, then preparing the mixture into uniform slurry by high-speed shearing emulsification, carrying out high-speed centrifugation on the slurry, and collecting the lower-layer slurry, wherein the solid content (weight ratio) of the lower-layer slurry is 6.6%; pouring the slurry into a circular stainless steel mold with the bottom surface diameter of 35cm, and paving to form a material cake with the thickness of about 2.2 cm; and standing the material cake and the die for 12 hours at room temperature, then putting the material cake and the die into a forced air drying oven, heating the material cake to 80 ℃, drying the material cake for 4 hours, then taking the material out, putting the material into a muffle furnace, heating the material to 850 ℃, and preserving the heat for 5 hours to completely carbonize the hydroxyethyl cellulose in the material. And cooling to room temperature, and taking out the black foam material in the mold to obtain the graphene foam material with good mechanical strength. The bottom surface (the surface soaked in water) is treated by oxygen plasma for 10 minutes to ensure that the surface has good hydrophilicity and can be used for thermal evaporation of purified water.
Example 3
200g of graphene oxide water slurry with the solid content of 5 wt% and 500g of sodium carboxymethylcellulose water solution with the solid content of 1 wt% are mixed and stirred to form uniform slurry, wherein the solid content is 2.2 wt%; pouring the slurry into a circular stainless steel mold with the bottom surface diameter of 35cm, and paving to form a material cake with the thickness of about 2.2 cm; and standing the material cake and the die for 12 hours at room temperature, then putting the material cake and the die into a forced air drying oven, heating the material cake to 80 ℃, drying the material cake for 4 hours, then taking the material out, putting the material into a muffle furnace, heating the material to 1000 ℃, and preserving the heat for 5 hours to completely carbonize the sodium carboxymethylcellulose in the material. And cooling to room temperature, and taking out the black foam material in the mold to obtain the graphene foam material with good mechanical strength. The bottom surface (the surface soaked in water) is treated by oxygen plasma for 10 minutes to ensure that the surface has good hydrophilicity and can be used for thermal evaporation of purified water.
The embodiment result shows that sunlight can be efficiently converted into heat by utilizing the blackbody structure and the high heat conduction property of the graphene foam; the capillary action of the foam structure is utilized to continuously convey water and reduce the evaporation potential barrier, thereby realizing the rapid distillation and desalination of seawater. Under the same illumination condition with the ambient temperature of 10-50 ℃, the water evaporation rate obtained by using the graphene foam is more than 1000 times of the natural evaporation rate of the water surface in the same area. The graphene foam material can be used for conveniently manufacturing a small-sized portable high-efficiency seawater desalination and solar sewage purification device, and meets the requirement of quickly preparing clean fresh water on the sea and outdoors.
Claims (6)
1. A preparation method of a graphene photothermal conversion material for seawater desalination and water purification treatment is characterized in that graphene powder, a polymer material with a chain-shaped molecular structure and a solvent are prepared into slurry, and the slurry is added into a mold for drying and heat treatment to carbonize organic substances in the material, so that a graphene foam material with good mechanical strength is obtained; carrying out hydrophilization treatment on one side of the bottom surface of the graphene film to prepare the graphene photothermal conversion material for distillation purification and desalination treatment of sewage and seawater;
in the slurry prepared from the graphene and the polymer material, the proportion range of the solid matter is 0.1-50% by weight, wherein the proportion range of the graphene and the polymer material is 1000: 1-1: 100 by weight;
the graphene slurry is added into a mold and then dried and sintered, wherein: the drying temperature is 50-250 ℃ and the drying time is 10 minutes-12 hours; the sintering temperature is 300-1000 ℃, and the time is 10 minutes-12 hours;
the polymer with chain molecular structure is one of sucrose, cellulose derivative, thermoplastic resin and thermosetting resin material, and the solvent is good solvent corresponding to the polymer material.
2. The method for preparing graphene photothermal conversion material for seawater desalination and water purification as claimed in claim 1, wherein the graphene material used is eigen-state graphene or graphene derivatives prepared by various methods; the thickness of the lamella of the eigenstate graphene or graphene derivative is that the number of carbon atom layers is less than 10, and the lamella diameter/thickness ratio of the lamella is more than 10.
3. The method for preparing a graphene photothermal conversion material for seawater desalination and water purification as claimed in claim 2, wherein the graphene derivative comprises one of modified graphene, graphene oxide, a sheet-like graphene structure grafted or coated with other molecular segments, and defective or doped graphene.
4. The method for preparing graphene photothermal conversion material for seawater desalination and water purification as claimed in claim 2, wherein the method for preparing the eigenstate graphene or graphene derivative comprises: graphene powder or liquid phase dispersion prepared by taking graphite as a raw material through expansion stripping, graphene prepared by taking a gaseous carbon source as a raw material through chemical vapor deposition or physical vapor deposition, and graphene powder or liquid phase dispersion formed by crushing or dispersing, or powder or liquid phase dispersion formed by gathering graphene-like two-dimensional sheet materials formed by chemical polymerization of small molecular substances.
5. The method for preparing the graphene photothermal conversion material for seawater desalination and water purification treatment according to claim 1, wherein the shape of the mold for graphene slurry molding is not particularly limited, and the graphene slurry can be subjected to heat treatment at 300-1000 ℃ without deformation or damage.
6. The method of preparing graphene photothermal conversion material for seawater desalination and water purification as claimed in claim 1, wherein the hydrophilization treatment of the bottom surface of the sintered foam is performed by a chemical oxidation method, an oxygen plasma treatment method, or a hydrophilic polymer coating.
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