CN113149115B - Multistage heterostructure membrane for photo-thermal seawater desalination and preparation method - Google Patents
Multistage heterostructure membrane for photo-thermal seawater desalination and preparation method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/14—Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
Abstract
The invention discloses a multistage heterostructure membrane for photo-thermal seawater desalination and a preparation method thereof, which takes a porous metal net as a substrate and prepares a porous metal-carbon nanotube film by a chemical vapor deposition method; then sulfide Ni grows on the surface of the porous metal film by a hydrothermal synthesis method 3 S 2 Forming porous metal/carbon nanotube/Ni 3 S 2 A heterostructure film. The metal net of the invention takes macroscopic holes as the transmission channel of water, after the carbon nano-tube is prepared on the metal net, because the carbon nano-tube is thinner, according to the general flow continuity equation in hydrodynamics: v 1 A 1 Where V is the flow velocity, a is the cross-sectional area of the pipe, C is a constant, the thinner the pipe is, the smaller the cross-sectional area a is, the larger the flow velocity V of the liquid in the pipe is, and the faster the liquid flows, which is equivalent to increasing the transport path of water, and Ni grows on the carbon nanotubes 3 S 2 The heterogeneous layer has excellent light absorption capacity, and increases the evaporation of seawater.
Description
Technical Field
The invention relates to a multistage heterostructure membrane for photo-thermal seawater desalination and a preparation method thereof, belonging to the field of material synthesis and preparation. In particular to a method for preparing a carbon nanotube material on porous metal by using a chemical vapor deposition method and then synthesizing Ni by using a hydrothermal method 3 S 2 Preparing a photo-thermal conversion and catalytic purification layer on the porous metal/carbon nanotube film by using porous metal/carbon nanotube/Ni 3 S 2 After the heterostructure film is arranged on the surface of seawaterThe seawater on the surface of the membrane is evaporated and the organic matters are decomposed by the heating action of the photo-thermal conversion and catalytic purification layer, thereby achieving the purposes of desalting and purifying the seawater. The invention combines chemical vapor deposition and hydrothermal synthesis to prepare porous metal/carbon nano tube/Ni 3 S 2 The heterogeneous structure film can change the reaction temperature and hydrothermal reaction time of vapor deposition to obtain carbon nanotube and sulfide Ni with different tube diameters and arrays 3 S 2 So as to combine the porous metal to form a heterostructure according to actual needs, and realize the multifunctional application of photothermal conversion and seawater desalination.
Background
With the shortage of fresh water resources in the world, seawater desalination has become one of the important means for obtaining fresh water resources. The conventional seawater desalination has high energy consumption, high cost and low efficiency, and simultaneously, the situation of energy shortage is also aggravated. Therefore, it is an important development direction to desalinate seawater by using renewable clean energy such as solar energy.
Chinese patent application No.: 202010183922.6 discloses a self-cleaning light absorption medium for photo-thermal seawater desalination and a preparation method thereof, the light absorption medium with high efficiency and self-cleaning has a surface light absorption coating with larger specific surface area by virtue of a micron-sized porous structure on the surface of polymer foam, the maximum light absorption efficiency (90%) and higher photo-thermal seawater desalination efficiency are obtained, and the problem that photo-thermal evaporation cannot be sustained due to the separation of salt on the surface of the traditional photo-thermal medium is solved.
Patent application No.: 202010011966.0 discloses a solar evaporator with hollow structure, its preparation method and application, the solar evaporator has hollow structure inside, and the outer shell can have a convex evaporation surface, compared with the plane evaporator, it has larger evaporation area per unit area, and is beneficial to the absorption of solar energy. The evaporator has stable shape and structure and can be used for a long time.
Patent application No.: 202010728027.8 discloses a preparation method and application of an extremely tolerant carbon nanotube hydrogel. The carbon nanotube hydrogel disclosed by the invention has an ultra-fast water transmission characteristic, has higher conductivity, shows excellent tolerance capability to acid, alkali, salt, organic and other environments, and can be reversibly recovered under large-degree compression, so that the carbon nanotube hydrogel has a better application prospect in the fields of wound healing, emergency tourniquets, biological medicine carrying, water environment treatment, seawater desalination, new energy devices and the like.
Patent application No.: 201910804891.9 discloses a multi-stage structured photothermal seawater desalination material, its preparation method and application, wherein a nano C material is deposited on a porous metal foam material by Plasma Enhanced Chemical Vapor Deposition (PECVD), and then a WO material with plasma resonance effect is synthesized by solvothermal reaction 3-x To obtain C/WO 3-x The heterostructure acts as a light absorbing material. Light absorber C/WO 3-x Heterostructure has very strong light absorption ability and light-heat conversion ability, is favorable to timely converting absorptive light energy into heat energy and is used for the sea water desalination, and moisture can not reach the extinction body surface and cause the salinity to pile up in the water evaporation process, can not pile up and harm the material because of the salinity, the longe-lived of material.
Patent application No.: 201911153479.1 discloses a photothermal water evaporator based on loofah sponge biomass, which is characterized in that loofah sponge is used as a raw material, and steps such as molding and carbonization are carried out to obtain a porous biomass charcoal piece, and the prepared material has self-floating performance, can efficiently absorb sunlight and convert the sunlight into heat energy, and obtains good solar water evaporation performance. After the biomass carbon sheet is subjected to in-situ deposition of the carbon nano tubes, the water evaporation performance is improved. The invention takes the loofah sponge as the raw material, the raw material is environment-friendly and renewable, the preparation process of the water evaporation device is simple, and the large-scale production can be realized; the water evaporation operation is convenient, and the method has good application prospect in the field of wastewater treatment.
The membrane material used for membrane distillation should meet the requirements of porosity, sufficient mechanical strength, good thermal stability and chemical stability, etc. However, most of the membrane materials used for seawater desalination at home and abroad at present have some defects, such as poor thermal stability, easy aging, poor solvent resistance, short service life of the membrane and the like. Therefore, the development of a novel, efficient and stable porous membrane material and a preparation method thereof are urgently needed, and the membrane material is also required to have high sunlight absorption and conversion efficiency and the like.
The technology similar to the invention is as follows:
chinese patent application No.: 201811307159.2 discloses a method for preparing a catalyst containing TiO on the surface by hydrothermal method and calcination 2 The porous ceramic heterostructure membrane has a complex preparation method, and impurities containing Ti are easy to appear in the calcining process due to the existence of Ti.
Chinese patent application No.: 201910804891.9 discloses a multi-stage structured photothermal seawater desalination material, its preparation method and application, wherein CH is required to be used in the process of depositing nano-C material by plasma enhanced chemical vapor deposition (PECVD for short) 4 、H 2 And Ar, etc., and has high preparation requirement and low forming rate.
Chinese patent application No.: 202010728027.8 discloses an extremely tolerant carbon nanotube hydrogel, its preparation method and application. Preparing carbon nanotube aerogel by floating catalytic chemical vapor deposition and secondary deposition (namely depositing a nano C material by Plasma Enhanced Chemical Vapor Deposition (PECVD)), introducing a carbon source, a reducing gas and a catalyst into a reaction chamber in the reaction process, and introducing a gas CH 4 As a carbon source, H 2 The carrier gas needs precise and accurate operation, so the preparation process has certain uncontrollable factors.
Disclosure of Invention
In order to improve the thermal stability and the chemical stability of a membrane material used for seawater desalination and keep good sunlight absorption and conversion efficiency, the invention provides a multistage heterostructure membrane for photothermal seawater desalination.
The invention also provides a preparation method of the multilevel heterostructure film.
In order to achieve the purpose, the invention adopts the technical scheme that:
a multi-stage heterostructure film for photo-thermal seawater desalination is characterized in that porous metal is used as a substrate, and a porous metal-carbon nanotube film is prepared by a chemical vapor deposition method; then sulfide Ni grows on the surface of the porous metal film by a hydrothermal synthesis method 3 S 2 Etc. to form porous metal/carbon nanotube/Ni 3 S 2 The heterostructure film enhances the photo-thermal conversion and catalytic purification effects; the carbon nano-tube and sulfide Ni with different tube diameters and arrays can be obtained by changing the reaction temperature and the hydrothermal reaction time of vapor deposition 3 S 2 So as to form a heterostructure according to actual needs. After the porous metal heterostructure film is placed on the surface of seawater, the seawater is evaporated and organic matters are decomposed through photothermal conversion, light absorption of a catalytic purification layer and photocatalysis, so that the purposes of desalting and purifying the seawater are achieved.
The preparation method of the multistage heterostructure membrane for the photothermal seawater desalination comprises the following steps:
the first step is as follows: substrate pretreatment
Cutting a porous metal Ni, Ti, Al or Cu net and the like into 2 x 2cm, and respectively carrying out ultrasonic cleaning on the porous metal net for 5-10 minutes by using acetone, absolute ethyl alcohol, 3% hydrochloric acid and deionized water to remove impurities and oxides on the surface.
The second step is that: preparation of carbon nanotubes
Growing a carbon nano tube by chemical vapor deposition in a tubular furnace at 760-960 ℃ in a nitrogen atmosphere, wherein acetonitrile is used as a carbon source, and ferrocene is used as a catalyst; when the method is implemented, firstly, the temperature of a tubular furnace is increased under 500sccm of nitrogen, when the temperature of the tubular furnace is increased to a required temperature (760-960 ℃), the flow rate of the nitrogen is adjusted to 200sccm, a mixed solution of liquid acetonitrile and ferrocene is injected at the same time, the injection rate is 15ml/h, the injection time is 8-12 minutes per cubic centimeter of steel wire mesh, the acetonitrile is subjected to cracking to obtain carbon atoms and carbon cluster molecules under a high-temperature condition, the decomposed carbon source molecules are subjected to adsorption reaction on the surfaces of catalyst particles, the carbon source molecules on the surfaces of the catalyst particles are separated out through diffusion, and finally, the carbon nano tubes are grown on the surfaces of porous metals according to a certain arrangement sequence. The carbon nano tubes with different tube diameters and different arrays can be obtained by changing the reaction temperature and the substrate, and a heterostructure is constructed according to actual requirements;
further: the mixed solution of acetonitrile and ferrocene was prepared by dissolving 0.4g of ferrocene powder in 20ml of acetonitrile and ultrasonically dispersing.
Further: the injection time of the mixed solution of acetonitrile and ferrocene was 40 minutes.
Step three, hydro-thermal synthesis of porous metal/carbon nano tube/Ni 3 S 2 Heterostructure thin films:
5mM (millimolar) Ni (NO) 3 ) 2 ·6H 2 O，5mMCH 4 N 2 S, 30ml of deionized water is mixed and stirred uniformly, the mixture and the obtained porous metal film are placed in a 50ml reaction kettle together, the reaction kettle is placed in a constant temperature forced air drying oven, the temperature is kept for 12 hours at 120 ℃, and in the process, nickel nitrate (Ni (NO) (Ni) is added 3 ) 2 ·6H 2 O) and thiourea (CH) 4 N 2 S) decomposition, the sulfur element and the nickel element react to generate Ni 3 S 2 And other sulfides, etc. to form a layer of Ni on the surface of the porous metal/carbon nanotube after the reaction is finished 3 S 2 A nanoribbon.
The fourth step: applications of
The porous metal heterostructure membrane is arranged on the surface of seawater to be treated, seawater is evaporated and organic matters are decomposed through photothermal conversion, light absorption of a catalytic purification layer and photocatalysis, so that the aim of desalting and purifying seawater is fulfilled, and the porous metal heterostructure membrane with the vertical array carbon nano tubes can be designed for improving the strength and the light absorption efficiency.
The invention has the beneficial effects that:
(1) the invention prepares the porous metal/carbon nanotube film by chemical vapor deposition synthesis, has simple process and experimental equipment, and can effectively control the synthesis conditions by adjusting the reaction temperature, the catalyst and the like. The reaction temperature is changed to obtain the carbon nano tube with the diameter of about 20-50 nm. The carbon material has good photo-thermal conversion performance and good light absorption performance in a wide waveband, can absorb sunlight and convert the sunlight into heat, and improves the evaporation rate of seawater desalination.
(2) Compared with a polymer membrane, the porous metal membrane has better thermal stability and chemical stability, the average evaporation rate of the porous metal membrane is not obviously changed after 50 hours of experimental circulation, and the carbon nano tube has excellent tolerance capacity and has good seawater desalination capacity no matter being used for a long time or being used in organic dye and heavy metal ion solution.
(3) Forming nano Ni on the surface of porous metal film 3 S 2 And the heterogeneous layer is used for synthesizing and constructing the photo-thermal material and structure, and the process method is simple and is suitable for popularization and application. Ni with different thicknesses can also be obtained by changing the hydrothermal reaction time 3 S 2 And nanoribbons are combined into a gradient structure according to actual needs. Ni 3 S 2 Has excellent light absorption capacity and corrosion resistance, the carbon nano tube belongs to a long tubular carbon material, Ni 3 S 2 Can grow on the carbon nano tube to form a natural water transmission channel to promote the evaporation of seawater.
(4) The metal net of the invention takes macroscopic holes as the transmission channel of water, after the carbon nano-tube is prepared on the metal net, because the carbon nano-tube is thinner, according to the general flow continuity equation in hydrodynamics: v 1 A 1 Where V is the flow velocity, a is the cross-sectional area of the pipe, C is a constant, the thinner the pipe is, the smaller the cross-sectional area a is, the larger the flow velocity V of the liquid in the pipe is, and the faster the liquid flows, which is equivalent to increasing the transport path of water, and Ni grows on the carbon nanotubes 3 S 2 The heterogeneous layer has excellent light absorption capacity, and increases the evaporation of seawater.
Drawings
FIG. 1 is a 3500-fold magnified scanning topography of an example of a carbon nanotube grown on a porous metallic Ni mesh;
FIGS. 2a and 2b are views illustrating the formation of Ni on the surface of a porous metal Ni/carbon nanotube by the method of the present invention 3 S 2 8000 and 200000 times of amplified nanoribbon scanning topography;
FIG. 3 is a graph comparing the mass loss of seawater desalination in one illumination of porous metal films grown at different hydrothermal temperatures;
FIG. 4 is a graph comparing evaporation efficiency of seawater desalination under one illumination for porous metal films grown at different hydrothermal temperatures;
FIG. 5 is a graph of the evaporation rate of porous metallic Ni/carbon nanotubes in one illumination cycle for 50 h.
Detailed Description
The technical scheme of the invention is further explained by combining the embodiment according to the attached drawings.
Example one
The first step is as follows: substrate pretreatment
Cutting the porous metal Ni net into 2 x 2cm, and ultrasonically cleaning the porous metal Ni net for 5-10 minutes by respectively using acetone, absolute ethyl alcohol, 3% hydrochloric acid and deionized water to remove impurities and oxides on the surface.
The second step is that: preparation of carbon nanotubes
The method comprises the steps of growing carbon nanotubes on the surface of a porous metal Ni net by utilizing a tubular furnace through chemical vapor deposition at 860 ℃ in a nitrogen atmosphere, using acetonitrile as a carbon source and ferrocene as a catalyst, firstly heating the tubular furnace at 500sccm of nitrogen, adjusting the flow rate of the nitrogen to 200sccm after the temperature of the tubular furnace is increased to 860 ℃, simultaneously injecting a mixed solution of the acetonitrile and the ferrocene, cracking carbon atoms and carbon cluster molecules out of the acetonitrile under a high-temperature condition, carrying out adsorption reaction on the decomposed carbon source molecules on the surface of catalyst particles, and growing the carbon nanotubes on the surface of the porous metal Ni net according to a certain arrangement sequence (see figure 1).
The third step: hydrothermal synthesis of porous metal/carbon nano tube/Ni 3 S 2 Heterostructure thin films
5mM Ni (NO) 3 ) 2 ·6H 2 O，5mM CH 4 N 2 S, 40ml of deionized water is mixed and stirred evenly, and the mixture and the obtained porous metal film are placed in a 50ml reaction kettle together. Placing the mixture into a constant temperature blast drying oven, keeping the temperature for 12 hours at 120 ℃, and forming a layer of Ni on the surface of the porous metal Ni/carbon nano tube after the reaction is finished 3 S 2 Nanobelts (see fig. 2a and 2 b). The quality loss of the prepared porous metal film for seawater desalination under one illumination is 2.57kgm -2 The evaporation efficiency was 158.39%. (see fig. 3 and 4, respectively).
The fourth step: applications of
The porous metal heterostructure membrane is arranged on the surface of seawater to be treated, seawater is evaporated and organic matters are decomposed through photothermal conversion, light absorption of a catalytic purification layer and photocatalysis, so that the aim of desalting and purifying seawater is fulfilled, and the porous metal heterostructure membrane with the vertical array carbon nano tubes can be designed for improving the strength and the light absorption efficiency.
Example two
Except that the third step is hydrothermally synthesized into porous metal/carbon nano tube/Ni 3 S 2 The hydrothermal heat preservation time of the heterostructure film is changed to be 8 hours, and other processes and parameters are the same as those of the first embodiment. The quality loss of the prepared porous metal film for seawater desalination under one illumination is 2.235kgm -2 The evaporation efficiency was 138.31%. (see fig. 3 and 4, respectively).
EXAMPLE III
Except that the third step is hydrothermally synthesized into porous metal/carbon nano tube/Ni 3 S 2 The hydrothermal heat preservation time of the heterostructure film is changed from 12h to 10h, and other processes and parameters are the same as those of the first embodiment. The prepared porous metal film has the mass loss of 2.3kgm for seawater desalination under one-time illumination -2 The evaporation efficiency was 139.2%. (see fig. 3 and 4, respectively).
Example four
The same procedures and parameters as those of the first embodiment are carried out except that the hydrothermal heat preservation time of 12h for the third step of hydrothermally synthesizing the porous metal/carbon nanotube/Ni 3S2 heterostructure film is changed into 16 h. The quality loss of the prepared porous metal film for seawater desalination under one-time illumination is 1.941kgm -2 The evaporation efficiency was 114.53%. (see fig. 3 and 4, respectively).
FIG. 5 is a graph of the evaporation rate of porous metallic Ni/carbon nanotubes in one illumination cycle for 50h, as seen in the graph. After the experiment is circulated for 50 hours, the average evaporation rate of the porous metal film is not obviously changed (figure 5), which shows that the porous metal film has better thermal stability and chemical stability, the carbon nano tube has excellent tolerance capability, and the seawater desalination capability is good no matter the porous metal film is used for a long time or in organic dye and heavy metal ion solution.
Claims (2)
1. Preparation method of multistage heterostructure membrane for photo-thermal seawater desalinationThe method is characterized in that the multistage heterostructure membrane for the photo-thermal seawater desalination is a porous metal-carbon nanotube membrane prepared by a chemical vapor deposition method by taking a porous metal net as a substrate; then sulfide Ni grows on the surface of the porous metal-carbon nano tube film by a hydrothermal synthesis method 3 S 2 Forming porous metal/carbon nanotube/Ni 3 S 2 The heterostructure film is prepared by the following steps:
the first step is as follows: substrate pretreatment
Cutting a porous metal Ni, Ti, Al or Cu net into 2 x 2cm, respectively using acetone, absolute ethyl alcohol, 3% hydrochloric acid and deionized water to ultrasonically clean the porous metal net for 5-10 minutes, and removing impurities and oxides on the surface;
the second step is that: preparation of porous metal-carbon nanotube film
Growing a carbon nano tube by chemical vapor deposition in a tubular furnace at 760-960 ℃ in a nitrogen atmosphere, wherein acetonitrile is used as a carbon source, and ferrocene is used as a catalyst; during implementation, firstly, heating the tubular furnace under 500sccm of nitrogen, adjusting the flow of nitrogen to 200sccm when the temperature of the tubular furnace is raised to a required temperature of 760-960 ℃, simultaneously injecting a mixed solution of liquid acetonitrile and ferrocene, wherein the injection rate is 15ml/h, the injection time is 8-12 minutes per cubic centimeter of porous metal mesh, acetonitrile is subjected to high-temperature cracking to obtain carbon atoms and carbon cluster molecules, the decomposed carbon source molecules are subjected to adsorption reaction on the surfaces of catalyst particles, the carbon source molecules on the surfaces of the catalyst particles are separated out through diffusion, and finally, carbon nano tubes are grown on the surfaces of the porous metal according to a certain arrangement sequence; the mixed solution of the acetonitrile and the ferrocene is formed by dissolving 0.4g of ferrocene powder in 20ml of acetonitrile and ultrasonically dispersing;
the third step: hydrothermal synthesis of porous metal/carbon nano tube/Ni 3 S 2 Heterostructure thin films
5mM Ni (NO) 3 ) 2 ·6H 2 O，5mMCH 4 N 2 S, 30ml of deionized water is mixed and stirred evenly, the mixture and the porous metal-carbon nano tube film obtained in the second step are placed in a 50ml reaction kettle together, the reaction kettle is placed in a constant temperature forced air drying oven for heat preservation for 12 hours at 120 ℃, and in the process, nitric acid is addedNickel (Ni (NO) 3 ) 2 ·6H 2 O) and thiourea (CH) 4 N 2 S) decomposition, the sulfur element and the nickel element react to generate Ni 3 S 2 And other sulfides, forming a layer of Ni on the surface of the porous metal/carbon nanotube after the reaction is finished 3 S 2 A nanoribbon.
2. The method of preparing a multi-stage heterostructure membrane for photothermal desalination of sea water according to claim 1, wherein the time for injecting the mixed solution of liquid acetonitrile and ferrocene is 40 minutes.
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