CN112897618B - Three-dimensional photothermal conversion material capable of efficiently treating saline water and wastewater, device and method - Google Patents
Three-dimensional photothermal conversion material capable of efficiently treating saline water and wastewater, device and method Download PDFInfo
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
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- Y02A20/138—Water desalination using renewable energy
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Abstract
The invention discloses a three-dimensional photothermal conversion material, a device and a method capable of efficiently treating saline water and wastewater, wherein the preparation method comprises the following steps: adjusting the pH value of the graphene oxide solution to 7-13 to obtain a solution A; preparing a polymer electrolyte solution to obtain a solution B; mixing the following components in a solution A: the concentration ratio of the solution B to the solution A is 3: 1-3: 12, and the solution B is dropwise added into the solution A to obtain a charged graphene oxide compound solution; immersing the pretreated clean and dry melamine foam into the charged graphene oxide compound solution to enable the melamine foam to fully absorb the charged graphene oxide compound solution; and (3) placing the melamine foam with saturated adsorption in a drying oven at the temperature of 60-200 ℃ for heat treatment for 6-24 hours, and cleaning and drying to obtain the three-dimensional photo-thermal conversion material. The material has high photo-thermal conversion rate, good performance stability, good elasticity, easy cutting, repeated recycling, simple preparation process, low synthesis cost and wide application range, and can be used for desalting seawater with low concentration to high concentration, purifying a composite polluted water body and the like.
Description
Technical Field
The invention belongs to the field of seawater desalination and sewage purification, and particularly relates to a three-dimensional photothermal conversion material, a device and a method capable of efficiently treating brine and wastewater.
Background
With the growth of population and the development of society, the problems of energy shortage and water resource shortage seriously threaten the survival and development of human beings. The solar evaporation technology can realize efficient water evaporation by using the converted heat energy by using sustainable sunlight as a driving force and by using a core component of a photothermal converter. In recent years, various photothermal converters have been reported, such as a semiconductor based on the principle of generating heat by plasmon resonance, a noble metal based on the principle of generating heat by recombination of photogenerated carriers, and a carbonaceous material based on the mechanism of generating heat by vibration and rotation of a molecular skeleton. However, the absorption range of the noble metal photothermal converter to light is difficult to regulate and has high cost, and the improvement of the semiconductor photothermal converter requires a sophisticated regulation technique. Based on this, carbonaceous materials are currently the most promising photothermal converters.
Seawater desalination is an important application field of current photothermal conversion.
The bottleneck of limiting the application of the carbonaceous material to efficient seawater desalination at present is that with the continuous operation of seawater desalination, salt such as sodium chloride and the like is easy to form crystals to be separated out on the surface of the light absorber, so that the absorption of the light energy is influenced, and the photo-thermal conversion efficiency of the light absorber is greatly reduced. There is therefore a great need for an efficient and feasible strategy for imparting excellent salt crystallization resistance to light absorbers.
It has been shown that hydrophilic light absorption can rapidly dissolve and dilute the salt ions concentrated on the surface of the absorber by evaporation, but because the light absorber is hydrophilic, a large amount of the converted heat can be carried away by the surrounding water and dissipated into the bulk water and material voids by conduction, convection, etc. For this reason, a feasible method is needed to reduce the loss of this part of energy.
The invention patent with publication number CN 109603596A discloses a photo-thermal seawater desalination membrane made of metal organic framework material, wherein a photo-thermal converter in the invention is composed of a photo-thermal conversion layer, a salt rejection layer and a buoyancy layer, and has good photo-thermal conversion rate and seawater desalination performance and good material stability. However, the thickness of the photothermal converter in the invention is too small to prevent the conduction and dissipation of heat generated at the interface, which leads to low photothermal conversion efficiency, and the metal-organic framework has complicated preparation process and higher cost.
The invention patent with publication number CN 107739066A discloses a method for preparing a graphene photothermal conversion material for seawater desalination and water purification treatment, which prepares graphene powder, a polymer with a chain-shaped molecular structure and a solvent into slurry, dries and carries out high-temperature heat treatment to obtain the photothermal conversion material with good mechanical strength, and the photothermal conversion material has good photothermal conversion performance after high-temperature carbonization, and the porous structure of polymer foam has excellent water absorption performance, so that the photothermal conversion material has excellent photothermal water evaporation efficiency when applied to seawater desalination. The photothermal conversion material is suitable for the rapid distillation desalination of seawater. However, such a photothermal conversion material synthesis process requires a large amount of energy input, does not meet the basic requirements for sustainable development, and does not consider desalination treatment of high-concentration brine.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a three-dimensional photothermal conversion material, a device and a method capable of efficiently treating saline water and wastewater. The three-dimensional photothermal conversion material has both high-efficiency photothermal conversion efficiency and high-concentration salt solution treatment capacity, and on one hand, the abundant and mutually communicated heat insulation porous networks are favorable for water distribution and steam delivery and effectively reduce heat loss, so that high-efficiency photothermal conversion is realized; on the other hand, the surface of the modified water-based paint is modified, so that the modified water-based paint can be suitable for treating low-concentration to high-concentration seawater and sewage. In addition, by taking commercial melamine as a support body of the photothermal conversion material, the using amount of graphene oxide can be greatly reduced, and the material preparation cost is reduced. Meanwhile, the preparation process is simple, high-temperature treatment is not needed, and the environment is friendly.
The invention adopts the following specific technical scheme:
a preparation method of a three-dimensional photothermal conversion material capable of efficiently treating saline water and wastewater comprises the following specific steps:
s1: adjusting the pH value of the graphene oxide solution to 7-13 to obtain a solution A; preparing a polymer electrolyte solution to obtain a solution B;
s2: mixing the following components in a solution A: dropwise adding the solution B into the solution A according to a concentration ratio of 3: 1-3: 12, and carrying out sufficient reaction through ultrasound to obtain a charged graphene oxide compound solution;
s3: immersing the pretreated clean and dry melamine foam into the charged graphene oxide compound solution, and immersing and extruding the melamine foam to enable the melamine foam to fully absorb the charged graphene oxide compound solution; and (3) placing the melamine foam with saturated adsorption in a drying oven at the temperature of 60-200 ℃ for heat treatment for 6-24 hours, and cleaning and drying to obtain the three-dimensional photo-thermal conversion material.
Preferably, the concentration of the graphene oxide solution in S1 is 3 mg/mL.
Preferably, the pH value of the graphene oxide solution in S1 is adjusted to 10-12 by a sodium hydroxide solution, and the pH value is preferably 12.
Preferably, the polymer electrolyte is one of polyethyleneimine, polydiallyldimethylammonium chloride, polyallylamine hydrochloride, polystyrene sulfonate, polyacrylic acid or sodium alginate, and is preferably polyethyleneimine.
Preferably, the mixing concentration ratio of the solution A to the solution B in the S2 is 3: 9.
Preferably, the pretreatment process of the melamine foam in S3 is specifically as follows: the melamine foam was washed with deionized water and absolute ethanol in this order, repeated several times, and then dried in an oven at 100 ℃.
A second object of the present invention is to provide a three-dimensional photothermal conversion material produced by any of the above production methods.
A third object of the present invention is to provide a photothermal conversion device capable of efficiently treating brine and wastewater, comprising the three-dimensional photothermal conversion material according to the second object, a water absorbing layer, a thermal insulator, and a reactor;
the reactor comprises a first shell and a second shell which are transparent, the first shell is sleeved outside the second shell with a hole at the top, and a condensation cavity is formed between the first shell and the second shell;
the bottom of the second shell is used for containing salt water or waste water, the thermal insulator is arranged above the water containing area in the second shell, the thermal insulator is provided with a water absorbing layer, and the bottom end of the water absorbing layer extends into the water containing area; the three-dimensional photothermal conversion material is arranged on the water absorption layer in a contact manner so as to absorb the water in the water absorption layer and heat and evaporate the water into the condensation cavity; the three-dimensional photothermal conversion material and the water containing area are separated by a thermal insulator, and heat exchange is reduced.
Preferably, the water-absorbing layer is a non-woven fabric, the thermal insulator is polystyrene foam, and the first shell and the second shell are both made of quartz.
A fourth object of the present invention is to provide a method for treating brine or wastewater by using the photothermal conversion apparatus according to the third object, which comprises the following steps:
adding brine or wastewater to be treated to a water-containing region of a photothermal conversion device, followed by placing the photothermal conversion device under a light source;
when light irradiates the three-dimensional photothermal conversion material, the light is subjected to a multi-scattering effect by the porous structure communicated with each other in the melamine foam, part of the light energy is absorbed by graphene oxide which is covered on the surface of the melamine foam and exists in a single-layer or few-layer form, and the rest of the light is transmitted into the three-dimensional photothermal conversion material and is absorbed after being scattered for multiple times; the graphene oxide absorbs light energy to generate heat, and the heat is limited on the surface of the graphene oxide by a thermal insulator and a polymer electrolyte so as to reduce the loss of the heat;
the saline water or the wastewater is in contact with the three-dimensional photothermal conversion material through the water absorption layer and is attached to the melamine foam in a film form, the heat generated by the graphene oxide is rapidly transferred to the surrounding water molecules, the water molecules existing in the film form rapidly absorb the heat and form steam, and the steam is evaporated from the pore channel of the melamine foam and overflows from the hole on the top of the second shell; the steam is condensed into liquid when meeting the top of the first shell at normal temperature and flows to the bottom along the inner wall of the first shell, so that the purification of the salt water or the waste water is realized, and the purified water is obtained.
Compared with the prior art, the invention has the following beneficial effects:
1) the photo-thermal conversion rate of the three-dimensional photo-thermal conversion material prepared by the invention under the illumination condition is respectively 4.30 times and 1.27 times of that of pure water and melamine foam.
2) The three-dimensional photothermal conversion material prepared by the invention has excellent water dispersion performance, unique microscopic thermal confinement effect, multi-scattering effect of a multi-dimensional interconnected pore structure and high light transmittance of the graphene oxide oligo-sheet layer, so that the photothermal conversion rate of the three-dimensional photothermal conversion material is extremely high; the equilibrium temperatures reached in the dry and wet states were 64.5 ℃ and 37.6 ℃ respectively, and the photothermal conversion efficiency reached 93.4%.
3) The three-dimensional photothermal conversion material prepared by the invention utilizes the melamine foam as the framework, so that the consumption of the graphene oxide can be greatly saved, and the manufacturing cost of the three-dimensional photothermal conversion material is reduced; in addition, the synthesis and preparation method of the three-dimensional photothermal conversion material is simple, mild in condition, convenient to use and excellent in performance.
4) The photothermal conversion device of the invention is easy to be prepared into small portable equipment, can also be applied to industrial practice by enlarging the size, and can continuously generate clean water only by inputting sunlight.
5) The three-dimensional photothermal conversion material prepared by the invention takes the three-dimensional foam as the substrate, can be recycled, has strong plasticity, can be suitable for use in various scenes, can realize high-efficiency evaporation of pure water, and can continuously and efficiently evaporate high-concentration saline water and wastewater.
6) According to the three-dimensional photothermal conversion material prepared by the invention, the carbonaceous material graphene oxide is selected as the photothermal converter, so that the sunlight absorption with high proportion can be realized, the hydrophilic melamine foam with high thermal insulation rate is compounded with the polymer electrolyte, the melamine foam with the hydrophilic property and the polymer electrolyte can ensure the sufficient supply of the water quantity of the three-dimensional photothermal conversion material, and meanwhile, the excellent thermal insulation property of the polystyrene foam can reduce the heat loss, so that more energy is used for the evaporation of water.
Drawings
FIG. 1 is a schematic view of a scanning electron microscope microstructure of a three-dimensional photothermal conversion material of the present invention at different magnifications;
fig. 2 is a schematic structural diagram of a multi-dimensional, multi-functional optical absorber obtained from the characterization results.
FIG. 3 is a graph showing the photothermal conversion rate and the treatment efficiency of the three-dimensional photothermal conversion material of the present invention for pure water (a) and saline water (b) of various concentrations;
FIG. 4 is a graph showing the effect of the three-dimensional photothermal conversion material of the present invention on the purification of seawater (a) and two different dye wastewaters (b);
FIG. 5 is a schematic view showing the structure of a photothermal conversion device according to the present invention;
the reference numbers in the figures are: 1 three-dimensional photothermal conversion material, 2 water absorbing layer, 3 thermal insulator, 4 first shell, 5 second shell.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and the detailed description. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
The invention provides a preparation method of a three-dimensional photothermal conversion material capable of efficiently treating salt water and wastewater, which comprises the following steps of preparing graphene oxide, preparing a charged graphene oxide compound, pretreating melamine foam, carrying the charged graphene oxide compound by the melamine foam through dipping and extrusion, and firmly integrating the compound and a melamine framework through heat treatment, wherein the preparation method comprises the following specific steps:
s1: and adjusting the pH value of the graphene oxide solution to 7-13 by using sodium hydroxide solutions with the concentrations of 0.1M and 0.05M respectively to obtain a solution A. In practice, the pH is preferably 12. And preparing the polymer electrolyte solution by selecting one of polyethyleneimine, polydiallyldimethylammonium chloride, polyallylamine hydrochloride, polystyrene sulfonate, polyacrylic acid or sodium alginate to obtain a solution B. In practical applications, the polymer electrolyte solution is preferably prepared by using a polyethyleneimine material. The molecular weight of the polymer electrolyte material is 1000-10000, wherein the preferred molecular weight is 10000.
The graphene oxide solution can be obtained by direct purchase or can be prepared by the following method:
s11: graphite flakes were added to a concentrated H containing 120mL at 80 deg.C2SO424.99g of K2S2O8And 24.99g of P2O5Keeping the solution in the solution for 4.5 hours to fully react,to obtain a mixed solution A.
S12: and rinsing the mixed solution A with deionized water until the pH of the eluate is neutral, and drying at 60 ℃ to obtain the pre-oxidized graphite.
S13: 30g of the powder of pre-oxidized graphite and 15g of sodium nitrate were put into 690mL of concentrated sulfuric acid at 0 ℃ to obtain a mixed cold solution. Then 90g of potassium permanganate is slowly added into the mixed cold solution which is vigorously stirred, and the temperature of the solution is kept to be lower than 4 ℃ in the process, so that mixed solution B is obtained.
S14: slowly pouring 1380mL of deionized water and 25mL of hydrogen peroxide solution with the mass fraction of 30% into the mixed solution B, fully reacting at 35 ℃, and keeping for 2 hours to obtain bright yellow mixed solution C.
S15: the mixture C was washed with a hydrochloric acid solution (10%, 10.8L) to remove residual sulfate ions, and then centrifuged at 8000 rpm to obtain concentrated graphene oxide, which was redispersed in deionized water and exfoliated again by sonication for 30 minutes. The above centrifugation and peeling operation is repeated a plurality of times (preferably three times) to obtain a mixed solution D.
S16: and dialyzing the mixed solution D, and soaking the mixed solution D by using deionized water to remove acid and other ions to obtain a graphene oxide solution (the concentration is preferably 3 mg/mL).
S2: mixing the following components in a solution A: and (3) dropwise adding the solution B into the solution A according to a concentration ratio of 3: 1-3: 12 (preferably 3:9), and carrying out sufficient reaction through ultrasound to obtain a charged graphene oxide compound solution.
S3: the melamine foam is washed by deionized water and absolute ethyl alcohol in sequence, repeated for a plurality of times and then placed in an oven at 60 ℃ for drying to obtain clean and dry melamine foam. The pretreated clean and dry melamine foam is immersed in the charged graphene oxide compound solution, and the melamine foam is immersed and extruded (namely, an immersion-extrusion method) to fully absorb the charged graphene oxide compound solution. And (3) placing the melamine foam with saturated adsorption in an oven with the temperature of 60-200 ℃ (preferably 100 ℃) for heat treatment for 6-24 hours, and cleaning and drying to obtain the three-dimensional photothermal conversion material.
As shown in fig. 1, which is a schematic view of the microstructure of the three-dimensional photothermal conversion material of the present invention, it can be seen that the three-dimensional porous connected skeleton of the melamine foam is maintained, and the compound formed by the graphene oxide and the polymer electrolyte is wrapped on the skeleton of the melamine. The graphene oxide and the polymer electrolyte are bonded by an electrostatic interaction force or the like, and the charged graphene oxide composite is bonded to the melamine skeleton by a van der waals force or the like.
Based on a unique multidimensional structure (as shown in FIG. 2), the designed light absorber has multiple properties, so that the light absorber has excellent solar desalination potential. First, the light absorber has excellent solar absorptance in the solar spectral range (96.7%). Macroscopically, the MF has an excellent multiple scattering effect. Scaling on the micro-scale, GO is a single layer covering the MF skeleton, so when sunlight is transmitted into the skeleton, GO will absorb most of the sunlight, the rest of the sunlight will be transmitted inside the 3D solar absorber, and then be fully absorbed. On a molecular scale, PEI is shaped like a brush, when sunlight hits the surface of PEI, on the one hand most of the sunlight will be transmitted to the GO layer, on the other hand the rest of the sunlight can be absorbed by multiple scattering effects due to the special morphology of PEI. Secondly, the transport of water is effective for the evaporation process. MF is hydrophilic and has a larger surface area than conventional solar absorbers, so that it can quickly replenish water lost by photothermal evaporation once it evaporates. Moreover, the brush-like shape of PEI facilitates the diffusion of water, so the heat generated by GO can be more easily transferred to the surrounding water molecules, enabling efficient and continuous operation of the evaporation process. Thirdly, the excellent thermal insulation properties of the three-dimensional optothermal converter result from the special arrangement of the components. The insulating MF and PEI surround the GO core, so heat can be efficiently transferred to the water film around the GO.
The invention provides a photothermal conversion device capable of efficiently treating brine and wastewater, which comprises a three-dimensional photothermal conversion material 1 prepared by the method, a water absorbing layer 2, a thermal insulator 3 and a reactor. The reactor comprises a first shell 4 and a second shell 5 which are transparent, the first shell 4 is sleeved outside the second shell 5, and a condensation cavity is formed between the first shell 4 and the second shell 5. The top of the second casing 5 is provided with a hole for the steam to evaporate from the inside of the second casing 5 into the condensation chamber. As shown in fig. 5, the top of the first casing 4 may be provided with a middle convex taper structure, so that the condensed steam flows down along the inner wall of the first casing 4, and does not drip into the first casing 4 again from the hole at the top of the second casing 5.
The bottom of the inner cavity of the second shell 5 is used for containing salt water or waste water, the heat insulator 3 is arranged above the water containing area in the second shell 5, the water absorbing layer 2 is arranged on the heat insulator 3, and the bottom end of the water absorbing layer 2 extends into the water containing area. In practical application, the water absorbing layer 2 can droop and fall into the water containing area from the periphery of the heat insulator 3, and holes can be formed in the heat insulator 3, so that the water absorbing layer 2 extends out of the holes of the heat insulator 3 and falls into the water containing area, and water in the water containing area can be conveyed to the top of the water absorbing layer 2 in time during use.
The three-dimensional photothermal conversion material 1 is placed on the water absorbing layer 2 and is in contact with the water absorbing layer 2 to absorb water in the water absorbing layer 2 and heat and evaporate the water into the condensation chamber. The three-dimensional photothermal conversion material 1 and the water containing region are separated by the thermal insulator 3, and heat exchange is reduced.
In practical application, the water absorption layer 2 can be set as a non-woven fabric for absorbing the water body to be treated in the water containing area and transferring the absorbed water body to the three-dimensional photothermal conversion material 1. The thermal insulator may be provided as a polystyrene foam to reduce the loss of conductive heat of the three-dimensional photothermal conversion material 1. The first case 4 and the second case 5 may be made of quartz.
The size of the three-dimensional photothermal conversion material can be flexibly adjusted and cut according to actual requirements, the size of the water-absorbing layer non-woven fabric is 6cm multiplied by 1mm, the size can be changed according to actual application scenes, and the size of the thermal insulation layer polystyrene foam is 5cm multiplied by 1cm, and can be changed according to actual requirements.
The method for treating the brine or the wastewater by using the photothermal conversion device comprises the following specific steps:
brine or wastewater to be treated is added to the water-containing area of the photothermal conversion device, the height of the brine or wastewater not exceeding the thermal insulator 3, and then the photothermal conversion device is placed under a light source. When light irradiates the three-dimensional photothermal conversion material 1, the light is subjected to a multi-scattering effect by the porous structure communicated with each other in the melamine foam, part of the light energy is absorbed by graphene oxide which is covered on the surface of the melamine foam and exists in a single layer or few layers, and the rest of the light is transmitted into the three-dimensional photothermal conversion material 1 and is absorbed after being scattered for multiple times. The graphene oxide absorbs light energy to generate heat, and the heat is limited on the surface of the graphene oxide by the thermal insulator 3 and the polymer electrolyte, so that the loss of heat is reduced. The saline water or the waste water is in contact with the three-dimensional photothermal conversion material 1 through the water absorption layer 2 and is attached to the melamine foam in the form of a film, heat generated by the graphene oxide is rapidly transferred to surrounding water molecules, and the water molecules in the form of the film rapidly absorb the heat and form steam, and the steam is evaporated from the pore channels of the melamine foam and overflows from the pore holes at the top of the second shell 5. The steam is condensed into liquid when meeting the top of the first shell 4 at normal temperature, and flows to the bottom along the conical top through the side wall to obtain purified water.
That is to say, the water absorbed by the water absorption layer is transferred to the surface of the light absorber graphene oxide through the porous three-dimensional skeleton melamine foam, and the heat energy converted by the graphene oxide is absorbed to generate heat exchange and generate steam. The vapor evaporates from the pores of the melamine foam and overflows from the pores at the top of the second shell 5, condenses into a liquid when encountering the top of the first shell 4 at normal temperature, and flows along the conical top through the side walls to the bottom. The saline water to be treated is subjected to photo-thermal evaporation to obtain clean water with ion removal rate superior to that of a distillation method and a membrane filtration method. Clear and transparent clean water can be obtained after the wastewater to be treated is subjected to solar photo-thermal treatment.
Example 1
In this embodiment, the photothermal conversion efficiency of the three-dimensional photothermal conversion material is evaluated as follows:
1) a certain volume of water is added into the water storage device, and a thermal insulator (polystyrene foam), a water absorbing layer (non-woven fabric) and a three-dimensional photothermal conversion material are sequentially arranged on the water storage device, namely the photothermal conversion efficiency evaluation simulation device is used.
2) The simulation device for evaluating the photo-thermal conversion efficiency of the simulated sunlight vertical irradiation records the change condition of the quality along with time through an online quality detection system, collects data to calculate the photo-thermal evaporation rate of unit area, normalizes the light energy input value, and calculates to obtain the photo-thermal conversion efficiency. The specific process is as follows:
firstly, carrying out a balance experiment for 1 hour under the condition of no light irradiation, recording the change conditions of temperature, humidity and moisture mass, and calculating the moisture mass change rate vi in unit time.
Secondly, the light power meter is used for calibrating the light intensity of the solar simulator to 1000W/m3Then, enabling the light spot to vertically irradiate the surface of the three-dimensional photothermal conversion material, recording the temperature and the humidity before and after irradiation, recording the mass change condition of water in real time through a computer connected with a balance, and calculating the water mass change rate vii in unit time;
and thirdly, the rate vi of the blank experiment group subtracted from the vii measured in the second step is the actual photo-thermal evaporation water rate under the light intensity irradiation, and the photo-thermal conversion efficiency of the three-dimensional photo-thermal conversion material can be calculated through a photo-thermal conversion efficiency formula.
In this embodiment, two sets of comparative experiments were also performed, the first set was to place no thermal insulator, no water-absorbing layer, and no three-dimensional photothermal conversion material, and only irradiate water in the water storage device, and the second set was to replace the three-dimensional photothermal conversion material with graphene oxide foam commonly used in the prior art.
The results are shown in FIG. 3, where the graph a shows pure water (H) under light irradiation2O), graphene oxide foam (GO @ MF), photothermal conversion rate and efficiency images of three-dimensional photothermal conversion material (PEI @ GO @ MF). As can be seen from the figure, the photothermal conversion rate of the three-dimensional photothermal conversion material is up to 1.394 kg/(m) compared with pure water and graphene oxide foam2H) the efficiency was 93.4%. b is a chart of photothermal conversion rate and efficiency of brine with four different concentrations from low to high by using the three-dimensional photothermal conversion material. It can be seen that the three-dimensional photothermal conversion material increases with the concentration of the salt solutionThe photothermal conversion rate and efficiency are well maintained, and at nearly saturated brine concentration, the efficiency is still higher than 80%.
Example 2
The method comprises the following steps: the pH of 19.5mL of a 7.7mg/mL graphene oxide solution was adjusted to 12 to give solution A. And preparing a polymer electrolyte solution with the concentration of 15mg/mL by using polyethyleneimine to obtain a solution B.
Dropwise adding the solution B into the solution A to enable the ratio of graphene oxide to POLYMER electrolyte (GO: POLYMER) to be 3: 1-3: 12, filling the rest volume with distilled water, and intensively shaking or ultrasonically mixing the solution uniformly to obtain a charged graphene oxide compound solution.
Step two: the block melamine foam was cut into a 4cm × 4cm × 1cm rectangular parallelepiped (example), and was immersed and extruded several times in water and ethanol, after which it was dried overnight in a 60-degree oven to obtain a clean and dry foam.
Step three: weighing the mass of clean and dry foam, selecting the foam with similar mass, respectively soaking the foam in a solution of GO, POLYMER, 3:1, 3:3, 3:6, 3:9 and 3:12, fully absorbing the soaking liquid by the foam through extrusion-soaking, and then respectively placing the foam soaked in different GO, POLYMER proportions in ovens at 60, 80, 100, 120, 140, 160, 180 and 200 ℃ for heat treatment to obtain the composite melamine foam.
Step four: washing the composite melamine foam with water and alcohol to remove the charged graphene oxide compound with the surface not fully reacted;
step five: placing the melamine foam subjected to water washing and alcohol washing in an oven to be dried overnight to obtain three-dimensional photothermal conversion materials with different GO to POLYMER ratios and heat treatment temperatures, and numbering for use;
step six: the photothermal conversion efficiency evaluation simulation device in embodiment 1 is used to evaluate three-dimensional photothermal conversion materials with different GO to POLYMER ratios and heat treatment temperatures, so as to preferably select the optimal GO to POLYMER ratio and heat treatment temperature.
The result shows that the three-dimensional photothermal conversion material with the ratio of GO to POLYMER being 3:9 and the heat treatment temperature being 100 ℃ has the best effect.
Step seven: the three-dimensional photothermal conversion material having the best effect obtained by the sixth step was placed in the photothermal conversion device, and the effect thereof was evaluated by treating seawater and sewage of various concentrations.
Step eight: and (5) collecting the steam condensate water in the step seven, and determining the change of the concentration of main ions in the seawater and the change of the concentration of pollutants in the sewage before and after the photothermal conversion by using an inductively coupled plasma mass spectrometry and an ultraviolet-visible spectrophotometry. The results are shown in fig. 4 and table 1, from which it can be seen that the removal rate of the main ions in the seawater and the organic matters in the sewage is more than 99% after the photo-thermal treatment.
TABLE 1 actual treatment effect of seawater desalination/sewage purification
Example 3
A method for preparing a three-dimensional photothermal conversion body was conducted as in example 2 by forming a 5mm by 5mm rectangular small opening in the photothermal conversion body with a circular cutter, and treating 20 wt% of simulated seawater with an intermediate water supply system at an illumination intensity of 1 kw.m2。
The result shows that the evaporation water rate and the photothermal conversion efficiency of the three-dimensional photothermal converter continuously run for 12 hours are not reduced, salt crystallization mainly occurs at the edge of the light absorber, and the salt crystallization gradually generates and grows up along with the prolonging of the illumination time and finally leaves the light absorber.
TABLE 2 actual treatment effect of light absorber of intermediate water supply on high concentration seawater
The example results show that the three-dimensional photothermal conversion material synthesized by using graphene oxide, polymer electrolyte and melamine foam has excellent light absorption and good insulating property, and can efficiently convert sunlight into heat. The excellent hydrophilic performance and the unique pore structure of the synthesized composite foam enable water to exist on the surface of the composite foam in a film form, can rapidly receive heat generated by graphene oxide, and is subjected to phase change to form steam, and then the steam escapes from the photothermal converter rapidly through a loose and porous structure of a melamine foam framework, so that the efficient and stable purification of low-to-high-concentration seawater and sewage is realized.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (9)
1. A preparation method of a three-dimensional photothermal conversion material capable of efficiently treating saline water and wastewater is characterized by comprising the following steps:
s1: adjusting the pH value of the graphene oxide solution to 12 to obtain a solution A; preparing a polymer electrolyte solution to obtain a solution B;
s2: mixing the following components in a solution A: dropwise adding the solution B into the solution A according to a concentration ratio of 3: 1-3: 12, and carrying out sufficient reaction through ultrasound to obtain a charged graphene oxide compound solution;
s3: immersing the pretreated clean and dry melamine foam into the charged graphene oxide compound solution, and immersing and extruding the melamine foam to enable the melamine foam to fully absorb the charged graphene oxide compound solution; and (3) placing the melamine foam with saturated adsorption in a drying oven at the temperature of 60-200 ℃ for heat treatment for 6-24 hours, and cleaning and drying to obtain the three-dimensional photo-thermal conversion material.
2. The method for preparing a three-dimensional photothermal conversion material according to claim 1, wherein the concentration of the graphene oxide solution in S1 is 3 mg/mL.
3. The method for preparing the three-dimensional photothermal conversion material according to claim 1, wherein the polymer electrolyte is one of polyethyleneimine, polydiallyldimethylammonium chloride, polyallylamine hydrochloride, polystyrene sulfonate, polyacrylic acid, or sodium alginate.
4. The method for producing a three-dimensional photothermal conversion material according to claim 1, wherein the mixing concentration ratio of the solution a and the solution B in S2 is 3: 9.
5. The method for preparing the three-dimensional photothermal conversion material according to claim 1, wherein the pretreatment process of the melamine foam in S3 is as follows: the melamine foam was washed with deionized water and absolute ethanol in this order, repeated several times, and then dried in an oven at 100 ℃.
6. A three-dimensional photothermal conversion material produced by the production method according to any one of claims 1 to 5.
7. A photothermal conversion device capable of efficiently treating brine and wastewater, comprising the three-dimensional photothermal conversion material (1) according to claim 6, a water absorbing layer (2), a thermal insulator (3), and a reactor;
the reactor comprises a first shell (4) and a second shell (5) which are transparent, the first shell (4) is sleeved outside the second shell (5) with a hole at the top, and a condensation cavity is formed between the first shell and the second shell;
the bottom of the second shell (5) is used for containing brine or wastewater, the thermal insulator (3) is arranged above a water containing area in the second shell (5), a water absorbing layer (2) is arranged on the thermal insulator (3), and the bottom end of the water absorbing layer (2) extends into the water containing area; the three-dimensional photothermal conversion material (1) is placed on the water absorption layer (2) in a contact mode to absorb water in the water absorption layer (2) and heat and evaporate the water into the condensation cavity; the three-dimensional photothermal conversion material (1) and the water containing area are separated by a thermal insulator (3), and heat exchange is reduced.
8. The photothermal conversion device according to claim 7, wherein the water absorbing layer (2) is a nonwoven fabric, the thermal insulator is polystyrene foam, and the first housing (4) and the second housing (5) are made of quartz.
9. A method for treating brine or wastewater based on the photothermal conversion device according to claim 7 or 8, which comprises the following steps:
adding brine or wastewater to be treated to a water-containing region of a photothermal conversion device, followed by placing the photothermal conversion device under a light source;
when light irradiates the three-dimensional photothermal conversion material (1), the light is subjected to a multi-scattering effect through the porous structure communicated with each other in the melamine foam, part of the light energy is absorbed by graphene oxide which is covered on the surface of the melamine foam and exists in a single-layer or few-layer form, and the rest of the light is transmitted into the three-dimensional photothermal conversion material (1) and is absorbed after being scattered for multiple times; the graphene oxide absorbs light energy to generate heat, and the heat is limited on the surface of the graphene oxide by a thermal insulator (3) and a polymer electrolyte so as to reduce the loss of heat;
saline water or wastewater is in contact with the three-dimensional photothermal conversion material (1) through the water absorption layer (2) and is attached to the melamine foam in a film form, heat generated by graphene oxide is rapidly transferred to surrounding water molecules, the water molecules existing in the film form rapidly absorb the heat and form steam, and the steam is evaporated from pore channels of the melamine foam and overflows from pores at the top of the second shell (5); the steam is condensed into liquid when meeting the top of the first shell (4) at normal temperature, and flows to the bottom along the inner wall of the first shell (4), so that the purification of the salt water or the waste water is realized, and the purified water is obtained.
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