CN114804272B - Wood-like blackbody material and preparation method and application thereof - Google Patents

Wood-like blackbody material and preparation method and application thereof Download PDF

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CN114804272B
CN114804272B CN202210459468.1A CN202210459468A CN114804272B CN 114804272 B CN114804272 B CN 114804272B CN 202210459468 A CN202210459468 A CN 202210459468A CN 114804272 B CN114804272 B CN 114804272B
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wood
blackbody
carboxymethyl cellulose
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sodium alginate
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CN114804272A (en
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俞书宏
赵浩雨
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University of Science and Technology of China USTC
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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
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)

Abstract

The invention provides a preparation method of a simulated wood blackbody material, which develops the simulated wood material with an artificial asymmetric structure and an oriented nano structure by an ice template method. The invention provides a wood-like blackbody material, which comprises: the polypyrrole-carboxymethyl cellulose-alginate composite material (CCAP) and calcium-cured carboxymethyl cellulose/sodium alginate composite material (CCA) have a double-layer structure, and the CCAP layer contains black polypyrrole, so that the solar energy absorptivity can be effectively improved, and the evaporation enthalpy of interfacial water can be reduced; the CCA layer is a hydrophilic polyhydroxy macroporous structure, and not only has equivalent water transmission capacity and salt tolerance capacity, but also is an excellent heavy metal capturing agent. In addition, all precursors of the artificial asymmetric structure wood material provided by the invention are biomass, so that the influence on the water ecological environment is ensured to be minimum in the regeneration process of the metal ion removing drinking water. The invention also provides application of the wood-like blackbody material.

Description

Wood-like blackbody material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photo-thermal conversion water evaporation, and particularly relates to a wood-like blackbody material, a preparation method and application thereof, in particular to preparation of a blackbody material with efficient photo-thermal conversion and hydrophilic-hydrophobic interface treatment of the material.
Background
With population growth, urbanization and socioeconomic development, water shortage conditions occur in different degrees in more than 100 countries. The reason for the lack of water is mainly three aspects, one is that more than 97% of water on the surface of the earth is high-salinity seawater which cannot be directly utilized; secondly, along with the rapid development of industry, 2.5% of surface fresh water faces various pollution problems, such as mine pollution, domestic sewage and the like; thirdly, the problem of water resource shortage is aggravated by unbalanced water resource distribution. With the rise of the interface photothermal conversion (ISSG) technology, seawater and sewage can be purified with little energy consumption and carbon footprint, and the method has wide industrialized prospect.
Methods for achieving desalination of sea water are diverse, such as continuous microfiltration technology, reverse osmosis technology, etc., which can naturally alleviate the problem of water shortage, but are not universal because not all water-deficient areas are coastal. The ideal goal of future wastewater treatment is to trend toward low energy consumption, while the reported hydrogel technology has been able to reduce the concentration of heavy metal ions in water by 7 orders of magnitude to meet the need for potable fresh water, no expansion has been made in terms of environmental protection and efficient heavy metal enrichment while producing healthy drinking water.
The main stream blackbody material at present mainly comprises a black polymer, a plasmon and a carbon-based absorbent, and although the black polymer, the plasmon and the carbon-based absorbent can realize the photo-thermal conversion efficiency of 95 percent, the swelling behavior of the polymer ensures that the polymer has poor drought resistance; the plasma absorber morphology is easily destroyed and challenges remain for practical photo-thermal water evaporation. Although carbon-based absorbers have the remarkable characteristics of natural broadband solar energy absorption, resistance to hot acid/base and ultraviolet light, and excellent heat conversion properties, they are considered as one of the optimal candidates for efficient photothermal conversion water evaporation; moreover, economy, sustainability and good processing characteristics lend themselves to wide-ranging applications. However, the inherent hydrophobicity and poor thermal insulation properties of carbon-based materials are not suitable for water transport and efficient thermal management, and although hydrophilicity can be achieved by surface modification or doping to induce heteroatoms, the introduction of other materials inevitably affects the tolerance of the carbon-based system.
Disclosure of Invention
In view of the above, the invention aims to provide a wood-like blackbody material, and a preparation method and application thereof.
The invention provides a wood-like blackbody material, which comprises:
a layer of calcified polypyrrole-carboxymethyl cellulose-alginate composite material;
calcified carboxymethyl cellulose-sodium alginate composite material layer.
Preferably, the wood-like blackbody material has a solar energy absorption capacity of 96-99%, a saturation capacity ratio of 18-22, and a heat transfer coefficient of 30-35 mW.m -1 ·K -1 The interfacial water evaporation enthalpy is 1450-1500 J.g -1 。
The invention provides a preparation method of a wood-like blackbody material, which comprises the following steps:
freezing and casting the mixed solution of carboxymethyl cellulose and sodium alginate to obtain a composite material;
reacting a mixed solution of sodium alginate and carboxymethyl cellulose, polypyrrole and ammonium persulfate to obtain a reaction product;
the reaction product and the composite material are compounded and then dried to obtain an intermediate product;
and calcification is carried out on the intermediate product, so that the simulated wood blackbody material is obtained.
Preferably, the method of freeze casting comprises:
arranging a mould on the copper sheet, and pouring the mixed solution of the carboxymethyl cellulose and the sodium alginate into the mould;
and (3) placing the copper block into liquid nitrogen, and placing the die on the copper block to obtain the composite material.
Preferably, the compounding method comprises:
pouring the reaction product into a mould filled with the composite material for solidification.
Preferably, the method of calcification comprises:
soaking the intermediate product in CaCl 2 And (5) after the solution is in solution, drying the solution to obtain the wood-like blackbody material.
The invention provides a metal recovery enrichment device, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The invention provides a sewage regeneration device, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The invention provides a heavy metal wastewater treatment device, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The invention provides a solar seawater desalination evaporator, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
In order to improve the photo-thermal conversion efficiency and the vapor aggregation rate, the prior studies have often been focused on changing the composition of the materials used, and there is little research on the engineering of nanostructures. The invention reasonably designs the nano structure by combining with ISSG technology, and has very important significance for improving the photo-thermal conversion efficiency and simultaneously removing heavy metal impurity ions and producing healthy drinking water. The natural plants have a directional parallel structure, and can enrich nutrient ions in soil in the photosynthesis and transpiration processes. The invention is inspired by the invention, and provides an artificial biocompatible asymmetric structure wood evaporator which can realize a large amount of metal ion enrichment during ISSG. The invention provides a preparation method of an enrichment recovery metal ion simulated wood blackbody material inspired by plant photosynthesis and transpiration mechanisms, and provides application advantages of the material in aspects of sewage purification and the like. The invention is inspired by the nanostructure arrangement of the nutrient ions in the natural plant physiological effect enriched soil, and an artificial double-sided structure simulated wood blackbody material with a directional nanostructure is provided for the first time by utilizing an ice template method so as to convey the water in the sewage and enrich the heavy metal ions in the sewage.
The invention is inspired by the nano structure arrangement of enriching nutrient ions in soil in the plant transpiration effect, and provides an artificial asymmetric structure wood-like material with a directional nano structure by an ice template method, which has a double-layer structure of polypyrrole-carboxymethyl cellulose-alginate composite material (CCAP) and calcium-solidified carboxymethyl cellulose/sodium alginate composite material (CCA); the CCAP layer contains black polypyrrole, so that the solar absorptivity can be effectively improved, and the evaporation enthalpy of interfacial water can be reduced; the CCA layer is of a hydrophilic polyhydroxy macroporous structure, not only has water transmission capability and salt tolerance capability, but also is an excellent heavy metal capturing agent, salt water or sewage is conveyed to an evaporation interface through solar energy and undergoes a phase change process, as is performed by leaves, fresh water regeneration is realized through condensed steam, and when water is evaporated, ions in water are enriched into the CCA layer of the artificial wood, as is the absorption of nutrient elements from soil by roots. In addition, all precursors of the artificial asymmetric structure wood material provided by the invention are biomass, so that the influence on the water ecological environment is ensured to be minimum in the regeneration process of the metal ion removing drinking water.
The blackbody material provided by the invention has excellent solar energy absorption capacity (98%), hydrophilicity and heat management performance (lambda=32.8 mW.m) -1 ·K -1 ) And low enthalpy of water evaporation (1475 J.g -1 ) And can reach 2.3 kg.m under 1 unit of solar irradiation -2 ·h -1 Since its macroporous super-hydrophilic skeleton is sufficient for water transport and spontaneous salt diffusion, it can exhibit excellent long-term evaporation stability and less performance decay in a metal solution. The wood-like blackbody material prepared by the invention provides a new thought for enriching heavy metals in the construction process of the high-performance solar seawater desalination evaporator, and has important significance for various applications including sewage regeneration and heavy metal wastewater treatment.
Drawings
FIG. 1 is a schematic diagram of an application principle of a simulated wood blackbody material provided by the invention;
FIG. 2 is a schematic diagram of a structure of a simulated wood blackbody material useful for metal recovery enrichment according to an embodiment of the present invention;
FIG. 3 is a physical diagram of the simulated wood blackbody material prepared in example 1 of the present invention;
FIG. 4 is an SEM image of the preparation of a simulated wood black body material according to example 1 of the present invention;
FIG. 5 is an XPS energy spectrum of the simulated wood black body material prepared in example 1 of the present invention;
FIG. 6 is a graph showing the time-dependent water contact angle performance of the simulated wood blackbody material prepared in example 1 of the present invention;
FIG. 7 is a FT-IR absorption spectrum of a wood-like blackbody material prepared in example 1 of the present invention;
FIG. 8 is a real-time environmental chart of the performance test of the simulated wood blackbody material prepared in example 1 of the present invention;
FIG. 9 shows the light absorptivity of the simulated wood black body material of example 1 of the present invention in the wavelength range of 250-2500 nm;
FIG. 10 is a graph showing the surface temperature of the simulated wood black body material prepared in example 1 of the present invention when it is immersed in water under 1 unit of sunlight;
FIG. 11 is a graph showing the comparison of the adsorption of metal ions during the evaporation of the simulated wood blackbody material prepared in example 1 of the present invention;
fig. 12 is a graph showing comparison of stability in water of the simulated wood blackbody materials (CAPs) prepared in examples 1, 2 and 3 of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a wood-like blackbody material, which comprises:
a layer of calcified polypyrrole-carboxymethyl cellulose-alginate composite material;
calcified carboxymethyl cellulose-sodium alginate composite material layer.
In the invention, the calcified polypyrrole-carboxymethyl cellulose-alginate composite material layer is arranged on the surface of the calcified carboxymethyl cellulose-sodium alginate composite material layer, the calcified polypyrrole-carboxymethyl cellulose-alginate composite material layer is an upper layer, the calcified carboxymethyl cellulose-sodium alginate composite material layer is a lower layer, and the calcified carboxymethyl cellulose-sodium alginate composite material layer contains cage complex formed after calcification. The schematic structural diagram of the simulated wood blackbody material provided by the embodiment of the invention is shown in fig. 2, wherein 1 is the simulated wood blackbody material inspired by plant physiological action and used for metal recovery and enrichment, 2 is a sodium alginate-carboxymethyl cellulose-polypyrrole composite material layer on the upper layer of the simulated wood material, 3 is a sodium alginate-carboxymethyl cellulose composite material layer on the lower layer of the simulated wood material, and 4 is a cage complex formed after calcification.
The invention provides a preparation method of a wood-like blackbody material, which comprises the following steps:
freezing and casting the mixed solution of carboxymethyl cellulose and sodium alginate to obtain a composite material;
reacting a mixed solution of sodium alginate and carboxymethyl cellulose, polypyrrole and ammonium persulfate to obtain a reaction product;
the reaction product and the composite material are compounded and then dried to obtain an intermediate product;
and calcification is carried out on the intermediate product, so that the simulated wood blackbody material is obtained.
The invention provides a preparation method of a simulated wood blackbody material for metal recovery and enrichment, which comprises the steps of firstly, freezing and casting a mixed solution of carboxymethyl cellulose and sodium alginate on flat copper to prefabricate a parallel channel structure similar to wood; then adding polypyrrole into the mixed solution of sodium alginate and carboxymethyl cellulose, oxidizing with ammonium persulfate, and covering the mixture on the carboxymethyl cellulose/sodium alginate composite material; then freeze-drying the obtained sample in a cold trap at-50 ℃; and finally, forming a cage complex by utilizing calcium ions in the alcohol phase and sodium alginate to crosslink a molecular network, so that the stability of the material in water is improved, and the material is prevented from being dissolved in the water. According to the invention, by utilizing an ice template method, a mixed solution of carboxymethyl cellulose and sodium alginate is frozen and cast on a copper flat plate to form a parallel channel structure of the wood-like structure; oxidizing white polypyrrole into black by utilizing the oxidizing property of ammonium persulfate; and (3) exchanging calcium ions in the alcohol solution with sodium ions in the sodium alginate by utilizing an ion exchange technology, so as to form a cage-shaped compound. The oriented parallel structure of the invention not only can effectively convey moisture, but also has the function of enriching metal ions.
In the present invention, the preparation method of the mixed solution of carboxymethyl cellulose and sodium alginate preferably comprises the following steps:
dissolving carboxymethyl cellulose powder and sodium alginate powder in water, stirring, and removing bubbles to obtain mixed solution (CA solution) of carboxymethyl cellulose and sodium alginate.
In the present invention, the water is preferably deionized water.
In the invention, the mass ratio of the carboxymethyl cellulose to the sodium alginate is preferably (0.5-2.0): 1, more preferably (1 to 1.5): 1, most preferably 1:1, a step of; the ratio of the carboxymethyl cellulose to the water is preferably (0.5-2.0) g:100mL, more preferably (1 to 1.5) g:100mL, most preferably 1g:100mL.
In the present invention, the stirring time is preferably 2 to 4 hours, more preferably 2.5 to 3.5 hours, and most preferably 3 hours.
In the present invention, the method of removing bubbles is preferably vacuum treatment.
In the present invention, the method of freeze casting preferably comprises:
arranging a mould on the copper sheet, and pouring the mixed solution of the carboxymethyl cellulose and the sodium alginate into the mould;
the copper block was placed in liquid nitrogen and the mold was placed on the copper block to obtain a wood-like parallel channel structure (composite).
In the present invention, the mold is preferably a polydimethylsiloxane mold.
In the present invention, it is preferable to pour a mixed solution of carboxymethyl cellulose and sodium alginate into 1/2 of the volume of the mold.
In the present invention, the copper block is preferably immersed in liquid nitrogen at a lower portion and exposed to air at an upper portion; the liquid nitrogen is preferably placed in an insulated open container.
In the present invention, the method of freeze casting more preferably comprises:
pouring liquid nitrogen into an insulated open container, putting a copper block, immersing the lower part of the copper block in the liquid nitrogen, and exposing the upper part of the copper block to air;
taking a copper sheet, placing a polydimethylsiloxane mould on the upper part of the copper sheet, pouring a CA solution with half the volume of the mould, and placing the copper sheet on a copper block in liquid nitrogen; after the solution solidifies, a parallel channel structure resembling wood is obtained.
In the present invention, the method of the reaction preferably comprises:
firstly mixing a mixed solution of sodium alginate and carboxymethyl cellulose with polypyrrole to obtain a mixed solution;
and (3) carrying out second mixing on the mixed solution and the ammonium persulfate solution to obtain a reaction product (CAP black solution).
In the present invention, the preparation method of the mixed solution of sodium alginate and carboxymethyl cellulose is the same as the preparation method of the mixed solution of carboxymethyl cellulose and sodium alginate in the above technical scheme, and will not be described herein.
In the invention, the volume ratio of the mixed solution of sodium alginate and carboxymethyl cellulose to polypyrrole is preferably (40-60): (1-2), more preferably (45-55): (1.3 to 1.7), most preferably 50:1.5.
in the present invention, the first mixing is preferably performed under stirring for a period of time of preferably 0.3 to 0.7 hours, more preferably 0.4 to 0.6 hours, and most preferably 0.5 hours.
In the present invention, the preparation method of the ammonium persulfate solution preferably includes:
and mixing ammonium persulfate with water to obtain an ammonium persulfate solution.
In the present invention, the water is preferably deionized water.
In the present invention, the ratio of the ammonium persulfate to water is preferably (0.2 to 0.6) g: (8-12) mL, more preferably (0.3-0.5) g: (9-11) mL, most preferably 0.4g:10mL.
In the invention, the dosage ratio of the mixed solution of sodium alginate and carboxymethyl cellulose to ammonium persulfate is preferably (40-60) mL: (0.2 to 0.6) g, more preferably (45 to 55) mL: (0.3 to 0.5) g, most preferably 50mL:0.4g.
In the present invention, the second mixing is preferably performed under stirring; the stirring time is preferably 2 to 4 hours, more preferably 2.5 to 3.5 hours, most preferably 3 hours, until no lump gel is present in the solution.
In the present invention, the second mixing preferably further comprises:
and carrying out vacuum treatment on the obtained product to remove bubbles, thereby obtaining the CAP black solution.
In the present invention, the compounding method preferably includes:
pouring the reaction product into a mould filled with the composite material for solidification.
In the present invention, the compounding method more preferably includes:
and pouring CAP solution into the solidified CA in the polydimethylsiloxane mould, and drying after the solution is completely solidified to obtain an intermediate product (the two-sided structure wood-like material).
In the present invention, the reaction product is preferably 1/2 of the volume of the above-mentioned mold.
In the present invention, the drying is preferably freeze-drying, and the drying time is preferably longer than 4 days; the drying temperature is preferably-40 to-60 ℃, more preferably-45 to-55 ℃, and most preferably-50 ℃.
In the present invention, the method of calcification preferably comprises:
soaking the intermediate product in CaCl 2 And after the solution is in solution, drying is carried out to obtain the wood-like blackbody material (the cage complex of the two-sided structural material).
In the present invention, the CaCl 2 The solution is preferably CaCl 2 An ethanol solution; the CaCl 2 The preparation method of the solution preferably comprises the following steps:
CaCl is added with 2 The powder was dissolved in ethanol.
In the present invention, the ethanol is preferably absolute ethanol.
In the present invention, the CaCl 2 And ethanol is preferably used in a proportion of (4 to 5) g: (180-220) mL, more preferably (4.2-4.8) g: (190-210) mL, most preferably 4.44g:200mL.
In the present invention, the soaking time is preferably more than 2 days.
In the present invention, the drying temperature is preferably 70 to 90 ℃, more preferably 75 to 85 ℃, and most preferably 80 ℃; the drying is preferably overnight to give a cage complex of the two-sided structured material.
The interface photo-thermal conversion water evaporation blackbody material is prepared by the following method: firstly, freezing and casting a mixed solution of carboxymethyl cellulose and sodium alginate on flat copper to prefabricate a parallel channel structure similar to wood; then adding polypyrrole into the mixed solution of sodium alginate and carboxymethyl cellulose, oxidizing with ammonium persulfate to obtain a black solution, and covering the black solution on the carboxymethyl cellulose/sodium alginate composite material to obtain a material with a two-sided structure; all samples were then freeze dried in a cold trap at-50 ℃; and finally, forming a cage complex by utilizing calcium ions in the alcohol phase and sodium alginate to crosslink a molecular network, so that the stability of the material in water is improved, and the material is prevented from being dissolved in the water.
The invention provides a metal recovery enrichment device, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The invention provides a sewage regeneration device, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The invention provides a heavy metal wastewater treatment device, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The invention provides a solar seawater desalination evaporator, which comprises: the wood-like blackbody material according to the above technical scheme, or the wood-like blackbody material prepared by the method according to the above technical scheme.
The application schematic diagram of the wood-like blackbody material provided by the invention is shown in figure 1.
The wood-like blackbody material based on plant physiological function inspired by the invention and capable of being used for metal recovery and enrichment has excellent solar energy absorption capacity (98%), hydrophilicity (saturation capacity ratio is 19.2) and heat management performance (lambda=32.8 mW.m) -1 ·K -1 ) The method comprises the steps of carrying out a first treatment on the surface of the Has high steam regeneration rate; exhibit good evaporation stability and less performance decay over a long period of time in a metal solution; has low interfacial water evaporation enthalpy (1475 J.g) -1 ) The water evaporation process with higher efficiency can be realized.
Example 1
1.0g of sodium alginate powder and 1.0g of carboxymethyl cellulose powder are taken and dissolved in 100mL of deionized water, stirred for 3h, and then the solution is subjected to vacuum treatment to remove bubbles, thus obtaining CA solution. Pouring liquid nitrogen into an insulated open container, putting a copper block, immersing the lower part of the copper block in the liquid nitrogen, and exposing the upper part of the copper block to air; taking a copper sheet, placing a polydimethylsiloxane mould on the upper part of the copper sheet, pouring a CA solution with half the volume of the mould, and placing the copper sheet on a copper block in liquid nitrogen; after the solution solidifies, a parallel channel structure resembling wood is obtained.
Taking 50mL of CA solution (the preparation method is the same as above), adding 1.5mL of polypyrrole, and stirring for 0.5h; adding 0.4g of ammonium persulfate into 10mL of deionized water, adding the obtained ammonium persulfate solution into the CA solution, and stirring for 3 hours until massive gel does not exist in the solution; and (3) carrying out vacuum treatment on the solution to remove bubbles, thereby obtaining the CAP black solution.
And pouring CAP solution (1/2 volume remained) into the solidified CA in the polydimethylsiloxane mould, and freeze-drying (50 ℃ below zero) for more than 4 days after the solution is completely solidified to obtain the wood-like material with the double-sided structure.
4.44g CaCl was taken 2 Powder, dissolved in 200mL absolute ethanol; soaking the two-sided structure wood-like material in CaCl 2 The cage complex of the two-sided structure material (simulated wood blackbody material) was obtained in ethanol solution for more than 2 days, followed by drying overnight at 80 ℃.
Fig. 3 is a physical diagram of the simulated wood blackbody material prepared in example 1, wherein in the left diagram, the upper part is sodium alginate/carboxymethyl cellulose solution, sodium alginate/carboxymethyl cellulose/polypyrrole solution before oxidation, sodium alginate/carboxymethyl cellulose/polypyrrole solution after oxidation, the lower part is a double-layer simulated wood material, the upper layer is a sodium alginate-carboxymethyl cellulose-polypyrrole composite layer, and the lower part is a sodium alginate-carboxymethyl cellulose layer; in the right graph, the upper part is a sodium alginate-carboxymethyl cellulose composite layer before calcification, a sodium alginate-carboxymethyl cellulose-polypyrrole composite layer before calcification, and the lower part is a sodium alginate-carboxymethyl cellulose composite layer after calcification and a sodium alginate-carboxymethyl cellulose-polypyrrole composite layer after calcification.
Fig. 4 is an SEM image of the wood-like material prepared in example 1, the left image is a calcified sodium alginate-carboxymethyl cellulose composite layer, the right image is a calcified sodium alginate-carboxymethyl cellulose-polypyrrole composite layer, and the middle image is an interface between the two layers.
Fig. 5 is an XPS spectrum of the simulated wood blackbody material prepared in example 1, and it can be seen that polypyrrole exists in the sodium alginate-carboxymethyl cellulose-polypyrrole composite layer, and calcification of both the sodium alginate-carboxymethyl cellulose composite layer and the sodium alginate-carboxymethyl cellulose-polypyrrole composite layer acts on the position of calcium alginate.
Fig. 7 is an FT-IR absorption spectrum of the simulated wood blackbody material prepared in example 1, wherein four absorption spectra are, in order from top to bottom, a sodium alginate-carboxymethyl cellulose composite layer before calcification, a sodium alginate-carboxymethyl cellulose-polypyrrole composite layer before calcification, a sodium alginate-carboxymethyl cellulose composite layer after calcification, and a sodium alginate-carboxymethyl cellulose-polypyrrole composite layer after calcification.
Example 2
2.0g of sodium alginate powder and 1.0g of carboxymethyl cellulose powder are taken and dissolved in 100mL of deionized water, stirred for 3h, and then the solution is subjected to vacuum treatment to remove bubbles, thus obtaining CA solution. Pouring liquid nitrogen into an insulated open container, putting a copper block, immersing the lower part of the copper block in the liquid nitrogen, and exposing the upper part of the copper block to air; taking a copper sheet, placing a polydimethylsiloxane mould on the upper part of the copper sheet, pouring a CA solution with half the volume of the mould, and placing the copper sheet on a copper block in liquid nitrogen; after the solution solidifies, a parallel channel structure resembling wood is obtained.
Taking 50mL of CA solution (the preparation method is the same as above), adding 1.5mL of polypyrrole, and stirring for 0.5h; adding 0.4g of ammonium persulfate into 10mL of deionized water, adding the obtained ammonium persulfate solution into the CA solution, and stirring for 3 hours until massive gel does not exist in the solution; and (3) carrying out vacuum treatment on the solution to remove bubbles, thereby obtaining the CAP black solution.
And pouring CAP solution (1/2 volume remained) into the solidified CA in the polydimethylsiloxane mould, and freeze-drying (50 ℃ below zero) for more than 4 days after the solution is completely solidified to obtain the wood-like material with the double-sided structure.
4.44g CaCl was taken 2 Powder, dissolved in 200mL absolute ethanol; soaking the two-sided structure wood-like material in CaCl 2 The cage complex of the two-sided structure material (simulated wood blackbody material) was obtained in ethanol solution for more than 2 days, followed by drying overnight at 80 ℃.
Example 3
1.0g of sodium alginate powder and 2.0g of carboxymethyl cellulose powder are taken and dissolved in 100mL of deionized water, stirred for 3h, and then the solution is subjected to vacuum treatment to remove bubbles, thus obtaining CA solution. Pouring liquid nitrogen into an insulated open container, putting a copper block, immersing the lower part of the copper block in the liquid nitrogen, and exposing the upper part of the copper block to air; taking a copper sheet, placing a polydimethylsiloxane mould on the upper part of the copper sheet, pouring a CA solution with half the volume of the mould, and placing the copper sheet on a copper block in liquid nitrogen; after the solution solidifies, a parallel channel structure resembling wood is obtained.
Taking 50mL of CA solution (the preparation method is the same as above), adding 1.5mL of polypyrrole, and stirring for 0.5h; adding 0.4g of ammonium persulfate into 10mL of deionized water, adding the obtained ammonium persulfate solution into the CA solution, and stirring for 3 hours until massive gel does not exist in the solution; and (3) carrying out vacuum treatment on the solution to remove bubbles, thereby obtaining the CAP black solution.
And pouring CAP solution (1/2 volume remained) into the solidified CA in the polydimethylsiloxane mould, and freeze-drying (50 ℃ below zero) for more than 4 days after the solution is completely solidified to obtain the wood-like material with the double-sided structure.
4.44g CaCl was taken 2 Powder, dissolved in 200mL absolute ethanol; soaking the two-sided structure wood-like material in CaCl 2 The cage complex of the two-sided structure material (simulated wood blackbody material) was obtained in ethanol solution for more than 2 days, followed by drying overnight at 80 ℃.
Performance detection
The water contact angle of the simulated wood blackbody material prepared by the embodiment of the invention is detected, the contact angle of the dropped liquid drop is recorded in real time by using a Dataphysics OCA 25 device, and the detection result is as follows: the water contact angle test results of the simulated wood blackbody material prepared in example 1 are shown in fig. 6, and it can be seen that all the materials are super-hydrophilic materials, and the hydrophilicity of the calcified materials is slightly improved. The simulated wood blackbody materials prepared in example 2 and example 3 each have a water contact angle of 0 °, i.e. are super hydrophilic.
The interface photo-thermal conversion performance of the simulated wood blackbody material prepared by the embodiment of the invention is detected, the performance test environment is shown as figure 8, and the test method of the solar energy absorption capacity comprises the following steps: the ultraviolet-visible-near infrared reflectance and transmission spectra were obtained by an ultraviolet-visible-near infrared spectrometer (SOLID 3700); the hydrophilicity test method comprises the following steps: recording the infiltration process in real time by using a DataPhysics OCA 25 device; the test method of the thermal management performance comprises the following steps: thermal conductivity was measured by a Hot Disk Techmax TPS1500 thermometer; the test method of the water evaporation enthalpy comprises the following steps: differential Scanning Calorimeter (DSC) analysis was performed on DSC Q2000; the test method of the steam regeneration rate under 1 unit of solar irradiation comprises the following steps: a xenon lamp simulation sunlight tester; as a result of the detection, the simulated wood blackbody material prepared in example 1 had a solar energy absorption capacity of 98%, a hydrophilic property, i.e., a saturated capacity ratio, of 19.2, and a thermal management property λ=32.8 mW.m, as shown in FIG. 9 -1 ·K -1 Enthalpy of evaporation of water 1475 J.g -1 And can reach 2.3 kg.m under 1 unit of solar irradiation -2 ·h -1 Is a high steam regeneration rate of (2); fig. 10 is a graph showing the surface temperature profile of the wood-like material prepared in example 1 immersed in water under 1 unit of sunlight, and the detection method is as follows: through thermal imaging camera
Figure SMS_1
head HiRes 640) to obtain an infrared thermogram; it can be seen that the temperature rise of CAP and CCAP is increased by 3℃and 10℃respectively, compared to pure deionized water (DIW), which is more conducive to water regeneration; fig. 11 is a comparison chart of adsorption of metal ions in the evaporation process of the simulated wood blackbody material prepared in example 1, and the detection method is as follows: inductively coupled plasma atomic absorption spectroscopy (ICP-AAS); it can be seen that after photo-thermal treatment, heavy metal ions in the water body are enriched in the CAP composite material.
The simulated wood blackbody materials prepared in example 2 and example 3 can realize the same photo-thermal conversion function as in example 1; however, the simulated wood blackbody materials prepared in example 2 and example 3 are relatively poor in water stability, and as shown in fig. 12, the simulated wood blackbody materials prepared in example 2 and example 3 all have a collapse phenomenon after being soaked in water for 2 days, and the CAP prepared in example 1 has a longer service life.
The macroporous super-hydrophilic skeleton of the simulated wood blackbody material prepared by the embodiment is sufficient for water transmission and spontaneous salt diffusion, can show excellent long-term evaporation stability and smaller performance attenuation in a metal solution, and opens up a new way for further developing a high-speed evaporation system and purifying wastewater containing metal ions.
The invention is inspired by the nanostructure arrangement of the nutrient ions in the enriching soil under the physiological action of the plants in the nature, and provides an artificial double-sided structure simulated wood blackbody material with a directional nanostructure prepared by an ice template method for the first time so as to transport the water in the sewage and enrich the heavy metal ions in the sewage. The blackbody material provided by the invention has excellent solar energy absorption capacity (98%), hydrophilicity (saturation capacity ratio is 19.2) and thermal management performance (lambda=32.8 mW.m) -1 ·K -1 ) And an evaporation enthalpy lower than that of the bulk water (1475 J.g -1 ) Can reach 2.3 kg.m under 1 unit of solar irradiation -2 ·h -1 Is a high steam generation rate of (a). The invention also provides a wood-like blackbody material which can exhibit excellent long-term evaporation stability and less performance degradation even in a high-concentration metal solution. The wood-like blackbody material provided by the invention provides a new direction for enriching heavy metals in the construction process of the high-performance solar seawater desalination evaporator, and has important significance for various applications including sewage regeneration and heavy metal wastewater treatment.
While the invention has been described and illustrated with reference to specific embodiments thereof, the description and illustration is not intended to limit the invention. It will be apparent to those skilled in the art that various changes may be made in this particular situation, material, composition of matter, substance, method or process without departing from the true spirit and scope of the invention as defined by the following claims, so as to adapt the objective, spirit and scope of the present application. All such modifications are intended to be within the scope of this appended claims. Although the methods disclosed herein have been described with reference to particular operations being performed in a particular order, it should be understood that these operations may be combined, sub-divided, or reordered to form an equivalent method without departing from the teachings of the present disclosure. Thus, unless specifically indicated herein, the order and grouping of operations is not a limitation of the present application.

Claims (7)

1. A simulated wood blackbody material comprising:
a layer of calcified polypyrrole-carboxymethyl cellulose-alginate composite material;
a layer of calcified carboxymethyl cellulose-sodium alginate composite material;
the preparation method of the wood-like blackbody material comprises the following steps:
freezing and casting the mixed solution of carboxymethyl cellulose and sodium alginate to obtain a composite material;
reacting a mixed solution of sodium alginate and carboxymethyl cellulose, polypyrrole and ammonium persulfate to obtain a reaction product;
the reaction product and the composite material are compounded and then dried to obtain an intermediate product;
calcification is carried out on the intermediate product to obtain a simulated wood blackbody material;
the method for freeze casting comprises the following steps:
arranging a mould on the copper sheet, and pouring the mixed solution of the carboxymethyl cellulose and the sodium alginate into the mould;
placing a copper block into liquid nitrogen, and placing the die on the copper block to obtain a composite material;
the compounding method comprises the following steps:
pouring the reaction product into a mould filled with a composite material for solidification;
the calcification method comprises the following steps:
soaking the intermediate product in CaCl 2 And (5) after the solution is in solution, drying the solution to obtain the wood-like blackbody material.
2. The simulated wood blackbody material of claim 1, having a solar absorption capacity of 96-99% and a heat transfer coefficient of 30-35 mW.m -1 ·K -1 The interfacial water evaporation enthalpy is 1450-1500 J.g -1 。
3. A preparation method of a wood-like blackbody material comprises the following steps:
freezing and casting the mixed solution of carboxymethyl cellulose and sodium alginate to obtain a composite material;
reacting a mixed solution of sodium alginate and carboxymethyl cellulose, polypyrrole and ammonium persulfate to obtain a reaction product;
the reaction product and the composite material are compounded and then dried to obtain an intermediate product;
calcification is carried out on the intermediate product to obtain a simulated wood blackbody material;
the method for freeze casting comprises the following steps:
arranging a mould on the copper sheet, and pouring the mixed solution of the carboxymethyl cellulose and the sodium alginate into the mould;
placing a copper block into liquid nitrogen, and placing the die on the copper block to obtain a composite material;
the compounding method comprises the following steps:
pouring the reaction product into a mould filled with a composite material for solidification;
the calcification method comprises the following steps:
soaking the intermediate product in CaCl 2 And (5) after the solution is in solution, drying the solution to obtain the wood-like blackbody material.
4. A metal recovery enrichment device comprising: the simulated wood blackbody material of claim 1 or the simulated wood blackbody material prepared by the method of claim 3.
5. A sewage regeneration device comprising: the simulated wood blackbody material of claim 1 or the simulated wood blackbody material prepared by the method of claim 3.
6. A heavy metal wastewater treatment device, comprising: the simulated wood blackbody material of claim 1 or the simulated wood blackbody material prepared by the method of claim 3.
7. A solar desalination evaporator comprising: the simulated wood blackbody material of claim 1 or the simulated wood blackbody material prepared by the method of claim 3.
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