CN113233532B - Low-cost photo-thermal material based on solar interface evaporation and preparation method thereof - Google Patents
Low-cost photo-thermal material based on solar interface evaporation and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 87
- 238000001704 evaporation Methods 0.000 title claims abstract description 58
- 230000008020 evaporation Effects 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 83
- 239000006260 foam Substances 0.000 claims abstract description 83
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 83
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000000243 solution Substances 0.000 claims abstract description 50
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229920000767 polyaniline Polymers 0.000 claims abstract description 39
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007800 oxidant agent Substances 0.000 claims abstract description 34
- 230000001590 oxidative effect Effects 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 239000010936 titanium Substances 0.000 claims abstract description 9
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 62
- 238000000034 method Methods 0.000 claims description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000009210 therapy by ultrasound Methods 0.000 claims description 18
- 229920000642 polymer Polymers 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 abstract description 12
- 238000002791 soaking Methods 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 238000010276 construction Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 12
- 238000005286 illumination Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000010612 desalination reaction Methods 0.000 description 4
- 235000021314 Palmitic acid Nutrition 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000013535 sea water Substances 0.000 description 3
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical group NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 2
- 235000021360 Myristic acid Nutrition 0.000 description 2
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 230000008467 tissue growth Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-GTFORLLLSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCC[14C](O)=O QIQXTHQIDYTFRH-GTFORLLLSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/56—Preparation of melamine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
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- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a low-cost photo-thermal material based on solar interface evaporation and a preparation method thereof, wherein the preparation method comprises the following steps: 1) soaking melamine foam in aniline solution, adding oxidant solution for reaction, taking out the melamine foam, washing and drying to obtain a polyaniline/melamine foam composite structure, and marking the polyaniline/melamine foam composite structure as PMF; 2) adding linear alkyl acid and nano titanium dioxide into lower alcohol, then immersing PMF into the titanium-containing mixed solution for reaction, taking out the PMF, washing and drying to finish the preparation. The invention innovatively utilizes the self-assembly characteristics of straight-chain alkyl acid, titanium dioxide, melamine foam and polyaniline to anchor TiO2The nano particles realize the construction of a surface layer micro-nano structure, have high-efficiency evaporation rate, photo-thermal conversion performance and dye degradation performance, and the evaporation rate is up to 2.346 kg.m under one sunlight‑2·h‑1The photo-thermal conversion efficiency can reach 128.38%.
Description
Technical Field
The invention belongs to the field of water treatment and surface function modification, and particularly relates to a low-cost photo-thermal material based on solar interface evaporation and a preparation method thereof.
Background
China is short of water resources, the per-capita water resource amount is only 1/4 which is the average level in the world, and the shortage of fresh water resources is the problem which needs to be solved urgently at present. Sea water desalination and sewage purification are two effective methods for solving the problem of water resource shortage. Clean water is mainly obtained by reverse osmosis, multistage flash evaporation, low-temperature multi-effect distillation and other methods, but the methods consume a large amount of fuel and electric power, so that the development of a novel technology which is low in cost, green and sustainable is urgently needed. Solar energy is increasingly concerned by experts and scholars at home and abroad as a green renewable energy source, and an interface evaporation technology based on the solar energy is gradually developed.
Solar interface evaporation technology uses a light absorbing material to absorb sunlight and convert it into heat for heating water at the air-liquid interface, so that the water escapes in the form of water vapor. Compared with the traditional heating mode, the interface evaporation has higher response speed and higher evaporation efficiency, and can quickly generate a large amount of steam. At present, the interface evaporation technology is mainly used in the fields of seawater desalination, distillation, solar power generation and the like. However, in the solar photo-thermal desalination process, pollutants such as salts and microorganisms may be generated on the surface and inside, which severely limits water supply, damages the absorption of photo-thermal materials to light, and blocks the pore channels, thereby reducing the steam conversion rate. In particular for waste water, a complex biogeochemical environment and complex components are inevitably involved, which increases the difficulty of purification.
Chinese patent CN111170393A discloses a solar evaporator with a hollow structure and a preparation method thereof, wherein the solar evaporator is formed into a hollow convex shape by hydrothermal reaction, but the evaporation rate is only 1.476 kg.m-2·h-1The evaporation efficiency is only 92.9%, and the performance needs to be improved. Chinese patent CN111282443A discloses a membrane material for seawater desalination by solar interface evaporation and a preparation method thereof, the method prepares PAA nanofiber membrane by electrostatic spinning technology, then imidizes to obtain PI nanofiber membrane, and finally obtains porous fluffy graphite fiber by laser ablation technology, the preparation process is complex, and the evaporation rate under one sun illumination is only 1.595 kg.m-2·h-1The performance needs to be improved.
The application provides a photo-thermal material for solar interface evaporation wastewater treatment, which has the advantages of simple preparation method, low cost, high absorptivity, high evaporation rate and high photo-thermal conversion efficiency, and a preparation method thereof.
Disclosure of Invention
In view of the above technical problems in the prior art, the present invention aims to provide a photothermal material for solar interface evaporation wastewater treatment, which has a simple preparation method, low cost, and high absorbance, evaporation rate, and photothermal conversion efficiency, and a preparation method thereof.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized by comprising the following steps of:
1) preparing a solution: dissolving aniline with hydrochloric acid uniformly to prepare an aniline solution for later use; dissolving the oxidant uniformly by hydrochloric acid to prepare an oxidant solution for later use;
2) and (3) growing polyaniline: adding melamine foam into a freshly prepared aniline solution, completely adsorbing the aniline solution by the melamine foam, then adding a freshly prepared oxidant solution, immersing the oxidant solution into the melamine foam, and contacting the oxidant solution with aniline to perform aniline oxidation polymerization reaction, so that a polyaniline polymer tissue grows in the melamine foam once to obtain a polyaniline/melamine foam composite structure, and marking the polyaniline/melamine foam composite structure as PMF; after the reaction is finished, cleaning the PMF by using pure water and ethanol, and drying in an oven;
3) repeating the operation step of the step 2) for 0-4 times, so that the polyaniline polymer tissue grows in the melamine foam for 1-5 times in total, and the obtained PMF enters the next procedure;
4) reacting a linear alkyl acid CH3(CH2)nAdding COOH into lower alcohol solvent, performing ultrasonic treatment for 5-20min, adding nanometer titanium dioxide, and performing ultrasonic treatment for 5-20min to obtain titanium-containing mixed solution; dipping the PMF into the titanium-containing mixed solution for a dipping reaction for 4-8h to obtain a titanium dioxide/polyaniline/melamine foam composite structure marked as TPMF; and finally, cleaning the mixture by pure water and ethanol, and drying the mixture in an oven to finish the preparation.
In the step 3) of the preparation method, when the operation of the step 2) is repeated 0 times, the dried material in the step 2) is directly subjected to the operation process of the next step 4) without further treatment, and the reaction for growing polyaniline is only performed once. And when the operation of the step 2) is repeated 1 time in the step 3), the aniline solution and the oxidant solution are sequentially added into the material dried in the step 2), and the material is dried after the reaction is finished and then enters the operation process of the next step 4), so that the polyaniline polymer structure grows in the melamine foam 2 times in total. And analogizing, when the operation of the step 2) is repeated for 2-4 times in the step 3), 3-5 times of growth of the polyaniline polymer structure is respectively carried out in the interior of the melamine foam.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that in the step 1), the aniline solution is prepared by mixing aniline and 0.8-1.2mol/L hydrochloric acid aqueous solution according to a volume ratio of 1:15-25 and then performing ultrasonic treatment for 5-25 min; the preparation process of the oxidant solution comprises the steps of mixing an oxidant and 0.8-1.2mol/L hydrochloric acid aqueous solution according to the mass ratio of 0.02-0.04:1, and carrying out ultrasonic treatment for 5-25 min.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that the oxidant is one or a mixture of ammonium persulfate and ferric trichloride; in the step 2), the ratio of the mass of the oxidant to the volume of the aniline is 0.2-0.5: 1.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that the oxidant is ammonium persulfate or is formed by mixing ammonium persulfate and ferric trichloride according to the ratio of 1: 1-1: 4.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that in the step 4), the linear alkyl acid CH3(CH2)nIn the molecular structure of COOH, n is an integer of 10-20, preferably 18; the lower alcohol solvent is methanol or ethanol, preferably ethanol; the linear alkyl acid CH3(CH2)nThe concentration of COOH added into the lower alcohol solvent is 0.005-0.2 g/mL.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that the step 4) is implementedThe nano titanium dioxide and the straight-chain alkyl acid CH3(CH2)nThe mass ratio of COOH is 1: 1-5, preferably 1: 3; the nano titanium dioxide is anatase titanium dioxide of 10-20 nm.
The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that the operation processes of the steps 2) to 4) are all carried out at room temperature; in the step 2), the time for carrying out aniline oxidation polymerization reaction is 2-6h, preferably 3 h; in the step 3), the operation steps of the step 2) are repeated for 1-2 times, so that the polyaniline polymer structure grows in the melamine foam for 2-3 times in total.
The low-cost photothermal material based on solar interface evaporation prepared by the method is characterized in that the low-cost photothermal material is divided into an upper part and a lower part, wherein the upper part is melamine foam, and the lower part is TPMF.
The advantages and the beneficial effects of the invention are as follows:
the invention innovatively utilizes the linear chain alkyl acid CH3(CH2)nSelf-assembly characteristics of COOH (particularly preferably octadecanoic acid) with titanium dioxide, melamine foam and polyaniline, anchoring TiO2The nano particles realize the construction of a surface layer micro-nano structure, the preparation method is simple, the cost is low, the prepared TPMF material is applied as a material for purifying solar interface evaporation wastewater, the TPMF material has high-efficiency evaporation rate, photo-thermal conversion performance and dye degradation performance, and the evaporation rate is up to 2.346 kg.m.under one sunlight-2·h-1The photothermal conversion efficiency can break through 1, can reach 128.38%, and can degrade the dye concentration in water from 10ppm to 0.0604 ppm.
Drawings
FIG. 1 is a schematic flow chart of the preparation of the low-cost photothermal material of the present invention;
FIG. 2 is a SEM image of TPMF-2L-3 prepared in example 13 of the present invention;
FIG. 3 is a diagram of the temperature rise of TPMF-2L-3 prepared in example 13 under the intensity of sunlight.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1
A preparation method of a low-cost photothermal material (a schematic preparation flow diagram is shown in figure 1) comprises the following steps:
1) preparing a solution:
adding 1mL of aniline into 20mL of 1mol/L hydrochloric acid aqueous solution, performing ultrasonic treatment for 20min, and preparing an aniline solution for later use after the ultrasonic treatment is finished. 0.365g of ammonium persulfate (APS, taken as an oxidant) is added into 10mL of 1mol/L hydrochloric acid aqueous solution for ultrasonic treatment for 20min to prepare an oxidant solution for later use.
2) And (3) growing polyaniline: melamine foam is prepared, and the specification of the melamine foam is a cuboid structure with the length of 3cm, the width of 3cm and the height of 2 cm. Adding the melamine foam into the aniline solution prepared in the step 1), soaking and absorbing for 30min at room temperature, wherein the aniline solution completely enters the lower part of the melamine foam, and the soaking height of the aniline solution on the melamine foam is about 1 cm.
Adding the oxidant solution prepared in the step 1) into the lower part of the melamine foam, immersing the oxidant solution into the lower part of the melamine foam, slightly increasing the infiltration height of the solution in the melamine foam, performing aniline oxidation polymerization reaction for 3 hours at room temperature, performing polyaniline polymer tissue growth in the lower part of the melamine foam for the first time, obtaining a polyaniline/melamine foam composite structure at the lower part of the melamine foam, and marking the polyaniline/melamine foam composite structure as PMF; after the reaction is finished, washing the melamine foam with PMF at the lower part for 2-3 times by pure water, then washing twice by ethanol so as to wash a small amount of unreacted aniline remained on the melamine foam, and finally drying in an oven.
3) Repeating the operation step of the step 2) for 0 time, so that the polyaniline polymer tissue grows in the lower part of the melamine foam for 1 time in total, and the obtained PMF enters the next procedure;
4) preparation of titanium dioxide/polyaniline/melamine foam (TPMF):
firstly, 0.2g of dodecanoic acid is added into 20mL of absolute ethyl alcohol for ultrasonic treatment for 20min, then 0.1g of anatase titanium dioxide with the particle size of 10-20nm is added, and the ultrasonic treatment is continued for 20min, so as to obtain a titanium-containing mixed solution. Then, dipping the PMF at the lower part of the melamine foam into the titanium-containing mixed solution for carrying out room temperature soaking reaction for 6 hours to obtain a titanium dioxide/polyaniline/melamine foam composite structure at the lower part of the melamine foam, wherein the mark is TPMF. After the reaction is finished, washing the melamine foam with TPMF at the lower part for 2-3 times by pure water, then washing twice by ethanol so as to wash out impurities remained on the melamine foam, and finally drying in an oven to finish the preparation. The low cost photothermal material prepared in example 1 was labeled as TPMF-1L-1.
The preparation scheme of TPMF-1L-1 in example 1 is shown in FIG. 1, and it can be seen that: the TPMF-1L-1 finally prepared is roughly divided into an upper part and a lower part, wherein the upper part is melamine foam, and the lower part is the TPMF. The prepared low-cost photo-thermal material with the upper part being white melamine foam and the lower part being TPMF can be inverted when the low-cost photo-thermal material is actually applied to a solar interface evaporation technology, the white melamine foam part of the low-cost photo-thermal material enters water to absorb moisture, and the TPMF part of the low-cost photo-thermal material is exposed in the air to absorb solar light.
The evaporation rate test of TPMF-1L-1 prepared in example 1 was carried out according to the following procedure: TPMF-1L-1 is divided into a melamine foam part and a TPMF part, the melamine foam part of the TPMF-1L-1 is completely immersed into 3.5 wt% of NaCl aqueous solution, the TPMF part of the TPMF-1L-1 is exposed in the air to absorb light energy, mass change of the solution is recorded by an analytical balance within 1.5h under the irradiation of a simulated xenon light source with the sun light intensity of 1, the evaporation rate of the solution is tested and calculated, the photo-thermal conversion efficiency of the solution is tested and calculated, and the results are listed in Table 1.
Wherein, the formula for calculating the evaporation rate of the test under the illumination is shown as formula (1) and the formula for calculating the photothermal conversion efficiency is shown as formula (2) under the condition of the irradiation of the simulated xenon light source with the sunlight intensity of 1.
Calculation formula of evaporation rate measured under illumination:
in the formula (1)：mlightRepresents the evaporation rate tested under illumination;
Δ m represents the change in mass over Δ T time;
and A represents the area of the material exposed to light.
The formula for calculating the photo-thermal conversion efficiency tested under illumination is as follows:
in the formula (2), η represents the photothermal conversion efficiency;
hLVthe expression of water evaporation enthalpy is a constant, and the value is 2444J/g;
coptan optical density, several units of solar intensity (copt 1 in example 1);
qirepresenting the intensity of illumination, and taking a value of 1 kw.m-2；
m＝mlight-mdark；
Wherein m isdarkThe result of the evaporation rate data representing the blank control is the result of the evaporation rate calculated by the test in the dark when the illumination environment (i.e., the simulated xenon light source illumination environment with the intensity of 1 sun light) of the above test is replaced with the one performed in the dark. The evaporation rate calculation method in the dark test can be calculated by referring to the method of formula (1).
The dye degradation test was performed on TPMF-1L-1 prepared in example 1, according to the following procedure: the melamine foam part of TPMF-1L-1 is completely immersed in a dye solution (namely, a methylene blue aqueous solution with the concentration of 10 ppm), the TPMF part of TPMF-1L-1 is exposed in the air to absorb light energy, and is placed in a self-made device, and evaporated water is collected within 4 hours under the irradiation of a simulated xenon light source with the solar light intensity of 3. The methylene blue concentration in the evaporated water was tested and the results are shown in table 1.
Example 2
Example 2 method for preparing a low-cost photothermal material example 1 was repeated except that "step 1) of example 2) in preparing an oxidizer solution, 0.365g of Ammonium Persulfate (APS) was replaced with 0.365g of APS and FeCl in total mass3Mixture of APS and FeCl3The mass ratio of (1: 1) and the other operations are the same as those in example 1, and finally the low-cost photothermal material is prepared.
Example 3
Example 3 method for preparing a low-cost photothermal material example 1 was repeated except that "step 1) of example 3) in preparing an oxidizer solution, 0.365g of Ammonium Persulfate (APS) was replaced with 0.365g of APS and FeCl in total mass3Mixture of APS and FeCl3The mass ratio of (1: 2) and the other operations are the same as those in example 1, and finally the low-cost photothermal material is prepared.
Example 4
Example 4 method for preparing a low-cost photothermal material example 1 was repeated except that "step 1) of example 4) in preparing an oxidizer solution, 0.365g of Ammonium Persulfate (APS) was replaced with 0.365g of APS and FeCl in total mass3Mixture of APS and FeCl3The mass ratio of (1: 3) and the other operations are the same as those in example 1, and finally the low-cost photothermal material is prepared.
Example 5
Method for preparing Low cost photothermal Material of example 5 example 1 was repeated except that "step 1) of example 5) in preparing the oxidizer solution, 0.365g of Ammonium Persulfate (APS) was replaced with 0.365g of APS and FeCl in total mass3Mixture of APS and FeCl3The mass ratio of (1: 4)', and the other operations are the same as example 1, and finally the low-cost photothermal material is prepared.
The test procedures of evaporation rate test and dye degradation test of the low-cost photothermal materials prepared in examples 2 to 5 were repeated in example 1, and the test results are shown in table 1.
Table 1: comparison of Properties of Low cost photothermal Material produced in examples 1-5
In table 1, the evaporation rate is the calculated evaporation rate result under the irradiation of a simulated xenon light source with a sunlight intensity of 1.
Example 6
Example 6 method for preparing low-cost photothermal material example 1 was repeated except for "replacing the mass of Ammonium Persulfate (APS) from 0.365g to 0.219 g", and the same operation as in example 1 was performed to finally prepare a low-cost photothermal material.
Example 7
Example 7 method for preparing low-cost photothermal material example 1 was repeated except for "replacing the mass of Ammonium Persulfate (APS) from 0.365g to 0.256 g", and the same operation as in example 1 was performed to finally prepare a low-cost photothermal material.
The evaporation rate and dye degradation tests of the low-cost photothermal materials prepared in examples 6-7 were carried out by repeating example 1, and the test results are shown in table 2.
TABLE 2
Example 8
Example 8 preparation method of low-cost photothermal material example 1 was repeated except for "repeating operation step 2) in step 3) 1 time so that polyaniline polymer structure was grown in the lower interior of the melamine foam 2 times in total and the resulting PMF was subjected to the next process", and the other operations were the same as example 1 to finally prepare low-cost photothermal material, which was labeled as TPMF-2L-1.
The specific preparation process of example 8 is:
1) preparing a solution:
adding 1mL of aniline into 20mL of 1mol/L hydrochloric acid aqueous solution, performing ultrasonic treatment for 20min, and preparing an aniline solution for later use after the ultrasonic treatment is finished. 0.365g of ammonium persulfate (APS, taken as an oxidant) is added into 10mL of 1mol/L hydrochloric acid aqueous solution for ultrasonic treatment for 20min to prepare an oxidant solution for later use.
2) And (3) growing polyaniline: melamine foam is prepared, and the specification of the melamine foam is a cuboid structure with the length of 3cm, the width of 3cm and the height of 2 cm. Adding the melamine foam into the aniline solution prepared in the step 1), soaking and absorbing for 30min at room temperature, wherein the aniline solution completely enters the lower part of the melamine foam, and the soaking height of the aniline solution on the melamine foam is about 1 cm.
Adding the oxidant solution prepared in the step 1) into the lower part of the melamine foam, immersing the oxidant solution into the lower part of the melamine foam, slightly increasing the infiltration height of the solution in the melamine foam, performing aniline oxidation polymerization reaction for 3 hours at room temperature, performing polyaniline polymer tissue growth in the lower part of the melamine foam for the first time, obtaining a polyaniline/melamine foam composite structure at the lower part of the melamine foam, and marking the polyaniline/melamine foam composite structure as PMF; after the reaction is finished, washing the melamine foam with PMF at the lower part for 2-3 times by pure water, then washing twice by ethanol so as to wash a small amount of unreacted aniline remained on the melamine foam, and finally drying in an oven.
3) Soaking the PMF at the lower part of the melamine foam dried in the step 2) into a mixed solution of 1mL aniline and 20mL hydrochloric acid aqueous solution (the concentration of hydrochloric acid is 1mol/L) again, soaking and absorbing for 30min at room temperature, then adding 20mL hydrochloric acid aqueous solution (the concentration of hydrochloric acid is 1mol/L) containing 0.365g ammonium persulfate, and carrying out aniline oxidation polymerization reaction for 3h at room temperature; after the reaction is finished, washing the melamine foam with PMF at the lower part for 2-3 times by pure water, then washing twice by ethanol, and finally drying in an oven.
4) Preparation of titanium dioxide/polyaniline/melamine foam (TPMF):
firstly, 0.2g of dodecanoic acid is added into 20mL of absolute ethyl alcohol for ultrasonic treatment for 20min, then 0.1g of anatase titanium dioxide with the particle size of 10-20nm is added, and the ultrasonic treatment is continued for 20min, so as to obtain a titanium-containing mixed solution. Then, dipping the PMF at the lower part of the melamine foam into the titanium-containing mixed solution for carrying out room temperature soaking reaction for 6 hours to obtain a titanium dioxide/polyaniline/melamine foam composite structure at the lower part of the melamine foam, wherein the mark is TPMF. After the reaction is finished, washing the melamine foam with TPMF at the lower part for 2-3 times by pure water, then washing twice by ethanol so as to wash out impurities remained on the melamine foam, and finally drying in an oven to finish the preparation. The low cost photothermal material prepared in example 8 was labeled as TPMF-2L-1.
Example 9
Example 9 preparation method of low-cost photothermal material example 1 was repeated except for "repeating the operation of step 2) 2 times in step 3) so that the polyaniline polymer structure was grown in the inside of the lower portion of the melamine foam 3 times in total and the resulting PMF was subjected to the next process", and the other operations were the same as example 1 to finally prepare a low-cost photothermal material, which was labeled as TPMF-3L-1.
Example 10
Example 10 method for preparing low-cost photothermal material example 1 was repeated except for "repeating the operation of step 2) 3 times in step 3) so that the polyaniline polymer structure was grown in the inside of the lower portion of the melamine foam 4 times in total and the resulting PMF was subjected to the next process", and the other operations were the same as example 1 to finally prepare low-cost photothermal material, which was labeled as TPMF-4L-1.
Example 11
Example 11 method for preparing a low-cost photothermal material example 1 was repeated except for "repeating the operation of step 2) 4 times in step 3) so that the polyaniline polymer structure was grown in the inside of the lower portion of the melamine foam 5 times in total and the resulting PMF was subjected to the next process", and the other operations were the same as example 1 to finally prepare a low-cost photothermal material, which was designated as TPMF-5L-1.
The evaporation rate and dye degradation tests of the low-cost photothermal materials prepared in examples 8-11 were carried out by repeating example 1, and the test results are shown in table 3.
TABLE 3
Example 12
Example 12 preparation method of low-cost photothermal material example 8 was repeated except that "step 4) was changed to 0.2g of titanium dioxide in addition amount from 0.1 g", and the same operation as in example 8 was performed to finally obtain a low-cost photothermal material, which was designated as TPMF-2L-2.
Example 13
Example 13 preparation method of low-cost photothermal material example 8 was repeated except that "in step 4), the added mass of titanium dioxide was changed from 0.1g to 0.3 g", and the same operation as in example 8 was performed to finally obtain a low-cost photothermal material, which was designated as TPMF-2L-3.
SEM images of the TPMF portion of TPMF-2L-3 at 80 microns, 10 microns, and 200nm are shown in FIG. 2. From fig. 2, it can be seen that the surface of the framework of the melamine foam becomes rough, and prototype particles appear, which proves that polyaniline and titanium dioxide are successfully loaded on the melamine foam.
The prepared TPMF-2L-3 is immersed in a 3.5 wt% NaCl aqueous solution, the surface temperature change of the TPMF-2L-3 is recorded by an infrared camera under the sunlight intensity, and the temperature rise condition of the TPMF-2L-3 under the sunlight intensity is shown in figure 3. As can be seen from fig. 3: the temperature is rapidly raised in the first 5 minutes, and the final temperature is stabilized at about 48 ℃.
Example 14
Example 14 preparation method of low-cost photothermal material example 8 was repeated except that "step 4) was changed to 0.4g of titanium dioxide in addition amount from 0.1 g", and the same operation as in example 8 was performed to finally obtain a low-cost photothermal material, which was designated as TPMF-2L-4.
Example 15
Example 15 preparation method of low-cost photothermal material example 8 was repeated except that "in step 4), the added mass of titanium dioxide was changed from 0.1g to 0.5 g", and the same operation as in example 8 was performed to finally obtain a low-cost photothermal material, which was designated as TPMF-2L-5.
The evaporation rate and dye degradation tests of the low-cost photothermal materials prepared in examples 12-15 were carried out by repeating example 1, and the test results are shown in table 4.
TABLE 4
Example 16
Example 16 method for producing a low-cost photothermal material example 13 was repeated except that in "step 4), dodecanoic acid was substituted with dodecanoic acid of the same quality as in example 13, to finally produce a low-cost photothermal material.
Example 17
Example 17 method for preparing low-cost photothermal material example 13 was repeated except that in "step 4), myristic acid was replaced with myristic acid of the same quality, and the same procedure as in example 13 was carried out to finally prepare low-cost photothermal material.
Example 18
Example 18 method for producing a low-cost photothermal material example 13 was repeated except that in "step 4), the same procedure as in example 13 was repeated except that the same amount of palmitic acid as the palmitic acid was used instead of the palmitic acid, thereby finally producing a low-cost photothermal material.
Example 19
Example 19 method for preparing low-cost photothermal material example 13 was repeated except that in "step 4), dodecanoic acid was replaced with octadecanoic acid of the same quality, and the same procedure as in example 13 was carried out to finally prepare low-cost photothermal material.
Example 20
Example 20 method for preparing low-cost photothermal material example 13 was repeated except that in "step 4), the same procedure as in example 13 was performed except that the same quality of eicosanoic acid was substituted for the dodecanoic acid, thereby finally preparing the low-cost photothermal material.
The evaporation rate and dye degradation tests of the low-cost photothermal materials prepared in examples 16-20 were carried out by repeating example 1, and the test results are shown in table 5.
TABLE 5
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (11)
1. A preparation method of a low-cost photo-thermal material based on solar interface evaporation is characterized by comprising the following steps:
1) preparing a solution: dissolving aniline with hydrochloric acid uniformly to prepare an aniline solution for later use; dissolving the oxidant uniformly by hydrochloric acid to prepare an oxidant solution for later use;
2) and (3) growing polyaniline: adding melamine foam into a freshly prepared aniline solution, completely adsorbing the aniline solution by the melamine foam, then adding a freshly prepared oxidant solution, immersing the oxidant solution into the melamine foam, and contacting the oxidant solution with aniline to perform aniline oxidation polymerization reaction, so that a polyaniline polymer tissue grows in the melamine foam once to obtain a polyaniline/melamine foam composite structure, and marking the polyaniline/melamine foam composite structure as PMF; after the reaction is finished, cleaning the PMF by using pure water and ethanol, and drying in an oven;
3) repeating the operation step of the step 2) for 0-4 times, so that the polyaniline polymer tissue grows in the melamine foam for 1-5 times in total, and the obtained PMF enters the next procedure;
4) reacting a linear alkyl acid CH3(CH2)nAdding COOH into lower alcohol solvent, performing ultrasonic treatment for 5-20min, adding nanometer titanium dioxide, and performing ultrasonic treatment for 5-20min to obtain titanium-containing mixed solution; dipping the PMF into the titanium-containing mixed solution for a dipping reaction for 4-8h to obtain a titanium dioxide/polyaniline/melamine foam composite structure marked as TPMF; finally, after being cleaned by pure water and ethanol, the mixture is dried in an oven, and the preparation is finished;
the ratio of the volume dosage of the aniline in the step 2) to the mass dosage of the nano titanium dioxide in the step 4) is 1 mL: 0.3 g.
2. The method for preparing a low-cost photothermal material based on solar interfacial evaporation according to claim 1, wherein in step 1), the aniline solution is prepared by mixing aniline and 0.8-1.2mol/L hydrochloric acid aqueous solution according to a volume ratio of 1:15-25, and performing ultrasonic treatment for 5-25 min; the preparation process of the oxidant solution comprises the steps of mixing an oxidant and 0.8-1.2mol/L hydrochloric acid aqueous solution according to the mass ratio of 0.02-0.04:1, and carrying out ultrasonic treatment for 5-25 min.
3. The method for preparing the low-cost photothermal material based on solar interfacial evaporation according to claim 1, wherein the oxidant is one or a mixture of ammonium persulfate and ferric trichloride; in the step 2), the ratio of the mass of the oxidant to the volume of the aniline is 0.2-0.5: 1.
4. The method for preparing the low-cost photothermal material based on solar interfacial evaporation according to claim 3, wherein the oxidant is ammonium persulfate or is a mixture of ammonium persulfate and ferric trichloride according to a ratio of 1: 1-1: 4.
5. The method for preparing low-cost photothermal material based on solar interfacial evaporation according to claim 1, wherein in step 4), the linear alkyl acid CH3(CH2)nIn the molecular structure of COOH, n = an integer of 10-20; the lower alcohol solvent is methanol or ethanol; the linear alkyl acid CH3(CH2)nThe concentration of COOH added into the lower alcohol solvent is 0.005-0.2 g/mL.
6. The method of claim 5, wherein the linear alkyl acid CH is selected from the group consisting of3(CH2)nIn the molecular structure of COOH, n = 18; the lower alcohol solvent is ethanol.
7. The method for preparing low-cost photothermal material based on solar interfacial evaporation according to claim 1, wherein in step 4), the nano titanium dioxide and the linear alkyl acid CH3(CH2)nThe mass ratio of COOH is 1: 1-5; the nano titanium dioxide is anatase titanium dioxide of 10-20 nm.
8. As claimed in claim 7The preparation method of the low-cost photo-thermal material based on solar interface evaporation is characterized in that in the step 4), the nano titanium dioxide and the linear chain alkyl acid CH3(CH2)nThe mass ratio of COOH was 1: 2.
9. The method for preparing a low-cost photothermal material based on solar interfacial evaporation as claimed in claim 1, wherein the steps 2) -4) are performed at room temperature; in the step 2), the time for carrying out aniline oxidation polymerization reaction is 2-6 h; in the step 3), the operation steps of the step 2) are repeated for 1-2 times, so that the polyaniline polymer structure grows in the melamine foam for 2-3 times in total.
10. The method for preparing a low-cost photothermal material based on solar interfacial evaporation according to claim 9, wherein in step 2), aniline oxidation polymerization is performed for 3 hours.
11. The low-cost photothermal material based on solar interfacial evaporation prepared by the method according to any one of claims 1-10, wherein said low-cost photothermal material is divided into upper and lower parts, the upper part being melamine foam and the lower part being said TPMF.
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