CN115850273B - Phenanthroline iron complex, preparation method and application thereof in electrochromic aspect - Google Patents
Phenanthroline iron complex, preparation method and application thereof in electrochromic aspect Download PDFInfo
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- -1 Phenanthroline iron complex Chemical class 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000003860 storage Methods 0.000 claims abstract description 74
- 239000000243 solution Substances 0.000 claims abstract description 41
- 239000007983 Tris buffer Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims description 86
- 239000003792 electrolyte Substances 0.000 claims description 35
- FIKAKWIAUPDISJ-UHFFFAOYSA-L paraquat dichloride Chemical compound [Cl-].[Cl-].C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 FIKAKWIAUPDISJ-UHFFFAOYSA-L 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- 239000003115 supporting electrolyte Substances 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000004065 semiconductor Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- FYOAILFCEUZWBX-UHFFFAOYSA-N [7-(hydroxymethyl)-1,10-phenanthrolin-4-yl]methanol Chemical compound C1=CC2=C(CO)C=CN=C2C2=C1C(CO)=CC=N2 FYOAILFCEUZWBX-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 229910003086 Ti–Pt Inorganic materials 0.000 claims description 8
- 239000003446 ligand Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- JIVLDFFWTQYGSR-UHFFFAOYSA-N 4,7-dimethyl-[1,10]phenanthroline Chemical compound C1=CC2=C(C)C=CN=C2C2=C1C(C)=CC=N2 JIVLDFFWTQYGSR-UHFFFAOYSA-N 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007832 Na2SO4 Substances 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 3
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical group [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 claims description 3
- 229910001488 sodium perchlorate Inorganic materials 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 21
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000011521 glass Substances 0.000 abstract description 4
- 238000000151 deposition Methods 0.000 abstract description 2
- 238000005192 partition Methods 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 description 12
- 238000006722 reduction reaction Methods 0.000 description 12
- 238000001802 infusion Methods 0.000 description 10
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
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- 238000010438 heat treatment Methods 0.000 description 4
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- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- MBOIBXSDCWRKJR-UHFFFAOYSA-N 1,10-phenanthroline-4,7-dicarboxylic acid Chemical compound C1=CC2=C(C(O)=O)C=CN=C2C2=C1C(C(=O)O)=CC=N2 MBOIBXSDCWRKJR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
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- 230000005684 electric field Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
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- 238000005057 refrigeration Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical class [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
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- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
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- 229920005989 resin Polymers 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
- Hybrid Cells (AREA)
Abstract
The invention relates to a phenanthroline iron complex, a preparation method and application thereof in electrochromic aspect. The existing electrochromic material has the problems of long color changing time, short cycle life and the like, and the electrochromic device has the problems of complex production process and the like. The invention provides a tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, and an electrochromic device can be constructed based on the phenanthroline iron complex. The material has simple preparation process and excellent performance, the electrochromic device constructed only needs to introduce the solution of the material into the transparent cavity to realize the electrochromic function, a multi-layer electrochromic structure is avoided, a conductive layer, an ion storage layer and positive and negative electrodes are not required to be arranged in a partition mode, the step of depositing the electrochromic material on the surface of conductive glass or an electrode is completely omitted, the difficulty of the production process is reduced, and meanwhile, the problems of harsh production conditions, high cost and the like are also overcome.
Description
Technical Field
The invention relates to an electrochromic material, in particular to a phenanthroline iron complex, a preparation method and application thereof in electrochromic.
Background
Electrochromic is a phenomenon in which the optical properties of a material are changed under the drive of an applied electric field, so that a reversible change in color occurs. The electrochromic device has light absorption or light transmission adjustability under the action of an electric field, can selectively absorb or reflect external heat radiation and internal heat diffusion, reduces consumption of a large amount of energy sources for keeping cool in summer and warm in winter of office buildings, residential houses and the like, finally achieves the purpose of saving energy, and simultaneously achieves the purpose of improving natural illumination degree. Currently, electrochromic materials are most widely used in electrochromic windows, and the electrochromic materials also have certain application in the fields of anti-dazzling rearview mirrors, military camouflage and the like.
The traditional electrochromic materials are mainly divided into inorganic electrochromic materials and organic electrochromic materials, wherein most of the inorganic electrochromic materials are transition metal oxides and Prussian blue derivatives, for example, WO 3、TiO2、NiO、IrO2, and the organic electrochromic materials are solid organic films formed by polypyrrole, monomer pyrrole, viologen and the like. The inorganic color-changing material has the problems of long color-changing time, short cycle life at high temperature/low temperature and the like, and the organic film material can be subjected to ultraviolet degradation, so that the large-scale application is unlikely to be realized.
The traditional electrochromic device has a five-layer structure, namely a transparent conductive layer (2 layers), an electrochromic layer, an electrolyte layer and an ion storage layer. The existing processes for preparing the electrochromic device with the sandwich structure mainly comprise a magnetron sputtering method, a sol-gel method, an electrochemical deposition method, a chemical vapor deposition method and the like, but the processes are operated in a high-temperature high-pressure or vacuum environment, and the prepared electrochromic device has the problems of unstable interface, uneven color change, long and short cycle life, difficult maintenance in the use process and the like. In addition, the current electrochromic device has extremely complex production process and extremely strict requirements on production conditions, so the production cost is always high.
Disclosure of Invention
The invention aims to provide a phenanthroline iron complex, a preparation method and application thereof in electrochromic aspect, so as to solve the problems of long color changing time, short cycle life at high temperature/low temperature and the like of the existing electrochromic material, and the problems of complex production process, high production cost and the like of electrochromic devices.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the phenanthroline iron complex is tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, and has the structure that:
wherein n is 2 or 3.
In another aspect, there is provided a preparation method of the phenanthroline iron complex, the method comprising:
4, 7-dimethyl-1, 10 phenanthroline is taken as a raw material, and 4, 7-dihydroxymethyl-1, 10 phenanthroline ligand is obtained by adopting a hydrothermal synthesis method;
uniformly mixing 4, 7-dihydroxymethyl-1, 10 phenanthroline ligand with FeCl 2·4H2 O under neutral condition to obtain tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex.
On the other hand, the application of the phenanthroline iron complex in electrochromic is provided, wherein the application is to construct an electrochromic device based on the phenanthroline iron complex.
Further, the electrochromic device comprises a photo anode, a common electrode, an anode liquid storage tank, a cathode liquid storage tank and an anode side transparent cavity, wherein the common electrode is a cathode;
The anode liquid storage tank is connected with the photo anode and the anode side transparent cavity through a liquid conveying pipeline, and the photo anode and the anode side transparent cavity are connected back to the anode liquid storage tank through a liquid conveying pipeline;
the cathode and the cathode liquid storage tank form circulation through a transfusion pipeline;
the anode liquid storage tank is internally provided with an anode electrolyte containing the phenanthroline iron complex, and the cathode liquid storage tank is internally provided with a cathode electrolyte containing methyl viologen.
Or the electrochromic device comprises a common electrode, a photocathode, an anode liquid storage tank, a cathode liquid storage tank and a cathode side transparent cavity, wherein the common electrode is an anode;
the cathode liquid storage tank is connected with the photocathode and the cathode side transparent cavity through a transfusion pipeline, and the photocathode and the cathode side transparent cavity are connected back to the cathode liquid storage tank through a transfusion pipeline;
the anode and the anode liquid storage tank form circulation through a transfusion pipeline;
the anode liquid storage tank is internally provided with an anode electrolyte containing the phenanthroline iron complex, and the cathode liquid storage tank is internally provided with a cathode electrolyte containing methyl viologen.
Or the electrochromic device comprises a photo anode, a photo cathode, an anode liquid storage tank, a cathode liquid storage tank, an anode side transparent cavity and a cathode side transparent cavity;
The anode liquid storage tank is connected with the photo anode and the anode side transparent cavity through a liquid conveying pipeline, and the photo anode and the anode side transparent cavity are connected back to the anode liquid storage tank through a liquid conveying pipeline;
the cathode liquid storage tank is connected with the photocathode and the cathode side transparent cavity through a transfusion pipeline, and the photocathode and the cathode side transparent cavity are connected back to the cathode liquid storage tank through a transfusion pipeline;
the anode liquid storage tank is internally provided with an anode electrolyte containing the phenanthroline iron complex, and the cathode liquid storage tank is internally provided with a cathode electrolyte containing methyl viologen.
Further, the anolyte is obtained by the following steps:
mixing the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex with water to obtain a phenanthroline iron complex solution;
Adding a supporting electrolyte into the phenanthroline iron complex solution, and stirring and mixing;
And adding a solvent to obtain the anode electrolyte.
Further, the catholyte is obtained by the following steps:
Mixing methyl viologen with water to obtain methyl viologen solution;
and adding a supporting electrolyte into the methyl viologen solution to obtain the catholyte.
Further, the supporting electrolyte is selected from NaClO4、KNO3、KCl、NaCl、Na2SO4、KClO4、NH4Cl、K2HPO4;
The solvent is selected from acetonitrile, ethanol and methanol.
Further, the photo-anode and the photo-cathode are both semiconductor photo-electrodes with PN junctions, the semiconductor structure of the photo-anode is n +-n-p+ -Si-Ti-Pt, and the semiconductor structure of the photo-cathode is p +-n-n+ -Si-Ti-Pt.
Compared with the prior art, the invention has the following beneficial effects:
The invention provides a tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, which is an electrochromic material, and can rapidly undergo oxidation or reduction reaction under the action of illumination or electrification so as to ensure that the color of a solution changes from transparent to colored forward and reverse, and has the advantages of simple preparation process, excellent performance, low production cost, long service life, recyclable electrolyte and the like. Based on the electrochromic material, the invention also provides an electrochromic device, the electrochromic function can be realized only by leading the electrochromic material into a transparent container with a cavity structure, the traditional multi-layer electrochromic structure is avoided, a conductive layer, an ion storage layer and positive and negative electrodes are not required to be arranged in the inner partition, the step of depositing the electrochromic material on the surface of conductive glass or an electrode is completely omitted, the difficulty of the production process is reduced, and the problems of harsh production conditions, high cost and the like are also overcome.
The electrochromic device based on the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex provided by the invention integrates the functions of photovoltaics, energy storage and color change, can realize energy storage while changing color, does not consume commercial power in the whole process, and all electric energy is supplied from a photovoltaic cell, so that the structure is simplified, and self-power supply is realized. The liquid flow battery energy storage system replaces the traditional solid storage battery energy storage device, and has the characteristics of high energy efficiency, long cycle life, good safety, modularized design, high power density and the like. The semiconductor photovoltaic cell with PN junction is used for replacing external power supply equipment of electrochromic device, so that consumption of electric energy such as thermal power is reduced, and carbon emission is reduced. The self-discharge problem in the solid electrochromic device is solved, the components of the electrolyte can be regulated and controlled or replaced at any time, for example, the purpose of increasing the capacity can be achieved by increasing the concentration or increasing the volume of the storage tank, so that the whole electrochromic device is convenient to maintain and maintain, and the service life of the electrochromic device is greatly prolonged.
The electrochromic device can be used for building glass, and can reduce a large amount of energy which is necessary to be consumed for cooling in summer and heating in winter of buildings such as office buildings, residential houses and the like by adjusting the absorption and transmission of light and absorbing or reflecting external heat radiation, thereby achieving the purpose of energy conservation. Meanwhile, the indoor effective sunlight illuminance is improved, the outdoor shading facilities can be reduced, and the lighting and attractive requirements of the existing building are met.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other embodiments of the drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view showing the constitution of a device according to example 1 of the present invention.
Fig. 2 is a view showing the structure of a photoelectrode according to embodiment 1 of the present invention.
FIG. 3 is a view showing the constitution of a device according to example 2 of the present invention.
Fig. 4 is a structural view of a photoelectrode in embodiment 2 of the present invention.
FIG. 5 is a view showing the constitution of a device according to example 3 of the present invention.
Fig. 6 is a structure diagram of a photoelectrode according to embodiment 3 of the present invention.
Fig. 7 is a schematic view of the application of the present invention to architectural glass.
The marks in the figure are as follows:
001-photo anode, 002-photo cathode, 003-common electrode, 004-anolyte, 005-catholyte, 006-diaphragm, 007-anode liquid storage tank, 008-cathode liquid storage tank, 009-1 pump, 010-2 pump, 011-3 pump, 012-4 pump, 013-infusion line, 014-wire, 015-switch, 016-load, 017-anode side transparent cavity, 018-cathode side transparent cavity.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. The drawings illustrate preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In the description of this patent, it is to be understood that all technical and scientific terms used have the same meaning as commonly understood by one of ordinary skill in the art to which this patent belongs. In case of conflict, the present specification, definitions, will control. Unless otherwise indicated, the technical means used in the examples are conventional means known to those skilled in the art, the reagents used in the examples are commercial products, the devices used in the examples are existing devices, and the limitations on the means, reagents or devices should not be interpreted as limitations on the present patent, and the same types of means, reagents or devices for solving the same technical problems are within the scope of protection of the present patent.
In the description of this patent, it should be understood that when an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or as a range bounded by a list of upper preferable values and lower preferable values, this should be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value with any lower range limit or preferred value, regardless of whether ranges are separately disclosed. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
In the description of this patent, it should be understood that, in describing the process, a plurality of steps are involved, and should not be construed as limiting the sequence of steps of the method, and the technical solution obtained by only changing the sequence of steps when solving the same technical problem is also within the protection scope of this patent.
The invention provides a phenanthroline iron complex, which is tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, and has the structure that:
wherein n is 2 or 3.
Iron in the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex is hexacoordinated metal ion, and three 4, 7-dihydroxymethyl-1, 10-phenanthroline are used as ligands, so that a coordination compound with a central symmetry structure is formed.
The preparation method of the phenanthroline iron complex comprises the following steps: 4, 7-dimethyl-1, 10 phenanthroline is taken as a raw material, and 4, 7-dihydroxymethyl-1, 10 phenanthroline ligand is obtained by adopting a hydrothermal synthesis method; uniformly mixing 4, 7-dihydroxymethyl-1, 10 phenanthroline ligand with FeCl 2·4H2 O under neutral condition to obtain tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex. The specific synthetic route is as follows:
(1) And simultaneously adding the 4, 7-dimethyl-1, 10 phenanthroline and potassium permanganate into a 30% sulfuric acid solution, and heating and refluxing for 8 hours to obtain the 4, 7-dicarboxyl-1, 10 phenanthroline.
(2) Adding 4, 7-dicarboxyl-1, 10 phenanthroline into a solution containing 10% methanol and 30% sulfuric acid, and heating and refluxing for 30 hours to obtain 4, 7-dimethoxy amide-1, 10 phenanthroline.
(3) Adding 4, 7-dimethoxy amide-1, 10 phenanthroline and sodium borohydride into an ethanol solution containing 60 percent, heating and refluxing for 15 hours to obtain 4, 7-dihydroxymethyl-1, 10 phenanthroline.
(4) Adding 4, 7-dihydroxymethyl-1, 10 phenanthroline and ferrous chloride tetrahydrate into an acetonitrile water solution with a volume ratio of 1:10 according to a molar ratio of 3:1, fully stirring, uniformly mixing, and then adding 1mol/L sodium chloride as a supporting electrolyte to obtain the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex.
In addition, the tri (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex can be oxidized by applying positive potential through an electrochemical method to obtain the tri (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex with higher valence.
The tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex obtained by the method is an ideal electrochromic material, and can be applied to the electrochromic field to construct electrochromic devices. The tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex is used as an electrochromic active substance in an electrochromic device, and can rapidly undergo oxidation or reduction reaction under the action of illumination or electrification so as to cause the color of a solution to change from transparent to colored forward and reverse, thus realizing color change, self-power supply and energy storage in the process and being applied to the related fields.
The electrochromic device comprises an anode and a cathode, wherein the anode can be a common electrode 003 or a photo-anode 001, the cathode can be a common electrode 003 or a photo-cathode 002, and the anode and the cathode are not simultaneously arranged as the common electrode 003. The electrochromic device also includes an anode reservoir 007, a cathode reservoir 008, and a transparent cavity. The transparent cavity cooperates with the photo anode 001 and the photo cathode 002 to set up: when the device is provided with the photo anode 001, an anode side transparent cavity 017 is configured for the photo anode 001 and the anode liquid storage tank 007; when the apparatus has a photocathode 002, a cathode-side transparent cavity 018 is provided for photocathode 002 and a cathode reservoir 008.
The photo-anode 001 and the photo-cathode 002 are both semiconductor photo-electrodes with PN junctions, the semiconductor structure of the photo-anode 001 is n +-n-p+ -Si-Ti-Pt, and the semiconductor structure of the photo-cathode 002 is p +-n-n+ -Si-Ti-Pt.
The anode liquid storage tank 007 is internally provided with an anode electrolyte 004, and can be prepared by adopting a tri (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, and the process is as follows:
S1: mixing the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex with water to obtain a phenanthroline iron complex solution;
S2: adding a supporting electrolyte into the phenanthroline iron complex solution, and stirring and mixing;
s3: solvent was added to obtain anolyte 004.
The cathode electrolyte 005 is arranged in the cathode liquid storage tank 008, contains negative electrode pairing active substances, can be prepared by adopting methyl viologen, and has the following process:
S1: mixing methyl viologen with water to obtain methyl viologen solution;
s2: a supporting electrolyte is added to the methyl viologen solution to obtain a catholyte 005.
The supporting electrolyte is selected from NaClO4、KNO3、KCl、NaCl、Na2SO4、KClO4、NH4Cl、K2HPO4, etc., and the solvent is selected from acetonitrile, ethanol, methanol, etc.
The electrochromic device can adopt the following three structural forms:
Example 1: color change of electrolyte at side of photo anode-anode of PV
As shown in fig. 1 and 2, the electrochromic device includes a photo anode 001, a common electrode 003, an anode reservoir 007, a cathode reservoir 008, and an anode side transparent cavity 017, the common electrode 003 being the cathode. A diaphragm 006 is provided between the photo-anode 001 and the common electrode 003, and a wire 014, a switch 015 and a load 016 are connected.
The anode liquid storage tank 007 is connected to the bottom of the photo-anode 001 through a liquid delivery pipeline 013 and a No. 1 pump 009, and is connected back to the anode liquid storage tank 007 through the liquid delivery pipeline 013 after the electrochemical reaction is finished, so that the reciprocating circulation is realized. Meanwhile, the anode liquid storage tank 007 is also connected into the anode side transparent cavity 017 through the infusion pipeline 013 and the No. 3 pump 011, and after the electrolyte in the anode side transparent cavity 017 is full, the electrolyte flows into the anode liquid storage tank 007 through the infusion pipeline 013, so that the reciprocating circulation is realized. The cathode and the cathode liquid storage tank 008 form circulation through a transfusion pipeline 013 and a No. 2 pump 010.
An anolyte 004 containing phenanthroline iron complex is arranged in the anode liquid storage tank 007. Preparing a solution of 0.001mol/L by adopting a tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex and deionized water, adding supporting electrolyte NaCl, wherein the concentration of the supporting electrolyte in the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex aqueous solution is 0.1mol/L, fully stirring and uniformly mixing, adding acetonitrile accounting for 1% of the volume fraction of the electrochromic active material solution, and uniformly mixing the solution to obtain the anode electrolyte 004.
Within the cathode reservoir 008 is a catholyte 005 containing a negative electrode partner active material. The negative electrode paired active material adopts methyl viologen solution with the concentration of 0.001mol/L, adopts 1mol/L KClO 4 as supporting electrolyte, and adopts water as solvent.
The polyethylene is processed into a transparent device with a planar surface shape by adopting an injection molding integrated preparation process, and is used as an anode side transparent cavity 017, the cavity volume is 0.01m 2, and the radius of a pipeline on the top substrate and the bottom substrate is 0.0001m.
The energy storage implementation mode of the embodiment is as follows:
When sunlight irradiates the photo-anode, photo-generated carriers are generated on PN junction of the semiconductor structure, holes flow from an n + region to a p + region, electrons flow from a p + region to an n + region, the photo-generated holes are captured by electroactive substances on an anode electrolyte interface, oxidation reaction is carried out on tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron, photo-generated electrons are led to one side of a cathode electrolyte through an external circuit, reduction reaction is carried out on methyl viologen, conversion from light energy to chemical energy is realized in the process, and energy conversion efficiency is up to 94%.
The color-changing and energy-saving implementation mode of the embodiment is as follows:
when illumination exists, the No. 3 pump 011 is turned on, the flow rate of the pump is set to be 40mL/min, at the moment, a part of anolyte is directly led into the transparent cavity 017 at the anode side, at the moment, along with the continuous oxidation of the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex by the photogenerated cavity, the color of the solution is gradually changed from the colorless in a reduced state to the red in an oxidized state, at the moment, the average transmittance of the transparent cavity at 508-520nm is 8.3%, at the moment, the transparent cavity in the red can block sunlight outside, so that the rise of the indoor temperature is avoided, and the use of refrigeration equipment such as indoor air conditioners is reduced. When no light is irradiated, the embodiment can be used as a photovoltaic flow battery, the working principle is the same as that of a common flow battery, when the flow battery outputs electric energy to an external load, the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex in the anolyte undergoes a reduction reaction, the color of the solution is gradually changed from red in an oxidation state to colorless in a reduction state, and at the moment, the average transmittance of a transparent cavity at 508-520nm is 93%.
Example 2: color change of electrolyte on side of Photovoltaic (PV) photocathode-cathode
As shown in fig. 3 and 4, the electrochromic device includes a common electrode 003, a photocathode 002, an anode reservoir 007, a cathode reservoir 008 and a cathode side transparent cavity 018, the common electrode 003 being the anode. A separator 006 is provided between the normal electrode 003 and the photocathode 002, and a wire 014, a switch 015 and a load 016 are connected.
The cathode liquid storage tank 008 is connected to the bottom of the photocathode 002 through a transfusion pipeline 013 and a No. 2 pump 010, and is connected to the cathode liquid storage tank 008 through the transfusion pipeline 013 after the electrochemical reaction is finished, so that the reciprocating circulation is realized. Meanwhile, the cathode liquid storage tank 008 is connected to the cathode side transparent cavity 018 through the infusion pipeline 013 and the No. 4 pump 012, and after the electrolyte in the cathode side transparent cavity 018 is full, the electrolyte flows into the cathode liquid storage tank 008 through the infusion pipeline 013, so that the reciprocating circulation is realized. The anode and anode reservoir 007 are circulated through infusion line 013 and pump number 1 009.
An anolyte 004 containing phenanthroline iron complex is arranged in the anode liquid storage tank 007. Preparing 0.1mol/L solution by using a tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex and deionized water, adding a supporting electrolyte KCl, wherein the concentration of the supporting electrolyte in the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex aqueous solution is 1mol/L, fully stirring and uniformly mixing, adding ethanol accounting for 10% of the volume fraction of the paired active material solution, and uniformly mixing the solution to obtain an anode electrolyte 004.
Within the cathode reservoir 008 is a catholyte 005 containing a negative electrode partner active material. The negative electrode electrochromic active material adopts methyl viologen solution with the concentration of 0.1mol/L, adopts 1mol/LNaClO 4 as supporting electrolyte, and adopts water as solvent.
The polypropylene was processed into a transparent device with a curved surface shape by a blow molding integrated preparation process, as a cathode side transparent cavity 018, a cavity volume of 0.1m 2, and a pipe radius on the top and bottom substrates of 0.001m.
The energy storage implementation mode of the embodiment is as follows:
When the solar light irradiates the photocathode, photo-generated carriers are generated on PN junctions of the semiconductor structure, holes flow from an n + region to a p + region, electrons flow from a p + region to an n + region, photo-generated electrons are captured by electroactive substances on a catholyte interface, so that methyl viologen undergoes a reduction reaction, an anode side common electrode loses electrons to cause tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron to undergo an oxidation reaction, the conversion from light energy to chemical energy is realized in the process, and the energy efficiency of the photovoltaic flow battery reaches 90%.
The color-changing and energy-saving implementation mode of the embodiment is as follows:
when illumination exists, the No. 4 pump 012 is turned on, the flow rate of the pump is set to be 100mL/min, at the moment, a part of catholyte is directly led into the transparent cavity, at the moment, along with continuous reduction of methyl viologen by photo-generated electrons, the color of the solution is gradually changed from colorless in an oxidation state to blue in a reduction state, at the moment, the average transmittance of the transparent cavity at 450-452nm is 4.1%, at the moment, the blue transparent cavity can block sunlight outside, so that the rise of indoor temperature is avoided, and the use of refrigerating equipment such as an indoor air conditioner is reduced. When no illumination exists, the embodiment can be used as a photovoltaic flow battery, the working principle is the same as that of a common flow battery, the flow battery outputs electric energy to an external load, meanwhile, methyl viologen in a catholyte is subjected to oxidation reaction, the color of a solution is gradually changed from the blue of a reduced state to the colorless of an oxidized state, and at the moment, the average transmittance of a transparent cavity at 450-452nm is 95%.
Example 3: electrolyte on two sides of photovoltaic anode and photovoltaic cathode changes color simultaneously
As shown in fig. 5 and 6, the electrochromic device includes a photo anode 001, a photo cathode 002, an anode reservoir 007, a cathode reservoir 008, an anode side transparent cavity 017 and a cathode side transparent cavity 018. A diaphragm 006 is provided between the photo-anode 001 and the photo-cathode 002, and a wire 014, a switch 015 and a load 016 are connected.
The anode liquid storage tank 007 is connected to the bottom of the photo anode 001 through a liquid delivery pipeline 013 and a No. 1 pump 009, and is connected to the anode liquid storage tank 007 through the liquid delivery pipeline 013 after the electrochemical reaction is finished, so that the reciprocating circulation is realized. Meanwhile, the anode liquid storage tank 007 is also connected into the anode side transparent cavity 017 through the infusion pipeline 013 and the No. 3 pump 011, and after the electrolyte in the anode side transparent cavity 017 is full, the electrolyte flows into the anode liquid storage tank 007 through the infusion pipeline 013, so that the reciprocating circulation is realized.
The cathode liquid storage tank 008 is connected to the bottom of the photocathode 002 through a transfusion pipeline 013 and a No. 2 pump 010, and is connected to the cathode liquid storage tank 008 through the transfusion pipeline 013 after the electrochemical reaction is finished, so that the reciprocating circulation is realized. Meanwhile, the cathode liquid storage tank 008 is connected to the cathode side transparent cavity 018 through the infusion pipeline 013 and the No. 4 pump 012, and after the electrolyte in the cathode side transparent cavity 018 is full, the electrolyte flows into the cathode liquid storage tank 008 through the infusion pipeline 013, so that the reciprocating circulation is realized.
An anolyte 004 containing phenanthroline iron complex is arranged in the anode liquid storage tank 007. Preparing 0.01mol/L solution by using tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex and deionized water, adding a supporting electrolyte NH 4 Cl, wherein the concentration of the supporting electrolyte in the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex aqueous solution is 0.1mol/L, adding methanol accounting for 5% of the volume fraction of the solution after fully stirring and uniformly mixing, and obtaining the anolyte after uniformly mixing the solution.
Within the cathode reservoir 008 is a catholyte 005 containing a negative electrode partner active material. The negative electrode electrochromic active material adopts methyl viologen solution with the concentration of 0.01mol/L, adopts 0.1mol/LNa 2SO4 as supporting electrolyte, and adopts water as solvent.
The transparent resin was processed into a transparent device having a planar surface shape by an extrusion molding integrated preparation process, as an anode-side transparent cavity 017 and a cathode-side transparent cavity 018, the cavity volume was 0.001m 2, and the pipe radius on the top substrate and the bottom substrate was 0.0001m.
The energy storage implementation mode of the embodiment is as follows:
The semiconductor structure of the photo-anode is n +-n-p+ -Si-Ti-Pt, the semiconductor structure of the photo-cathode is p +-n-n+ -Si-Ti-Pt, when sunlight irradiates the photo-anode and the photo-cathode at the same time, photo-generated carriers are generated on PN junctions of the semiconductor structure, holes flow from an n + area to a p + area, electrons flow from a p + area to an n + area, at the moment, the photo-generated holes generated on one side of the photo-anode are captured by an electroactive substance on an anolyte interface, so that the tri (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex is subjected to an oxidation reaction, the photo-generated electrons generated on one side of the photo-cathode are captured by an electroactive substance on a catholyte interface, so that the reduction reaction of methyl viologen occurs, the photo-generated electrons generated on one side of the photo-anode and the photo-generated holes generated on one side of the photo-cathode are subjected to deactivation through an external circuit, the conversion of light energy to chemical energy is realized, and the energy efficiency of the battery reaches 92%.
The color-changing and energy-saving implementation mode of the embodiment is as follows:
When illumination exists, the No. 3 pump 011 and the No. 4 pump 012 are turned on, the flow rates of the pumps are set to be 50mL/min, at the moment, a part of anode and cathode electrolyte are respectively and directly led into the two transparent cavities, a photo-generated cavity at one side of the photo-anode continuously oxidizes tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, the color of the solution is gradually changed from the colorless in a reduced state to the red in an oxidized state, at the moment, the average transmittance of the transparent cavities at 508-520nm is 8.3%, at the moment, a red color changing device can block sunlight outside, so that the rise of the indoor temperature is avoided, and the use of refrigeration equipment such as indoor air conditioners is reduced. The photo-generated electrons on one side of the photocathode continuously reduce methyl viologen, the color of the solution is gradually changed from colorless in an oxidation state to blue in a reduction state, the average transmittance of the transparent cavity at 450-452nm is 4.1%, and the blue color-changing device can block sunlight outside, so that the rise of indoor temperature is avoided, and the use of refrigerating equipment such as indoor air conditioners is reduced. When no light is emitted, the embodiment can be used as a photovoltaic flow battery, the working principle is the same as that of a common flow battery, when the flow battery outputs electric energy to an external load, the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex in the anolyte undergoes a reduction reaction, the color of the solution is gradually changed from red in an oxidation state to colorless in a reduction state, and at the moment, the average transmittance of the electrochromic device at 508-520nm is 93%. The methyl viologen in the catholyte is subjected to oxidation reaction, the color of the solution is gradually changed from the blue in a reduced state to the colorless in an oxidized state, and the average transmittance of the transparent cavity at 450-452nm is 95%.
In the embodiment shown in fig. 7, the transparent cavity in the electrochromic device can be used as building glass, and of course, the transparent cavity can also be applied to other occasions needing to be discolored, so that the effects of energy storage, color changing, energy saving and the like are achieved.
The foregoing description of the invention has been presented for purposes of illustration and description, and is not intended to be limiting. Several simple deductions, modifications or substitutions may also be made by a person skilled in the art to which the invention pertains, based on the idea of the invention.
Claims (10)
1. The phenanthroline iron complex is characterized in that:
the phenanthroline iron complex is tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex, and has the structure that:
wherein n is 2 or 3.
2. The preparation method of the phenanthroline iron complex of claim 1, wherein the preparation method is characterized by comprising the following steps:
The method comprises the following steps:
4, 7-dimethyl-1, 10 phenanthroline is taken as a raw material, and 4, 7-dihydroxymethyl-1, 10 phenanthroline ligand is obtained by adopting a hydrothermal synthesis method;
uniformly mixing 4, 7-dihydroxymethyl-1, 10 phenanthroline ligand with FeCl 2·4H2 O under neutral condition to obtain tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex.
3. The use of the phenanthroline iron complex according to claim 1 in electrochromic applications, wherein:
the application is to construct an electrochromic device based on the phenanthroline iron complex.
4. A use according to claim 3, characterized in that:
the electrochromic device comprises a photo anode (001), a common electrode (003), an anode liquid storage tank (007), a cathode liquid storage tank (008) and an anode side transparent cavity (017), wherein the common electrode (003) is a cathode;
The anode liquid storage tank (007) is connected into the photo anode (001) and the anode side transparent cavity (017) through a liquid conveying pipeline (013), and the photo anode (001) and the anode side transparent cavity (017) are connected back to the anode liquid storage tank (007) through the liquid conveying pipeline (013);
The cathode and the cathode liquid storage tank (008) form circulation through a transfusion pipeline (013);
The anode liquid storage tank (007) is internally provided with an anode electrolyte (004) containing the phenanthroline iron complex, and the cathode liquid storage tank (008) is internally provided with a cathode electrolyte (005) containing methyl viologen.
5. A use according to claim 3, characterized in that:
The electrochromic device comprises a common electrode (003), a photocathode (002), an anode liquid storage tank (007), a cathode liquid storage tank (008) and a cathode side transparent cavity (018), wherein the common electrode (003) is an anode;
The cathode liquid storage tank (008) is connected into the photocathode (002) and the cathode side transparent cavity (018) through a liquid conveying pipeline (013), and the photocathode (002) and the cathode side transparent cavity (018) are connected back to the cathode liquid storage tank (008) through the liquid conveying pipeline (013);
the anode and the anode liquid storage tank (007) form circulation through a transfusion pipeline (013);
The anode liquid storage tank (007) is internally provided with an anode electrolyte (004) containing the phenanthroline iron complex, and the cathode liquid storage tank (008) is internally provided with a cathode electrolyte (005) containing methyl viologen.
6. A use according to claim 3, characterized in that:
The electrochromic device comprises a photo anode (001), a photo cathode (002), an anode liquid storage tank (007), a cathode liquid storage tank (008), an anode side transparent cavity (017) and a cathode side transparent cavity (018);
The anode liquid storage tank (007) is connected into the photo anode (001) and the anode side transparent cavity (017) through a liquid conveying pipeline (013), and the photo anode (001) and the anode side transparent cavity (017) are connected back to the anode liquid storage tank (007) through the liquid conveying pipeline (013);
The cathode liquid storage tank (008) is connected into the photocathode (002) and the cathode side transparent cavity (018) through a liquid conveying pipeline (013), and the photocathode (002) and the cathode side transparent cavity (018) are connected back to the cathode liquid storage tank (008) through the liquid conveying pipeline (013);
The anode liquid storage tank (007) is internally provided with an anode electrolyte (004) containing the phenanthroline iron complex, and the cathode liquid storage tank (008) is internally provided with a cathode electrolyte (005) containing methyl viologen.
7. The use according to claim 4, 5 or 6, characterized in that:
The anode electrolyte (003) is obtained by the following steps:
mixing the tris (4, 7-dihydroxymethyl) -1, 10-phenanthroline iron complex with water to obtain a phenanthroline iron complex solution;
Adding a supporting electrolyte into the phenanthroline iron complex solution, and stirring and mixing;
adding a solvent to obtain the anolyte (003).
8. The use according to claim 7, characterized in that:
the catholyte (004) is obtained through the following steps:
Mixing methyl viologen with water to obtain methyl viologen solution;
Adding a supporting electrolyte into the methyl viologen solution to obtain the catholyte (004).
9. The use according to claim 8, characterized in that:
the supporting electrolyte is selected from NaClO4、KNO3、KCl、NaCl、Na2SO4、KClO4、NH4Cl、K2HPO4;
The solvent is selected from acetonitrile, ethanol and methanol.
10. The use according to claim 6, characterized in that:
The photo anode (001) and the photo cathode (002) are both semiconductor photo electrodes with PN junctions, the semiconductor structure of the photo anode (001) is n +-n-p+ -Si-Ti-Pt, and the semiconductor structure of the photo cathode (002) is p +-n-n+ -Si-Ti-Pt.
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| CN109053722A (en) * | 2018-07-12 | 2018-12-21 | 南京邮电大学 | The application of ferrosin complex and synthetic method and memristor and memristor |
| CN110950861A (en) * | 2019-11-01 | 2020-04-03 | 广西师范大学 | Mononuclear dysprosium complex with 1, 10-phenanthroline-2, 9-dicarboxylic acid as ligand and preparation method and application thereof |
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| CN109053722A (en) * | 2018-07-12 | 2018-12-21 | 南京邮电大学 | The application of ferrosin complex and synthetic method and memristor and memristor |
| CN110950861A (en) * | 2019-11-01 | 2020-04-03 | 广西师范大学 | Mononuclear dysprosium complex with 1, 10-phenanthroline-2, 9-dicarboxylic acid as ligand and preparation method and application thereof |
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