CN115448357B - Method for synthesizing lead halide perovskite by recycling lead ions in aqueous solution - Google Patents
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- 150000002500 ions Chemical class 0.000 title claims abstract description 29
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 28
- 150000004820 halides Chemical class 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000004064 recycling Methods 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 10
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 14
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 14
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 14
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 235000019253 formic acid Nutrition 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- -1 cesium bromide formic acid Chemical compound 0.000 claims description 5
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 231100000331 toxic Toxicity 0.000 abstract description 4
- 230000002588 toxic effect Effects 0.000 abstract description 4
- 239000008346 aqueous phase Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 abstract 2
- 238000011084 recovery Methods 0.000 description 5
- 229960001484 edetic acid Drugs 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/006—Compounds containing, besides lead, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a method for synthesizing lead halide perovskite by recycling lead ions in an aqueous solution. According to the method, disodium ethylenediamine tetraacetate modified MOF-808 is selected as a template, lead ions in the aqueous solution are recovered as a lead source, and lead halide perovskite grows in situ in the pore canal of the MOF-808. According to the invention, disodium ethylenediamine tetraacetate modified MOF-808 is selected as a template, lead ions in the aqueous solution are recovered as a lead source, and lead halide perovskite grows in situ in the pore canal of the MOF-808, so that the controllable preparation from toxic lead in an aqueous phase environment to the lead halide perovskite is realized. The method has low cost and good reproducibility, has certain economic effect and meets the environmental protection requirement.
Description
Technical Field
The invention relates to the technical field of lead recovery, in particular to a method for synthesizing lead halide perovskite by recycling lead ions in aqueous solution.
Background
Toxic lead constitutes a potential threat to the environment, health and safety, greatly impeding commercialization of lead-halide perovskite. From the 20% efficiency of the lead-halide perovskite-based photovoltaic device and the 500nm thickness of the lead-halide perovskite, it is known that about 3.5 tons of lead is required for 1 gigawatt of electricity. To achieve the 20% goal of the lead halogen perovskite-based photovoltaic device power generation occupying the 8500 gigawatt power market by 2050, nearly 6000 tons of lead are required each year. The use of lead is a huge and indispensable for lead-halogen perovskite-based optoelectronic devices, and the direct utilization of lead ions has a great influence on both economy and environment.
However, in the current method for recycling lead, the compound formed by the chemical precipitation method needs to undergo multiple steps of chemical reactions to obtain lead salt of the synthetic lead halide perovskite (Matlock, B.S.Howerton, D.A.Atwood, ind Eng chem. Res.2002,41, 1519-1582.); the generation of lead salt byproducts can be avoided by an ion exchange method, but the recovery and utilization efficiency of toxic lead is relatively low under the influence of a balance constant (I.Ali, V.K.Gupta, nat.Nanotechnol.2016,11, 365-371.); the recovery and utilization effect is better through a film filtering method, but the input cost of a filtering device is too high (S.Bolisetty, R.Mezzenga, nat.Protoc.2006,1, 2661-2667.) and the technical problems of complicated steps, low recovery rate, too high cost and the like of the recovery and utilization of lead ions in the aqueous solution in the prior art are solved.
Disclosure of Invention
The present invention aims to solve the above-mentioned drawbacks of the prior art and to provide a method for synthesizing lead halide perovskite by recycling lead ions in an aqueous solution.
According to the method for synthesizing lead halide perovskite by recycling lead ions in the aqueous solution, disclosed by the invention, the MOF-808 modified by disodium ethylenediamine tetraacetate is selected as a template, the lead ions in the aqueous solution are recycled as a lead source, and the lead halide perovskite grows in situ in a pore channel of the MOF-808.
Further, disodium edetate modified MOF-808 is specifically described as follows:
1) Carrying out solution thermal reaction on trimesic acid, zirconium oxychloride octahydrate, formic acid and N, N-dimethylformamide to obtain MOF-808;
2) Soaking the MOF-808 in N, N dimethylformamide and anhydrous acetone respectively for a period of time, and calcining at a certain temperature for a period of time to obtain activated MOF-808;
3) And adding the activated MOF-808 into an aqueous solution of disodium ethylenediamine tetraacetate, reacting for a period of time at a certain temperature, and then soaking in anhydrous acetone for a period of time to obtain the MOF-808 modified by disodium ethylenediamine tetraacetate, namely MOF-808-EDTA.
Further, the particle size of the synthesized MOF-808 is 500-5000nm.
Further, the mass ratio of MOF-808 to disodium ethylenediamine tetraacetate is 1:20-200, and the modification time is 10-48h.
Further, the specific operation of in situ growth of lead halide perovskite in the pore channels of MOF-808 is as follows:
(1) Adding the modified MOF-808-EDTA into an aqueous solution containing lead ions, adsorbing at room temperature, centrifuging and drying to obtain MOF-808-EDTA@Pb adsorbing lead ions 2+ ；
(2) MOF-808-EDTA@Pb 2+ Adding oleic acid and oleylamine into toluene solution, stirring, slowly dripping cesium bromide formic acid solution, and reacting to obtain MOF-808-EDTA@CsPbBr 3 。
Further, the mass volume ratio of the MOF-808-EDTA to the aqueous solution containing lead ions is 0.01-1g/mL, and the concentration of the lead ions in the aqueous solution is 10-1000mg/mL.
Further, MOF-808-EDTA@Pb 2+ The mass volume ratio of the oil to the oleic acid is 0.001-0.01:1-10 g/. Mu.L.
Further, MOF-808-EDTA@Pb 2+ The mass volume ratio of the oil amine to the oleylamine is 0.001-0.01:1-10 g/. Mu.L.
Further, the concentration of the formic acid solution of cesium bromide is 1-10mg/mL, and the mass volume ratio of the MOF-808-EDTA@Pb2+ to the formic acid solution of cesium bromide is 0.001-0.01:1-5 g/. Mu.L, and the reaction time is 1-10s.
Compared with the prior art, the invention has the following technical effects:
according to the invention, disodium ethylenediamine tetraacetate modified MOF-808 is selected as a template, lead ions in the aqueous solution are recovered as a lead source, and lead halide perovskite grows in situ in the pore canal of the MOF-808, so that the controllable preparation from toxic lead in an aqueous phase environment to the lead halide perovskite is realized. The method has low cost and good reproducibility, has certain economic effect and meets the environmental protection requirement.
Drawings
FIG. 1 is an SEM image (scale bar 5 μm) of MOF-808 prepared according to the practice of the present invention;
FIG. 2 shows the MOF-808@CsPbBr obtained by the practice of the present invention 3 Element mapping image (scale 50 nm);
FIG. 3 shows MOF-808, MOF-808-EDTA and MOF-808-EDTA@Pb prepared in accordance with an embodiment of the present invention 2+ Is a FTIR spectrum of (C);
FIG. 4 shows the MOF-808-EDTA@CsPbBr prepared in example 1 of the present invention 3 Wherein a is XRD spectrum and b is fluorescence spectrum;
FIG. 5 shows MOF-808-EDTA@CsPbBr prepared in example 2 of the present invention 3 Wherein a is XRD spectrum and b is fluorescence spectrum;
FIG. 6 shows MOF-808-EDTA@CsPbBr prepared in example 3 of the present invention 3 Wherein a is XRD spectrum and b is fluorescence spectrum;
FIG. 7 is a reaction scheme of the present invention.
Detailed Description
The following are specific embodiments of the present invention and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
A method for synthesizing lead halide perovskite by recycling lead ions in an aqueous solution, comprising the following steps:
1) Adding 0.5mmol of trimesic acid, 0.5mmol of zirconium oxychloride octahydrate, 20mL of formic acid and 20mL of N, N-dimethylformamide into a 60mL reaction kettle, and reacting for 2 days at 130 ℃ to obtain MOF-808;
2) Soaking the MOF-808 in 10mL of N, N dimethylformamide and 10mL of anhydrous acetone for 3 days, and calcining at 150 ℃ for 1 day to obtain activated MOF-808;
3) As shown in FIG. 7, 0.1g of activated MOF-808 was added to 50mL of an aqueous solution containing 1.86g of disodium edetate, reacted at 60℃for 1 day, and immersed in 10mL of anhydrous acetone for 1 day to obtain disodium edetate-modified MOF-808-EDTA;
4) Adding the modified MOF-808-EDTA (ethylene diamine tetraacetic acid) of 0.1g into a lead nitrate aqueous solution of 20mg/mL, adsorbing for 10 hours at room temperature, centrifuging and drying to obtain the MOF-808-EDTA@Pb adsorbing lead ions 2+ ；
5) Adding the modified MOF-808, 4 mu L of oleic acid and 4 mu L of oleylamine which adsorb lead ions into 1mL of toluene solution, slowly dripping 1 mu L of cesium bromide formic acid solution with the concentration of 10mg/mL after stirring with great force, and reacting for 3 seconds to obtain MOF-808-EDTA@CsPbBr 3 。
MOF-808-EDTA@CsPbBr obtained in this example 3 Comprises MOF-808-EDTA and CsPbBr 3 In the crystalline phase, the fluorescence emission peak was at 466nm, as shown in FIG. 4.
FIG. 1 is an SEM image (scale bar 5 μm) of MOF-808 prepared according to the practice of the present invention;
FIG. 2 shows the MOF-808@CsPbBr obtained by the practice of the present invention 3 Element mapping image (scale 50 nm);
FIG. 3 shows MOF-808, MOF-808-EDTA and MOF-808-EDTA@Pb prepared in accordance with an embodiment of the present invention 2+ Is a FTIR spectrum of (C);
example 2
A method for synthesizing lead halide perovskite by recycling lead ions in an aqueous solution, which is characterized by comprising the following steps:
1) Adding 0.5mmol of trimesic acid, 0.5mmol of zirconium oxychloride octahydrate, 20mL of formic acid and 20mL of N, N-dimethylformamide into a 60mL reaction kettle, and reacting for 2 days at 130 ℃ to obtain MOF-808;
2) Soaking the MOF-808 in 10mL of N, N dimethylformamide and 10mL of anhydrous acetone for 3 days, and calcining at 150 ℃ for 1 day to obtain activated MOF-808;
3) Adding 0.1g of activated MOF-808 into 50mL of aqueous solution containing 1.86g of disodium ethylenediamine tetraacetate, reacting for 1 day at 60 ℃, and soaking in 10mL of anhydrous acetone for 1 day to obtain disodium ethylenediamine tetraacetate modified MOF-808-EDTA;
4) Adding the modified MOF-808-EDTA (ethylene diamine tetraacetic acid) 0.1g into a lead nitrate aqueous solution of 100mg/mL, adsorbing for 16h at room temperature, centrifuging and drying to obtain the MOF-808-EDTA@Pb adsorbing lead ions 2+ ；
5) Adding the modified MOF-808, 5 mu L of oleic acid and 5 mu L of oleylamine which adsorb lead ions into 1mL of toluene solution, stirring the mixture vigorously, slowly dripping 1 mu L of cesium bromide formic acid solution with the concentration of 10mg/mL, and reacting for 5 seconds to obtain MOF-808-EDTA@CsPbBr 3 。
MOF-808-EDTA@CsPbBr obtained in this example 3 Comprises MOF-808-EDTA and CsPbBr 3 The crystal phase, fluorescence emission peak at 471nm, is shown in FIG. 5.
Example 3
A method for synthesizing lead halide perovskite by recycling lead ions in an aqueous solution, which is characterized by comprising the following steps:
1) Adding 0.5mmol of trimesic acid, 0.5mmol of zirconium oxychloride octahydrate, 20mL of formic acid and 20mL of N, N-dimethylformamide into a 60mL reaction kettle, and reacting for 2 days at 130 ℃ to obtain MOF-808;
2) Soaking the MOF-808 in 10mL of N, N dimethylformamide and 10mL of anhydrous acetone for 3 days, and calcining at 150 ℃ for 1 day to obtain activated MOF-808;
3) Adding 0.1g of activated MOF-808 into 50mL of aqueous solution containing 1.86g of disodium ethylenediamine tetraacetate, reacting for 1 day at 60 ℃, and soaking in 10mL of anhydrous acetone for 1 day to obtain disodium ethylenediamine tetraacetate modified MOF-808-EDTA;
4) Adding the modified MOF-808-EDTA (ethylene diamine tetraacetic acid) of 0.1g into 50mg/mL lead nitrate aqueous solution, adsorbing for 20h at room temperature, centrifuging and drying to obtain the MOF-808-EDTA@Pb adsorbing lead ions 2+ ；
5) Adding the modified MOF-808, 8 mu L of oleic acid and 8 mu L of oleylamine which adsorb lead ions into 1mL of toluene solution, slowly dripping 2 mu L of cesium bromide formic acid solution with the concentration of 10mg/mL after stirring with great force, and reacting for 5 seconds to obtain MOF-808-EDTA@CsPbBr 3 。
MOF-808-EDTA@CsPbBr obtained in this example 3 Comprising MOF-808-EDTA and CsPbBr 3 The fluorescence emission peak was at 465nm in the crystalline phase, as shown in FIG. 6.
The above is not relevant and is applicable to the prior art. While certain specific embodiments of the present invention have been described in detail by way of example, it will be appreciated by those skilled in the art that the foregoing examples are provided for the purpose of illustration only and are not intended to limit the scope of the invention, and that various modifications or additions and substitutions to the described specific embodiments may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the invention as defined in the accompanying claims. It should be understood by those skilled in the art that any modification, equivalent substitution, improvement, etc. made to the above embodiments according to the technical substance of the present invention should be included in the scope of protection of the present invention.
Claims (3)
1. A method for synthesizing lead halide perovskite by recycling lead ions in aqueous solution is characterized by selecting MOF-808 modified by disodium ethylenediamine tetraacetate as a template, recycling the lead ions in the aqueous solution as a lead source, and growing the lead halide perovskite in situ in pore channels of the MOF-808, and specifically comprises the following steps:
s1, carrying out solution thermal reaction on 0.5mmol of trimesic acid, 0.5mmol of zirconium oxychloride octahydrate, 20mL formic acid and 20 mLN, N dimethylformamide to obtain MOF-808;
s2, soaking the MOF-808 in N, N dimethylformamide and anhydrous acetone respectively for a period of time, and calcining at a certain temperature for a period of time to obtain activated MOF-808;
s3, adding the MOF-808 activated by 0.1. 0.1g into a 50mL aqueous solution containing 1.86g disodium ethylenediamine tetraacetate, reacting for a period of time at a certain temperature, and then soaking in anhydrous acetone for a period of time to obtain MOF-808 modified by disodium ethylenediamine tetraacetate, namely MOF-808-EDTA;
s4, adding the MOF-808-EDTA modified by 0.1 and g into an aqueous solution containing 20 mg/mL-100 mg/mL of lead ions, adsorbing at room temperature, centrifuging and drying to obtain the MOF-808-EDTA@Pb adsorbing the lead ions 2+ ；
S5, mixing 0.001-g g MOF-808-EDTA@Pb 2+ Adding 4-8 mu L of oleic acid and 4-8 mu L of oleylamine into toluene solution, stirring, slowly dripping 1-2 mu L of cesium bromide formic acid solution with the concentration of 10mg/mL, and reacting to obtain MOF-808-EDTA@CsPbBr 3 。
2. The method of claim 1, wherein the synthetic MOF-808 has a particle size of 500 to 5000nm.
3. The method of claim 1, wherein in step S3, the modification time is 10 to 48 and h.
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