CN109569727A - A kind of preparation and application of double halides perovskite photochemical catalysts of highly effective hydrogen yield - Google Patents
A kind of preparation and application of double halides perovskite photochemical catalysts of highly effective hydrogen yield Download PDFInfo
- Publication number
- CN109569727A CN109569727A CN201811536577.9A CN201811536577A CN109569727A CN 109569727 A CN109569727 A CN 109569727A CN 201811536577 A CN201811536577 A CN 201811536577A CN 109569727 A CN109569727 A CN 109569727A
- Authority
- CN
- China
- Prior art keywords
- perovskite
- photochemical catalysts
- double halides
- double
- application
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 150000004820 halides Chemical class 0.000 title claims abstract description 17
- 239000001257 hydrogen Substances 0.000 title claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 11
- 229910052794 bromium Inorganic materials 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 230000001699 photocatalysis Effects 0.000 claims description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007146 photocatalysis Methods 0.000 claims description 8
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 6
- 229940071870 hydroiodic acid Drugs 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 125000001246 bromo group Chemical group Br* 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical group [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052801 chlorine Chemical group 0.000 claims description 2
- 239000000460 chlorine Chemical group 0.000 claims description 2
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 125000000962 organic group Chemical group 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 2
- 239000011575 calcium Substances 0.000 claims 2
- 229910052791 calcium Inorganic materials 0.000 claims 2
- 229910052719 titanium Inorganic materials 0.000 claims 2
- 239000010936 titanium Substances 0.000 claims 2
- 229930188620 butyrolactone Natural products 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 238000000935 solvent evaporation Methods 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052736 halogen Inorganic materials 0.000 abstract description 4
- 229910052697 platinum Inorganic materials 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 150000002367 halogens Chemical class 0.000 abstract 1
- 239000010970 precious metal Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 9
- -1 halogen acids Chemical class 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011011 black crystal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- GZUXJHMPEANEGY-UHFFFAOYSA-N methyl bromide Substances BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/40—Complexes comprising metals of Group IV (IVA or IVB) as the central metal
- B01J2531/44—Lead
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation and application of double halides perovskite photochemical catalysts of highly effective hydrogen yield, belong to the preparation technical field of catalyst.Double halides perovskite photochemical catalysts are made using a kind of simple technique, constituent content and forbidden bandwidth in perovskite crystal can be regulated and controled by controlling the ratio that two kinds of halogens are added in precursor solution.The catalyst preparation process is simple, and cost is relatively low, and reaction temperature is at 40~110 DEG C, normal pressure.For gained catalyst under visible light conditions, non precious metal platinum cocatalyst auxiliary shows excellent catalytic activity.
Description
Technical field
The present invention relates to hydroiodic acid is catalytically decomposed under visible light to prepare hydrogen, and in particular to double halides perovskite light
The preparation and its application of catalyst.
Background technique
In the modernized society of global economy and scientific and technological level fast lifting, environmental problem early has become the concern of people
One of focus.Energy and environment pollution problem influences people's life bring to embody more obvious, water environment in recent years
Pollution, haze air etc. threaten people's health, and in short supply the also having to by people of another aspect petroleum coal resources
Attention.Therefore, clean energy resource is developed, the use for wideling popularize clean fuel becomes solves the problems, such as energy and environment at present
One of important channel.
The Driven by Solar Energy division of halogen acids (HX) is to prepare one of Main way of hydrogen, is to solve energy and environmental problem
Excellent approach.In addition, oxidation reaction produces increment chemical substance, such as I while being related to HX cracking2/I3 -, in the energy and
It serves many purposes in health industry.In 2017, Korean science man Nam was by perovskite CH3NH3PbI3It applies in photodissociation hydrogen iodine
In sour hydrogen preparation field, and achieve huge progress.However, CH3NH3PbI3It is easily compound with hole that there are light induced electrons, light utilization efficiency
Low disadvantage limits it in the application of energy field.Therefore it needs to develop new catalyst.
Summary of the invention
The technical problems to be solved by the present invention are: providing, a kind of catalytic capability is strong, and synthesis technology is simple, operating condition temperature
With the double halides perovskite catalyst preparation methods of economic and practical photocatalysis hydroiodic acid decomposing hydrogen-production.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows: a kind of photochemical catalyst preparation method, including
Following steps:
1) according to chemical general formula APbI3-xBxMiddle element molar ratio carry out ingredient, weigh AI, PbI of corresponding amount2、AB、
PbB2, as perovskite persursor material, A is one of methylamino, carbonamidine base and dimethylamino or a variety of mixing organic groups
Group, B is bromine or chlorine, wherein 0 < x < 3, preferably 0.05≤x≤0.2;
2) according to the mole of persursor material, the persursor material in step 1) is dissolved in organic solvent, preferred disposition
The perovskite precursor liquid that concentration at Pb is 0.1-5mol/L, organic solvent are gamma-butyrolacton (GBL), N, N- dimethyl formyl
The mixed solution of one or both of amine (DMF) and dimethyl sulfoxide (DMSO).
3) it under agitation by the obtained perovskite precursor liquid of step 2), is kept for 2~10 hours for 40~110 DEG C;
4) the resulting perovskite solution of the step 3) is heated, 50~120 DEG C are kept for 4~20 hours, and solvent steams
Hair, is precipitated with crystal grain;
5) perovskite crystal obtained by step 4) is multiple using ether centrifuge washing, and be centrifuged;
6) perovskite crystal obtained by step 5) is dried and is such as dried at 60 DEG C, APbI is made3-xBxPhotochemical catalyst.
The invention also includes the APbI of above-mentioned photochemical catalyst preparation method preparation3-xBxPhotochemical catalyst is in photocatalysis hydroiodic acid
Separation produces the application in hydrogen.
It specifically includes: the halogen acids mixed solution containing HI and HBr being added in Xiang Shiying photo catalysis reactor, is then added
Double halides perovskites to solution is saturated, and double halides perovskites are added on the basis of solution saturation, are divided with pure nitrogen gas air-blowing 30
Then clock is sealed and is irradiated under 300W xenon lamp.
The beneficial effects of the present invention are: mixed anion type perovskite system is used, crystal defect is improved, extends
Carrier lifetime enhances carrier transport, therefore improves perovskite crystal photocatalysis performance and stability.
The features such as preparation method that the present invention uses has simple process and low cost, and preparation condition is mild.
Detailed description of the invention
Fig. 1 is sample CH obtained by the present invention3NH3PbI3-xBrx(x=0,0.05,0.10,0.15,0.20) X-ray powder
Last diffracting spectrum.
Fig. 2 is sample CH obtained by the present invention3NH3PbI3-xBrx(x=0,0.05,0.10,0.15,0.20) it is ultraviolet-can
Light-exposed abosrption spectrogram.
Fig. 3 is sample CH obtained by the present invention3NH3PbI3-xBrx(x=0,0.05,0.10,0.15,0.20) forbidden band is wide
Spend distribution map
Fig. 4 is sample CH obtained by the present invention3NH3PbI3-xBrx(x=0,0.05,0.10,0.15,0.20) photocatalysis
Produce hydrogen activity comparison.
Specific embodiment
In order to describe the present invention in more detail, spy lifts following example, and but not limited to this.
Embodiment 1
Double halides perovskite photochemical catalyst CH are prepared in the present embodiment3NH3PbI3-xBrxMethod it is as follows:
1) according to chemical general formula CH3NH3PbI2.7Br0.3Proportion, take the 2mmol lead iodide (PbI of corresponding amount2)、
1.8mmol methylpyridinium iodide amine (CH3NH3) and 0.2mmol methyl bromide amine (CH I3NH3Br it) (is adjusted as perovskite persursor material
Whole CH3NH3I and CH3NH3The ratio of Br can obtain the CH of other bromine dopings3NH3PbI3-xBrxPersursor material);
2) persursor material is dissolved in 1mL gamma-butyrolacton (GBL), configures the perovskite precursor liquid of 2mol/L, solution
Yellowly;
3) under the conditions of magnetic agitation by step 2) acquired solution, in nitrogen atmosphere, 70 DEG C are kept for 8 hours;
4) the step 3) solution is heated 12 hours in 110 DEG C of heating mantle, until solvent evaporating completely, remains black
Crystal grain.
5) crystal grain obtained by step 4) is used ether centrifuge washing 3 times, is centrifuged 8min under the revolving speed of 8000r/min;
6) by the 60 DEG C of vacuumizing and dryings in a vacuum drying oven of crystal grain obtained by step 5), CH is made3NH3PbI2.7Br0.3Light is urged
Agent.
Embodiment 2
CH is prepared according to the method for embodiment 13NH3PbI3-xBrx, x=0,0.05,0.10,0.15,0.20.
It is as follows to the method for material prepared progress photocatalytic activity test in embodiment:
Photocatalyzed Hydrogen Production test is the progress in the system of closed quartz test tube (volume 60mL) (under atmospheric pressure).Irradiation
Light source selects is the 300W xenon lamp equipped with 420nm optical filter.Sample is evaluated by chromatographic hydrogen output
Photocatalytic activity.By double halides perovskite CH3NH3PbI2.7Br0.3Being added to the mixed solution of 20mL halogen acids, (HI:HBr rubs
You are than adding the bis- halides perovskites of 50mg on the basis of solution saturation, being divided with high pure nitrogen air-blowing 30 to be extremely saturated in 9:1)
Then clock is sealed and is irradiated under 300W xenon lamp, sample 500 μ L gases manually, carry out analysis detection with gas chromatograph.
Experimental result:
Fig. 1 illustrates the CH of different bromine dopings of the invention3NH3PbI3-xBrxX ray diffracting spectrum, it can be seen that
Synthesized CH3NH3PbI3-xBrxThere are not other miscellaneous peaks, component is purer.The incorporation of bromine keeps diffraction maximum position inclined to high angle
It moves, part tetragonal phase crystallographic plane diffraction peak (004) crystal face disappears, and cubic phase crystallographic plane diffraction peak (220) crystal face accounts for leading, this is illustrated
Bromo element is successfully doped into perovskite crystal structure.
Fig. 2 illustrates the CH of different bromine dopings3NH3PbI3-xBrxUv-visible absorption spectroscopy figure, can from figure
To find out the raising with bromine doping, absorbs band edge and small blue shift occurs, but absorption region still covers entire visible-range,
This illustrates that bromo element is successfully doped into perovskite crystal structure.
Fig. 3 illustrates the CH of different bromine dopings3NH3PbI3-xBrxForbidden bandwidth distribution map, as can be seen from the figure with
The increase of bromine doping, catalyst forbidden bandwidth gradually increase, show longer carrier diffusion distance, less current-carrying
Son is compound.
Fig. 4 illustrates the CH of different bromine dopings3NH3PbI3-xBrxPhotochemical catalyst is used for the curve of Photocatalyzed Hydrogen Production, by scheming
4 it is found that under visible light, CH3NH3PbI2.7Br0.1Hydrogen output is up to 1471 μm of olh-1g-1, production hydrogen activity is apparently higher than single
Halogenated perovskite is 40 times of its performance or so, and is higher by 8 times or so than the single halogenated perovskite of platinum load.This explanation
Double halides perovskites of bromine doping can be used as novel photocatalyst photocatalysis hydroiodic acid decomposing hydrogen-production, and without the negative of platinum
It carries.
Claims (6)
1. a kind of double halides perovskite photochemical catalysts, which is characterized in that chemical general formula APbI3-xBx, A is methylamino, carbonamidine base
With one of dimethylamino or a variety of mixing organic groups, B is bromine or chlorine, wherein 0 < x < 3.
2. a kind of double halides perovskite photochemical catalysts described in accordance with the claim 1, which is characterized in that 0.05≤x≤0.2.
3. the method for preparing a kind of double halides perovskite photochemical catalysts of any of claims 1 or 2, which is characterized in that including
Following steps:
1) according to chemical general formula APbI3-xBxMiddle element molar ratio carry out ingredient, weigh AI, PbI of corresponding amount2、AB、
PbB2, as perovskite persursor material;
2) according to the mole of persursor material, the persursor material in step 1) is dissolved in organic solvent, organic solvent is γ-
The mixed solution of one or both of butyrolactone (GBL), n,N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO);
3) it under agitation by the obtained perovskite precursor liquid of step 2), is kept for 2~10 hours for 40~110 DEG C;
4) the resulting perovskite solution of the step 3) is heated, 50~120 DEG C are kept for 4~20 hours, solvent evaporation, companion
There is crystal grain precipitation;
5) perovskite crystal obtained by step 4) is multiple using ether centrifuge washing, and be centrifuged;
6) perovskite crystal obtained by step 5) is dried, APbI is made3-xBxPhotochemical catalyst.
4. according to the method for claim 3, which is characterized in that step 2) is configured to the calcium that the concentration of Pb is 0.1-5mol/L
Titanium ore precursor liquid.
5. a kind of application of double halides perovskite photochemical catalysts of any of claims 1 or 2 is separated in photocatalysis hydroiodic acid and is produced
Application in hydrogen.
6. according to the application of claim 5, which is characterized in that the hydrogen containing HI and HBr is added in Xiang Shiying photo catalysis reactor
Then hydracid mixed solution is added double halides perovskites to solution and is saturated, double halides calcium are added on the basis of solution saturation
Then titanium ore was sealed and was irradiated under 300W xenon lamp with pure nitrogen gas air-blowing 30 minutes.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811536577.9A CN109569727B (en) | 2018-12-14 | 2018-12-14 | Preparation and application of high-efficiency hydrogen-producing double-halide perovskite photocatalyst |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811536577.9A CN109569727B (en) | 2018-12-14 | 2018-12-14 | Preparation and application of high-efficiency hydrogen-producing double-halide perovskite photocatalyst |
Publications (2)
Publication Number | Publication Date |
---|---|
CN109569727A true CN109569727A (en) | 2019-04-05 |
CN109569727B CN109569727B (en) | 2020-11-20 |
Family
ID=65928724
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811536577.9A Active CN109569727B (en) | 2018-12-14 | 2018-12-14 | Preparation and application of high-efficiency hydrogen-producing double-halide perovskite photocatalyst |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109569727B (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111185228A (en) * | 2020-02-23 | 2020-05-22 | 吉林大学 | Carbonized polymer dot/perovskite composite photocatalyst, preparation method and application thereof in aspect of producing hydrogen by photocatalytic cracking of HI |
CN113122041A (en) * | 2021-05-11 | 2021-07-16 | 陕西科技大学 | High-efficiency antibacterial leather finishing agent containing double-component halide perovskite and preparation method thereof |
CN114377724A (en) * | 2022-01-27 | 2022-04-22 | 山东大学 | Halide perovskite-based platinum monatomic photocatalytic material and preparation method and application thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104332560A (en) * | 2014-09-04 | 2015-02-04 | 武汉大学 | Preparation method of chlorine-bromine-iodine-mixing perovskite light absorption layer material |
CN104617219A (en) * | 2014-12-26 | 2015-05-13 | 西安电子科技大学 | Planar perovskite solar cell based on CH3NH3PbI<2+x>Cl<1-x> optical active layer and preparation method thereof |
CN105895916A (en) * | 2015-02-13 | 2016-08-24 | 北京大学 | Preparation method of organic and inorganic hybrid perovskite material and new application |
CN107876087A (en) * | 2017-11-03 | 2018-04-06 | 山东大学 | The preparation of methylamine lead iodine redox graphene composite photocatalyst material and its application of photocatalysis hydrogen production |
CN108258120A (en) * | 2018-01-12 | 2018-07-06 | 北京化工大学 | A kind of perovskite solar cell inexpensively stablized and the photoelectrocatalysidevice device of driving |
CN108682746A (en) * | 2018-04-25 | 2018-10-19 | 中国科学院合肥物质科学研究院 | A kind of surface is modified organic inorganic hybridization perovskite material and method of modifying and application |
-
2018
- 2018-12-14 CN CN201811536577.9A patent/CN109569727B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104332560A (en) * | 2014-09-04 | 2015-02-04 | 武汉大学 | Preparation method of chlorine-bromine-iodine-mixing perovskite light absorption layer material |
CN104617219A (en) * | 2014-12-26 | 2015-05-13 | 西安电子科技大学 | Planar perovskite solar cell based on CH3NH3PbI<2+x>Cl<1-x> optical active layer and preparation method thereof |
CN105895916A (en) * | 2015-02-13 | 2016-08-24 | 北京大学 | Preparation method of organic and inorganic hybrid perovskite material and new application |
CN107876087A (en) * | 2017-11-03 | 2018-04-06 | 山东大学 | The preparation of methylamine lead iodine redox graphene composite photocatalyst material and its application of photocatalysis hydrogen production |
CN108258120A (en) * | 2018-01-12 | 2018-07-06 | 北京化工大学 | A kind of perovskite solar cell inexpensively stablized and the photoelectrocatalysidevice device of driving |
CN108682746A (en) * | 2018-04-25 | 2018-10-19 | 中国科学院合肥物质科学研究院 | A kind of surface is modified organic inorganic hybridization perovskite material and method of modifying and application |
Non-Patent Citations (3)
Title |
---|
SAMUEL D. STRANKS ET AL.: ""Electron-Hole Diffusion Lengths Exceeding 1 Micrometer in an Prganometal Trihalide Perovskite Absorber"", 《SCIENCE》 * |
SUNGHAK PARK ET AL.: ""Photocatalytic hydrogen generation from hydriodic acid using methylammonium lead iodide in dynamic equilibrium with aqueous solution"", 《NATURE ENERGY》 * |
WAN-JIAN YIN ET AL.: ""Anomalous Alloy Properties in Mixed Halide Perovskites"", 《THE JOURNAL OF PHYSICAL CHEMISTRY LETTERS》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111185228A (en) * | 2020-02-23 | 2020-05-22 | 吉林大学 | Carbonized polymer dot/perovskite composite photocatalyst, preparation method and application thereof in aspect of producing hydrogen by photocatalytic cracking of HI |
CN111185228B (en) * | 2020-02-23 | 2022-11-04 | 吉林大学 | Carbonized polymer dot/perovskite composite photocatalyst, preparation method and application thereof in aspect of producing hydrogen by photocatalytic cracking of HI |
CN113122041A (en) * | 2021-05-11 | 2021-07-16 | 陕西科技大学 | High-efficiency antibacterial leather finishing agent containing double-component halide perovskite and preparation method thereof |
CN113122041B (en) * | 2021-05-11 | 2022-04-01 | 陕西科技大学 | High-efficiency antibacterial leather finishing agent containing double-component halide perovskite and preparation method thereof |
CN114377724A (en) * | 2022-01-27 | 2022-04-22 | 山东大学 | Halide perovskite-based platinum monatomic photocatalytic material and preparation method and application thereof |
Also Published As
Publication number | Publication date |
---|---|
CN109569727B (en) | 2020-11-20 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Wang et al. | Revealing the role of oxygen vacancies in bimetallic PbBiO2Br atomic layers for boosting photocatalytic CO2 conversion | |
Zhang et al. | An etching and re-growth method for the synthesis of bismuth ferrite/MIL-53 (Fe) nanocomposite as efficient photocatalyst for selective oxidation of aromatic alcohols | |
Guan et al. | Photoreduction of carbon dioxide with water over K2Ti6O13 photocatalyst combined with Cu/ZnO catalyst under concentrated sunlight | |
Chiarello et al. | Photocatalytic hydrogen production by liquid-and gas-phase reforming of CH3OH over flame-made TiO2 and Au/TiO2 | |
CN109569727A (en) | A kind of preparation and application of double halides perovskite photochemical catalysts of highly effective hydrogen yield | |
CN110368924B (en) | Bismuth titanate/bismuth vanadate composite photocatalyst and application thereof in photothermal catalytic purification of organic gas pollutants | |
CN110882705B (en) | Microwave synthesis oxygen vacancy BiOCl/Bi 2 S 3 Catalyst and preparation method and application thereof | |
CN109174145B (en) | Dimolybdenum carbide/titanium dioxide composite photocatalyst and preparation method and application thereof | |
CN112076777B (en) | For CO2Reduced photocatalyst and preparation method thereof | |
CN113198496B (en) | Metallic indium-doped lead cesium bromide perovskite quantum dot photocatalyst, preparation method and application thereof in reduction of carbon dioxide | |
CN110394194B (en) | Controllable preparation method of novel photocatalyst based on inorganic ligand modification | |
CN108355701A (en) | Ag supports two-dimentional graphite phase carbon nitride nanosheet photocatalyst and its preparation method and application | |
CN114377724B (en) | Halide perovskite-based platinum monoatomic photocatalytic material and preparation method and application thereof | |
He et al. | Preparation, characterization and activity evaluation of V2O5–LaVO4 composites under visible light irradiation | |
Li et al. | Photocatalytic performance of TiO2/Bi2WO6 photocatalysts with trace Fe3+ dopant for gaseous toluene decomposition | |
Liu et al. | Visible-light-driven photocatalysis over nano-TiO2 with different morphologies: From morphology through active site to photocatalytic performance | |
US5346679A (en) | Method for reduction of carbon dioxide, catalyst for the reduction, and method for production of the catalyst | |
He et al. | Facile synthesis of Bi2O3 nanocrystals for photocatalytic NO oxidation and its conversion pathway via in situ DRIFTS | |
Muraoka et al. | Oxygen‐Doped Ta3N5 Nanoparticles for Enhanced Z‐Scheme Carbon Dioxide Reduction with a Binuclear Ruthenium (II) Complex under Visible Light | |
CN111957333A (en) | Yb (Yb)2O3/g-C3N4Preparation method and application of bifunctional catalyst | |
CN107486213A (en) | A kind of hollow BiVO4The preparation method of micron film photochemical catalyst | |
CN110787829B (en) | Mo nanosphere cocatalyst and preparation method and application thereof | |
CN109876826B (en) | Preparation method of sulfur-rich vacancy photocatalyst | |
CN115025783B (en) | Synthetic method and application of multi-niobium oxygen cluster/ZIF-67 derivative composite material | |
CN113522273B (en) | Preparation method of oxygen vacancy-rich tungsten trioxide and application of oxygen vacancy-rich tungsten trioxide in photocatalytic reaction |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |