CN108144607A - Iridium acid strontium class catalyst, preparation method and its application in terms of electro-catalysis cracks acid aquatic products oxygen - Google Patents
Iridium acid strontium class catalyst, preparation method and its application in terms of electro-catalysis cracks acid aquatic products oxygen Download PDFInfo
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- CN108144607A CN108144607A CN201711426794.8A CN201711426794A CN108144607A CN 108144607 A CN108144607 A CN 108144607A CN 201711426794 A CN201711426794 A CN 201711426794A CN 108144607 A CN108144607 A CN 108144607A
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Abstract
A kind of pure phase iridium acid strontium class catalyst, preparation method and its application in terms of efficient electric catalytic pyrolysis acidity aquatic products oxygen, belong to inorganic functional material field.It is to be evaporated iridium source, organic polyhydric alcohol, barium source, organic multicomponent acid and water by different proportion Hybrid Heating, then the reactant being evaporated is calcined into a period of time, the obtained hydrochloric acid of 0.5~2mol/L of product, sulfuric acid, perchloric acid etc. will be calcined again and impregnates 3~10h, you can obtain out of phase iridium acid strontium.The wherein monoclinic phase iridium acid strontium SrIrO of gained3Crystallinity is high, in the hexagon piece of rule, can replace traditional acid water oxidation catalyst iridium dioxide, reduce the dosage of precious metal iridium to a certain extent.Its electro-catalysis water crack parsing oxygen current density reaches 10mA/cm2When, it is only necessary to overpotential 248mV, the latent active highest in the water-splitting oxygen-separating catalyst reported at present, far better than current industry noble metal catalyst, and performance is stablized unattenuated, has broad application prospects.
Description
Technical field
The invention belongs to inorganic functional material fields, and in particular to a series of pure phase iridium acid strontium class catalyst, preparation method
And its application in terms of efficient electric catalytic pyrolysis acidity aquatic products oxygen.
Background technology
With the rapid development of economic society, increased population, energy problem is increasingly prominent.Develop in sustainable energy and lead
In domain, such as fuel cell and electro-catalysis production hydrogen, electro-chemical water cracking production oxygen reaction is most important, but produces oxygen kinetics
Limit its catalytic performance and commercial applications.In acid water oxidation, problem more highlights, and most of catalysis material is in strong acid
It is difficult to stablize with producing under oxygen overpotential.Traditional metal oxide containing precious metals (IrO2, RuO2) there is catalyst higher acid water to aoxidize
(OER) it is active, RuO2The excellent in the catalysis of electrochemistry acidity water oxygenization, but stability is very poor.IrO2In electrochemistry water oxygen
It is showed well in change, but expensive and scarcity of resources limits its large-scale application.So find substitution precious metal iridium
Oxide or the dosage for reducing precious metal iridium, and the catalysis material with better acid water oxidation production oxygen activity and stability is
The key of acid water-splitting production oxygen.
In in recent years, with the propulsion of correlative study, a series of acid production VPO catalysts are developed.For example, have
The IrO of oxygen activity is produced in the water-splitting of high intrinsic acidityx/SrIrO3(Science 2016 volume 353 page 1011)；Iridium base double-perovskite
Type High-efficient Water oxidation catalyst (volume 7 page 12363 of Nat.Commun.2016) and hydro-thermal method synthesize pyrochlore constitution
Bi2Ir2O7Produce VPO catalysts (volume 24 page 4192 of Chem.Mater.2014).Although these catalyst property in terms of acidity produces oxygen
Matter is better, but its synthetic method is all complex, needs template-mediated crystalline phase synthetic method or high temperature and pressure solid phase mostly
Synthetic method.It in view of the above-mentioned problems, we use more pervasive sol-gal process, can generate, generate under normal pressure (101.325kPa)
The acid water oxidation activity of object is more excellent and stablizes, can be as very excellent acid water splitting water oxidation catalyst material.
Invention content
The present invention has been synthesized a series of out of phase iridium acid strontium classes and has been urged for the purpose of synthesizing efficient acid water oxidation catalyst
Agent, wherein monoclinic phase iridium acid strontium SrIrO3With highest acid production oxygen activity, appearance and size is in six square pieces of nano-micro level,
Realize the application in terms of efficiently acid water oxygen；Orthorhombic phase iridium acid strontium SrIrO3Acid water oxidation activity has been reported,
Latent active highest in the acid water oxidation catalyst of report, prior synthesizing method is more difficult, needs high temperature and pressure or crystalline substance
Mutually induce.We are realized with a kind of normal pressure (101.325kPa) method i.e. sol-gal process synthesis orthorhombic phase iridium acid in the present invention
Strontium；Wherein cubic phase Sr2Ir3O8Synthetic method is mostly synthesis in solid state in the document reported, and cannot synthesize pure phase.This hair
The bright metering by regulating compound, discovery is a series of can to synthesize pure phase Sr2Ir3O8Proportioning, and successfully synthesize pure
The cubic phase Sr of phase nano-micro level2Ir3O8Cubic block.
The iridium acid strontium class catalyst being previously mentioned of the present invention is by iridium source, organic polyhydric alcohol, barium source, organic multicomponent acid and water
It is evaporated by certain proportion Hybrid Heating, then calcines the reactant being evaporated a period of time, then obtained product use will be calcined
Hydrochloric acid, sulfuric acid, perchloric acid of 0.5~2mol/L etc. impregnate 3~10h, you can obtain respective compound.
To obtain out of phase iridium acid strontium, the mole that we fix iridium source is na, by the mole n for adjusting barium sourcebWith
The mole n of organic multicomponent acidc, obtain a series of out of phase iridium acid strontium compounds；Concrete operation step is as follows：
First, monoclinic phase iridium acid strontium SrIrO3The preparation of catalyst：
(1) configuration of mixed solution：Weigh ncMole organic multicomponent acid, nbMole barium source and naMole iridium source,
In, nc：nb：na=8：4：1、8：8：1、8：16：1 or 8：24：1, it is then added in the mixed solution of organic multicomponent alcohol and water and mixes
It closes uniform；
(2) drying and calcination：The mixed solution that step (1) is obtained dry 5~10h in 120~200 DEG C of environment, will
The last heating rate with 0.5~5 DEG C/min of dried solid sample pulverizing heats up, then 120~220 DEG C, 230
1~10h, 1~10h, 2~4h and 1~10h, natural cooling are heated respectively at~320 DEG C, 330~520 DEG C and 620~720 DEG C
Black powder is obtained to room temperature；
(3) acid processing：The hydrochloric acid of 0.5~2mol/L of black powder, sulfuric acid, the perchloric acid that step (2) is finally obtained
It Deng 6~10h of immersion, is cleaned with ethyl alcohol, monoclinic phase iridium acid strontium SrIrO is obtained after dry3Catalyst.
2nd, orthorhombic phase iridium acid strontium SrIrO3The preparation of catalyst：
(1) configuration of mixed solution：Weigh ncMole organic multicomponent acid, nbMole barium source and naMole iridium source,
In, nc：nb：na=12~40：8：1, it is then added in the mixed solution of organic multicomponent alcohol and water and is uniformly mixed；
(2) drying and calcination：The mixed solution that step (1) is obtained dry 5~10h in 120~200 DEG C of environment, will
Dried solid sample grind into powder is heated up with the heating rate of 0.5~5 DEG C/min, then 120~220 DEG C, 230~
1~10h, 1~10h, 2~4h and 1~10h are heated respectively at 320 DEG C, 330~520 DEG C and 620~720 DEG C, are naturally cooled to
Room temperature obtains black powder；
(3) acid processing：The hydrochloric acid of 0.5~2mol/L of black powder, sulfuric acid, the perchloric acid that step (2) is finally obtained
It Deng 6~10h of immersion, is cleaned with ethyl alcohol, orthorhombic phase iridium acid strontium SrIrO is obtained after dry3Catalyst.
3rd, cubic phase Sr2Ir3O8The preparation of cubic block catalyst：
(1) configuration of mixed solution：Weigh ncMole organic multicomponent acid, nbMole barium source and naMole iridium source,
In, nc：nb：na=0~4：4~10：1, it is then added in the mixed solution of organic multicomponent alcohol and water and is uniformly mixed；
(2) drying and calcination：The mixed solution that step (1) is obtained dry 5~10h in 120~200 DEG C of environment, will
Dried solid sample grind into powder is heated up with the heating rate of 0.5~5 DEG C/min, then 120~220 DEG C, 230~
1~10h, 1~10h, 2~4h and 1~10h are heated respectively at 320 DEG C, 330~520 DEG C and 620~720 DEG C, are naturally cooled to
Room temperature obtains black powder；
(3) acid processing：The hydrochloric acid of 0.5~2mol/L of black powder, sulfuric acid, the perchloric acid that step (2) is finally obtained
It Deng 6~10h of immersion, is cleaned with ethyl alcohol, cubic phase Sr is obtained after dry2Ir3O8Cubic block catalyst.
In the above method, iridium source includes but not limited to the sour potassium of chlordene iridium (IV), the sour potassium of chlordene iridium (III), iridium chloride, chlorine iridium
Acid etc. or its mixture.
In the above method, barium source includes but not limited to strontium nitrate, strontium chloride, strontium hydroxide, strontium carbonate etc. or its mixture.
In the above method, organic multicomponent alcoholic solvent includes but not limited to the polyol solvents such as ethylene glycol, glycerine.
In the above method, organic multicomponent acid includes but not limited to the polycarboxylic compounds such as citric acid, tartaric acid, oxalic acid.
In the above method, nc：nb：naMolar ratio be not limited to the ratio listed, suitably adjust triadic relation, can be with
Synthesize the pure phase of three kinds of substances.
Advantageous effect
1. synthesis technology is simple, experimental arrangement facilitates controllable, short preparation period, reproducible, can mass production.
2. the monoclinic phase iridium acid strontium SrIrO of gained3Crystallinity is high, in the hexagon piece of rule, inside crystal structure
Distinctive iridium oxygen octahedra coplanar connection structure optimizes the shortcomings that iridium oxygen key key oxygen ability itself is too strong, material is made to have in itself
There are fabulous acid water splitting water oxidation activity and stability.Traditional acid water oxidation catalyst iridium dioxide can be replaced,
The dosage of precious metal iridium is reduced to a certain extent, is had broad application prospects.
3. the orthorhombic phase iridium acid strontium SrIrO of gained3For the powder body material of nano-micro level, in existing report, this method
Synthesis technology is the simplest controllable, and sample purity is high.It can be changed into IrO in oxygen is produced in acid water-splittingx/SrIrO3, have higher
Acid water splitting water oxidation activity.
4. the cubic phase Sr of gained2Ir3O8Cubic block powder body material is equal with high crystallinity and purity and appearance and size
One is adjustable, by changing the type in iridium source, can realize Sr2Ir3O8Cube block size from micron order to nanoscale between transformation.
In existing report, which is to synthesize pure phase for the first time, and method is simply controllable.
Description of the drawings
Fig. 1:Monoclinic phase iridium acid strontium SrIrO in embodiment 13X-ray diffraction (XRD) collection of illustrative plates (figure A)；Orthorhombic phase iridium acid strontium
SrIrO3X-ray diffraction (XRD) collection of illustrative plates (figure B)；Cubic phase Sr2Ir3O8X-ray diffraction (XRD) collection of illustrative plates (figure C).
Fig. 2：Six square piece iridium acid strontium SrIrO of monoclinic phase in embodiment 13Scanning electron microscope (SEM) photo (figure A)；Orthorhombic phase block
Shape iridium acid strontium SrIrO3Scanning electron microscope (SEM) photo (figure B)；Cubic block Sr2Ir3O8Scanning electron microscope (SEM) photo (figure C).
Fig. 3：Using 1 product of the embodiment of the present invention as water-splitting catalyst, in acidic buffer solution (0.5M H2SO4) in water crack
Parse the polarization curve of oxygen (OER)；Monoclinic phase iridium acid strontium SrIrO3Water crack parsing oxygen polarization curve (figure A)；Orthorhombic phase iridium acid strontium
SrIrO3Water crack parsing oxygen polarization curve (figure B)；Cubic phase Sr2Ir3O8Water crack parsing oxygen polarization curve (figure C).
Fig. 4：Using 1 product of the embodiment of the present invention as water-splitting catalyst, in acidic buffer solution (0.5M H2SO4) in water crack
Parse the stability curve of oxygen (OER).Monoclinic phase iridium acid strontium SrIrO3Water crack parsing oxidative stability curve (figure A)；Orthorhombic phase iridium
Sour strontium SrIrO3Water crack parsing oxidative stability curve (figure B)；Cubic phase Sr2Ir3O8Water crack parsing oxidative stability curve (figure C).
Specific embodiment
The invention will be further described by way of example and in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to
Following embodiments.It it will be apparent to those skilled in the art that can be to the present invention in the case of without departing from spirit and scope of the present invention
Variation or adjustment are made, these variations or adjustment are also included in protection scope of the present invention.
Embodiment 1
Monoclinic phase iridium acid strontium SrIrO3Preparation：First, the sour potassium of 80mg (0.166mmol) chlordene iridium (IV) is put into 4mL
In ethylene glycol, it is stirred at room temperature to dissolving completely, for dark-brown clear solution, referred to as solution a.By 280mg (1.332mmol) lemon
Strontium nitrate is dissolved in 5mL distilled water by acid and 280mg (1.323mmol), is stirred at room temperature to colourless transparent solution, referred to as solution
b.Solution b is added drop-wise to dropwise in solution a, mixed solution is evaporated 6h under 180 DEG C of environment after stirring.This implementation
In example, nc：nb：na=8：8：1.Then the solid sample grind into powder that will be evaporated, with the heating rate of 1.7 DEG C/min 200
DEG C, 6h, 6h, 3h and 6h are heated respectively at 300 DEG C, 500 DEG C and 700 DEG C.After furnace cooling, by the salt of black powder 1mol/L
Acid soak 6h, is cleaned with ethyl alcohol, and sample powder is collected after dry.
Orthorhombic phase iridium acid strontium SrIrO3Preparation：First, the sour potassium of 80mg (0.166mmol) chlordene iridium (IV) is put into 4mL
In ethylene glycol, it is stirred at room temperature to dissolving completely, for dark-brown clear solution, referred to as solution a.By 840mg (3.997mmol) lemon
Acid and 280mg (1.323mmol) strontium nitrate are dissolved in 5mL distilled water, are stirred at room temperature to colourless transparent solution, referred to as solution b.
Solution b is added drop-wise to dropwise in solution a, mixed solution is placed under 180 DEG C of environment after stirring and is evaporated 6h.This implementation
In example, nc：nb：na=24：8：1.Then the solid sample grind into powder that will be evaporated, is existed with the heating rate of 1.7 DEG C/min
6h, 6h, 3h and 6h are heated respectively at 200 DEG C, 300 DEG C, 500 DEG C and 700 DEG C.With stove etc. but after, by black powder 1mol/L
Salt acid soak 6h, cleaned with ethyl alcohol, sample powder collected after dry.
Cubic phase Sr2Ir3O8The preparation of cubic block：First, the sour potassium of 80mg (0.166mmol) chlordene iridium (IV) is put into 4mL
In ethylene glycol, it is stirred at room temperature to dissolving completely, for dark-brown clear solution, referred to as solution a.By 140mg (0.662mmol) nitric acid
Strontium is dissolved in 5mL distilled water, is stirred at room temperature to colourless transparent solution, referred to as solution b.Solution b is added drop-wise to solution a dropwise
In, mixed solution is placed under 180 DEG C of environment after stirring and is evaporated 6h.In the present embodiment, nc：nb：na=0：4：1 so
The solid sample grind into powder that will be evaporated afterwards, with the heating rate of 1.7 DEG C/min at 200 DEG C, 300 DEG C, 500 DEG C and 700 DEG C
It is lower to heat 6h, 6h, 3h and 6h respectively.With stove etc. but after, the salt acid soak 6h of black powder 1mol/L is cleaned with ethyl alcohol,
Sample powder is collected after drying.
Electro-catalysis water crack parsing oxygen (OER) property is carried out in standard three electrode electrolytic cell to material prepared by the above method
Test；In the naphthols aqueous isopropanol for being 10%~50% in volume content by product mix of the present invention, solution is dropped in into platinum carbon
As working electrode in electrolytic cell on electrode；Reference electrode is saturated calomel electrode, to electrode be platinum filament, electrolyte 0.5M
H2SO4.It is it should be noted that all equal in property figure by the potential that reference electrode obtains of saturation calomel in electro-catalysis test
Reversible hydrogen electrode potential is converted to, external power supply is electrochemical workstation main battery.
The material prepared to the above method has carried out some structures and performance study.Figure 1A is the monoclinic phase iridium acid strontium obtained
SrIrO3X-ray diffraction (XRD) collection of illustrative plates；Figure 1B is the orthorhombic phase iridium acid strontium SrIrO obtained3X-ray diffraction (XRD)；Fig. 1 C are
The cubic phase Sr of acquisition2Ir3O8Cubic block X-ray diffraction (XRD).It will be seen that in this way obtaining from Fig. 1
Iridium acid strontium class compound is pure phase.
Fig. 2 is scanning electron microscope (SEM) photo of the iridium acid strontium class compound obtained, and Fig. 2A shows the monoclinic phase iridium obtained acid
The hexagon that strontium diameter is about 1 μm, thickness is about 50nm.Fig. 2 B show the orthorhombic phase iridium acid strontium obtained for micron-sized blocky sample
Product.Fig. 2 C show the cubic phase Sr obtained2Ir3O8The cubic block that the square length of side is about 200nm or so.
It is water-splitting catalyst in acid sulfuric acid (0.5M H that Fig. 3, which is product of the present invention,2SO4) water crack parsing oxygen in solution
(OER) polarization curve.Fig. 3 A are monoclinic phase iridium acid strontium SrIrO3Water-splitting oxygen evolution reaction polarization curve is in overpotential
248mV reaches current density for 10mA/cm2.Fig. 3 B are orthorhombic phase iridium acid strontium SrIrO3Water-splitting oxygen evolution reaction polarization curve,
Overpotential is 270mV, reaches current density for 10mA/cm2.Fig. 3 C are cubic phase Sr2Ir3O8The polarization of water-splitting oxygen evolution reaction is bent
Line is 295mV in overpotential, reaches current density for 10mA/cm2.Show that three kinds of catalyst all have preferable catalytic activity,
Wherein monoclinic phase iridium acid strontium is the most excellent.
Fig. 4 is that product of the present invention is acid water catalyst for cracking electrolyte sulfuric acid (0.5M H2SO4) in solution water crack parse
The stability curve of oxygen (OER).Fig. 4 A are monoclinic phase iridium acid strontium SrIrO3Current density is maintained at 10mA/cm when water crack parses oxygen2
Reaction overpotential and time graph；Fig. 4 B orthorhombic phase iridium acid strontiums SrIrO3Current density is maintained at 10mA/ when water crack parses oxygen
cm2Reaction overpotential and time graph；Fig. 4 C are cubic phase Sr2Ir3O8Current density is maintained at 10mA/ when water crack parses oxygen
cm2Reaction overpotential and time graph.It is single in the oxygen evolution reaction environment of three kinds of iridium acid strontium class compounds in this test condition
Monoclinic phase iridium acid strontium SrIrO3With highest catalytic stability, in the case where analysing oxygen overpotential, production oxygen activity does not change substantially in 10h
Become, orthorhombic phase iridium acid strontium SrIrO3With cubic phase Sr2Ir3O8Catalytic stability it is more weaker, under production oxidisability slightly has in 10h
Drop.
Embodiment 2
It is same as Example 1, only monoclinic phase iridium acid strontium SrIrO3Preparation in by 280mg (1.323mmol) strontium nitrate
It reduces to 140mg (0.662mmol), at this time nc：nb：na=8：4：1, the amount and condition of other reactants are constant.
Perovskite Phase iridium acid strontium SrIrO3Preparation in the amount of 840mg (3.997mmol) citric acid is reduced to 420mg
(1.999mmol), at this time nc：nb：na=12：8：1, the amount and condition of other reactants are constant.
Cubic phase Sr2Ir3O8Preparation in the amount of 140mg (0.662mmol) strontium nitrate increased into 350mg
(1.654mmol), at this time nc：nb：na=0：10：1, the amount and condition of other reactants are constant.
Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches 10mA/cm2；Orthorhombic phase
Iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block,
When overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 3
It is same as Example 1, only monoclinic phase iridium acid strontium SrIrO3Preparation in by 280mg (1.332mmol) strontium nitrate
Increase as 560mg (2.646mmol), at this time nc：nb：na=8：16：1, the amount and condition of other reactants are constant.
Perovskite Phase iridium acid strontium SrIrO3Preparation in the amount of 840mg (3.969mmol) citric acid increased into 1120mg
(5.330mmol), at this time nc：nb：na=32：8：1, the amount and condition of other reactants are constant.
Cubic phase Sr2Ir3O8Preparation in add in 140mg (0.666mmol) citric acid, at this time nc：nb：na=4：4：1,
The amount and condition of his reactant are constant.
Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches 10mA/cm2；Orthorhombic phase
Iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block,
When overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 4
It is same as Example 1, only monoclinic phase iridium acid strontium SrIrO3Preparation in by 280mg (1.323mmol) strontium nitrate
Increase as 560mg (2.646mmol), at this time nc：nb：na=8：16：1, the amount and condition of other reactants are constant.
Perovskite Phase iridium acid strontium SrIrO3Preparation in the amount of 840mg (3.997mmol) citric acid increased into 1120mg
(5.330mmol), at this time nc：nb：na=32：8：1, the amount and condition of other reactants are constant.
Cubic phase Sr2Ir3O8Preparation in add in 140mg (0.666mmol) citric acid, at this time nc：nb：na=4：4：1,
The amount and condition of his reactant are constant.
Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches 10mA/cm2；Orthorhombic phase
Iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block,
When overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 5
It is same as Example 1, only monoclinic phase iridium acid strontium SrIrO3Preparation in by 280mg (1.323mmol) strontium nitrate
Increase as 840mg (3.969mmol), at this time nc：nb：na=8：24：1, the amount and condition of other reactants are constant.
Perovskite Phase iridium acid strontium SrIrO3Preparation in the amount of 840mg (3.997mmol) citric acid increased into 1400mg
(6.662mmol), at this time nc：nb：na=40：8：1, the amount and condition of other reactants are constant.
Cubic phase Sr2Ir3O8Preparation in add in 140mg (0.666mmol) citric acid, 140mg (0.662mmol) nitric acid
The amount of strontium is increased to 350mg (1.654mmol) n at this timec：nb：na=4：10：1, the amount and condition of other reactants are constant.
Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches 10mA/cm2；Orthorhombic phase
Iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block,
When overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 6
It is same as Example 1, the sour potassium of chlordene iridium (IV) is only changed to the sour potassium of chlordene iridium (III), the molal quantity in iridium source is not
Become, be 0.166mmol.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, the material
Material current density reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches
10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 7
It is same as Example 1, the sour potassium of chlordene iridium (IV) is only changed to chloro-iridic acid hydrate, the molal quantity in iridium source is constant,
For 0.166mmol.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, the material
Current density reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches
10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 8
It is same as Example 1, chlordene iridium (IV) acid potassium in out of phase preparation is only changed to iridium chloride, mole in iridium source
Number is constant, is 0.166mmol.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV,
The material current density reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 275mV, the material current density
Reach 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 9
It is same as Example 1, strontium nitrate in out of phase preparation is only changed to strontium chloride, the mole of barium source is constant.
The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches
10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cube
Phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 10
It is same as Example 1, strontium nitrate in out of phase preparation is only changed to strontium hydroxide, the mole of barium source is not
Become.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches
To 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；It is vertical
Square phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 11
It is same as Example 1, strontium nitrate in out of phase preparation is only changed to strontium carbonate, the mole of barium source is constant.
The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, which reaches
10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cube
Phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 12
It is same as Example 1, citric acid in out of phase preparation is only changed to tartaric acid, prepares monoclinic phase iridium acid strontium
SrIrO3The mole of tartaric acid is 1.332mmol.Prepare orthorhombic phase iridium acid strontium SrIrO3Tartaric acid mole is
3.9996mmol.Prepare cubic phase Sr2Ir3O8Cubic block tartaric acid mole is 0.666mmol.The electrocatalysis of gained sample
Energy：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 260mV, which reaches 10mA/cm2；Orthorhombic phase iridium acid
Strontium SrIrO3, when overpotential is 295mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block has served as
When potential is 310mV, which reaches 10mA/cm2。
Embodiment 13
It is same as Example 1, ethylene glycol is only changed to glycerine, the volume of fixed alcohol is 4mL.The electricity of gained sample is urged
Change performance：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 250mV, which reaches 10mA/cm2；Orthorhombic phase
Iridium acid strontium SrIrO3, when overpotential is 275mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block,
When overpotential is 305mV, which reaches 10mA/cm2。
Embodiment 14
It is same as Example 1, only calcination temperature is become with the heating rate of 2 DEG C/min at 200 DEG C, 300 DEG C, 500
DEG C and 800 DEG C at heat 6h, 6h, 3h and 6h respectively.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, served as
When potential is 265mV, which reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 290mV,
The material current density reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 330mV, the material current is close
Degree reaches 10mA/cm2。
Embodiment 15
It is same as Example 1, only calcination temperature is become with the heating rate of 1.7 DEG C/min at 300 DEG C, 500 DEG C,
6h, 6h, 3h and 6h are heated respectively at 600 DEG C and 700 DEG C.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when
When overpotential is 245mV, which reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 270mV
When, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 300mV, material electricity
Current density reaches 10mA/cm2。
Embodiment 16
It is same as Example 1, only calcination temperature is become with the heating rate of 1.5 DEG C/min at 500 DEG C, 600 DEG C and
6h is heated respectively at 700 DEG C.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 245mV,
The material current density reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 270mV, the material current density
Reach 10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 17
It is same as Example 1, only calcination temperature is become at 600 DEG C and 700 DEG C dividing with the heating rate of 1 DEG C/min
6h is not heated.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 245mV, the material current
Density reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 270mV, which reaches 10mA/
cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 18
It is same as Example 1, only calcination temperature is become to be increased to 700 from room temperature with the heating rate of 1.7 DEG C/min
6h is heated at DEG C.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, material electricity
Current density reaches 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 278mV, which reaches
10mA/cm2；Cubic phase Sr2Ir3O8Cubic block, when overpotential is 315mV, which reaches 10mA/cm2。
Embodiment 19
It is same as Example 1, the hydrochloric acid of the 1mol/L of acid processing is only changed to 0.5M H2SO4Solution.Gained sample
Electrocatalysis characteristic：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 245mV, which reaches 10mA/cm2；Just
Hand over phase iridium acid strontium SrIrO3, when overpotential is 270mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8It is vertical
Square, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 20
It is same as Example 1, the hydrochloric acid of the 1mol/L of acid processing is only changed to 1M HClO4Solution.The electricity of gained sample
Catalytic performance：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 245mV, which reaches 10mA/cm2；It is orthogonal
Phase iridium acid strontium SrIrO3, when overpotential is 270mV, which reaches 10mA/cm2；Cubic phase Sr2Ir3O8Cube
Block, when overpotential is 300mV, which reaches 10mA/cm2。
Embodiment 21
It is same as Example 1, only by acidic catalyst electrolyte sulfuric acid (0.5M H2SO4) solution is changed to 0.1M HClO4
Solution.The electrocatalysis characteristic of gained sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 255mV, the material current density
Reach 10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 278mV, which reaches 10mA/cm2；
Cubic phase Sr2Ir3O8Cubic block, when overpotential is 315mV, which reaches 10mA/cm2。
Embodiment 22
It is same as Example 1, only by acidic catalyst sulfuric acid (0.5M H2SO4) solution is changed to 1M H2SO4Solution.Institute
Obtain the electrocatalysis characteristic of sample：Monoclinic phase iridium acid strontium SrIrO3, when overpotential is 240mV, which reaches
10mA/cm2；Orthorhombic phase iridium acid strontium SrIrO3, when overpotential is 265mV, which reaches 10mA/cm2；Cube
Phase Sr2Ir3O8Cubic block, when overpotential is 290mV, which reaches 10mA/cm2。
Claims (7)
1. the preparation method of an eka-iridium acid strontium catalyst, its step are as follows：
(1) configuration of mixed solution：Weigh ncMole organic multicomponent acid, nbMole barium source and naMole iridium source, wherein,
nc：nb：na=8：4：1、8：8：1、8：16：1 or 8：24：1, it is then added in the mixed solution of organic multicomponent alcohol and water and mixes
Uniformly；
(2) drying and calcination：The mixed solution that step (1) is obtained dry 5~10h in 120~200 DEG C of environment, by drying
The last heating rate with 0.5~5 DEG C/min of solid sample afterwards pulverizing heats up, then 120~220 DEG C, 230~
1~10h, 1~10h, 2~4h and 1~10h are heated respectively at 320 DEG C, 330~520 DEG C and 620~720 DEG C, are naturally cooled to
Room temperature obtains black powder；
(3) acid processing：The leachings such as the hydrochloric acid of 0.5~2mol/L of black powder that step (2) is finally obtained, sulfuric acid, perchloric acid
6~10h is steeped, is cleaned with ethyl alcohol, monoclinic phase iridium acid strontium SrIrO is obtained after dry3Catalyst；
Or,
(1) configuration of mixed solution：Weigh ncMole organic multicomponent acid, nbMole barium source and naMole iridium source, wherein,
nc：nb：na=12~40：8：1, it is then added in the mixed solution of organic multicomponent alcohol and water and is uniformly mixed；
(2) drying and calcination：The mixed solution that step (1) is obtained dry 5~10h in 120~200 DEG C of environment, by drying
Solid sample grind into powder afterwards is heated up with the heating rate of 0.5~5 DEG C/min, then 120~220 DEG C, 230~320
DEG C, heat 1~10h, 1~10h, 2~4h and 1~10h, cooled to room temperature respectively at 330~520 DEG C and 620~720 DEG C
Obtain black powder；
(3) acid processing：The leachings such as the hydrochloric acid of 0.5~2mol/L of black powder that step (2) is finally obtained, sulfuric acid, perchloric acid
6~10h is steeped, is cleaned with ethyl alcohol, orthorhombic phase iridium acid strontium SrIrO is obtained after dry3Catalyst；
Or,
(1) configuration of mixed solution：Weigh ncMole organic multicomponent acid, nbMole barium source and naMole iridium source, wherein,
nc：nb：na=0~4：4~10：1, it is then added in the mixed solution of organic multicomponent alcohol and water and is uniformly mixed；
(2) drying and calcination：The mixed solution that step (1) is obtained dry 5~10h in 120~200 DEG C of environment, by drying
Solid sample grind into powder afterwards is heated up with the heating rate of 0.5~5 DEG C/min, then 120~220 DEG C, 230~320
DEG C, heat 1~10h, 1~10h, 2~4h and 1~10h, cooled to room temperature respectively at 330~520 DEG C and 620~720 DEG C
Obtain black powder；
(3) acid processing：The leachings such as the hydrochloric acid of 0.5~2mol/L of black powder that step (2) is finally obtained, sulfuric acid, perchloric acid
6~10h is steeped, is cleaned with ethyl alcohol, cubic phase Sr is obtained after dry2Ir3O8Cubic block catalyst.
2. the preparation method of eka-iridium acid strontium catalyst as described in claim 1, it is characterised in that：Iridium source is chlordene iridium (IV)
The sour potassium of sour potassium, chlordene iridium (III), iridium chloride, chloro-iridic acid or its mixture.
3. the preparation method of eka-iridium acid strontium catalyst as described in claim 1, it is characterised in that：Barium source is strontium nitrate, chlorine
Change strontium, strontium hydroxide, strontium carbonate or its mixture.
4. the preparation method of eka-iridium acid strontium catalyst as described in claim 1, it is characterised in that：Organic polyhydric alcohol is second two
Alcohol or glycerine.
5. the preparation method of eka-iridium acid strontium catalyst as described in claim 1, it is characterised in that：Organic multicomponent acid is lemon
Acid, tartaric acid or oxalic acid.
A 6. eka-iridium acid strontium catalyst, it is characterised in that：It is to be prepared as the method described in Claims 1 to 5 any one.
7. application of the iridium acid strontium catalyst in terms of electro-catalysis cracks acid aquatic products oxygen described in claim 6.
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