CN108855159A - A kind of phosphatization cobalt and its preparation method and application with the synthesis of Prussian blue derivative - Google Patents
A kind of phosphatization cobalt and its preparation method and application with the synthesis of Prussian blue derivative Download PDFInfo
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- CN108855159A CN108855159A CN201810678362.4A CN201810678362A CN108855159A CN 108855159 A CN108855159 A CN 108855159A CN 201810678362 A CN201810678362 A CN 201810678362A CN 108855159 A CN108855159 A CN 108855159A
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Abstract
The present invention relates to a kind of phosphatization cobalts and its preparation method and application with the synthesis of Prussian blue derivative.The preparation method includes the following steps：S1：Dispersion stabilizer, potassium cobalticyanide and cobalt salt are mixed, reaction is stood, washs the Prussian blue derivative presoma of drying to obtain；S2：1 ~ 3 h is roasted after Prussian blue derivative presoma in S1 is warming up to 350 ~ 450 DEG C under air conditions with the heating rate of 1 ~ 5 DEG C/min up to cobaltosic oxide particle；S3：1 ~ 5h is roasted after cobaltosic oxide particle and phosphorus source are warming up to 285 ~ 350 DEG C under inert gas conditions with the heating rate of 1 ~ 5 DEG C/min to get phosphatization cobalt.Provided by the invention preparation method is simple, reproducible, and raw materials are cheap and easy to get, and product is stablized；The phosphatization cobalt being prepared has good electro catalytic activity and electric conductivity, has good catalytic performance to oxygen evolution reaction.
Description
Technical field
The invention belongs to electrolysis water fields, and in particular to a kind of phosphatization cobalt and its system with the synthesis of Prussian blue derivative
Preparation Method and application.
Background technique
With the rapid development of industry, the energy problem that the mankind are faced is also more severe.Currently, our most of energy
Source comes from fossil fuel.However, the burning of fossil fuel causes serious environmental problem.Electrolysis water has great potentiality
Sustainable and clean hydrogen source is provided, due to its brilliant energy density and environment friendly, this is considered as most being hopeful to take
For the new energy of fossil fuel.As the important component of water decomposition, oxygen evolution reaction is because experience one is complicated
Four electronics（4e）Transfer process leads to slow dynamics, in order to improve the efficiency of water decomposition, to oxygen evolution reaction catalyst
Research has increase.Especially for many years recently, considerable research work concentrates on exploitation non-precious metal catalyst（Such as mistake
Cross metal oxide, nitride, carbide etc.）, rather than some high-cost limited useful catalysts, such as iridium（Ir）And ruthenium
（Ru）Oxide, although they have very high oxygen evolution reaction catalytic activity, reserves are limited, expensive, are not able to satisfy
The mass production demand of electrolysis water.Therefore, exploring can be with the inexpensive oxygen evolution reaction catalyst of large-scale application with important
Meaning.
Up to the present, it has been reported that some pairs of oxygen evolution reactions have the base metal electro-catalysis of good chemical property
Agent, such as transition metal oxide, hydroxide, layered double-hydroxide（LDHs）, sulfide and phosphate etc..In different analysis
Oxygen reacts in elctro-catalyst, the transition metal phosphide reported recently（TMP）It is very promising, not only due to their abundance is high
With it is at low cost, and due to they in alkaline solution have very high alkaline stability.Transition metal phosphide is a kind of more function
Energy material is widely used in energy conversion and storage, catalyst, the fields such as magnetic and photoelectricity.Recent research indicate that with some
Transition metal phosphide（Such as Ni5P4And Fe2P）Equally, cobalt-based phosphide is not only traditional evolving hydrogen reaction in water splitting processes
Catalyst, and be a kind of promising oxygen evolution reaction catalysts.
Recently, Prussian blue similar object（PBA）As for energy related application such as battery, supercapacitor or hydrogen reduction
A kind of new material of reaction and be widely studied.Although multifunctionality and stabilization of the Prussian blue similar object in electrochemical process
Property obtained good exploration, but their applications in water oxygen field only have a few examples.With its metal oxide
It compares, the water decomposition activity of cyanide bridge material is poor.In contrast, oxide derived from Prussian blue similar object, phosphatization
Object, selenides, carbide etc. have had been reported for analysis oxygen and evolving hydrogen reaction.
Therefore, a kind of preparation method of simple process is developed to obtain the Prussian blue of the analysis oxygen catalytic performance for having excellent
The phosphide of analog has important research significance and application value.
Summary of the invention
It is an object of the invention to overcome the defect and deficiency of oxygen evolution reaction catalysts poor activity in the prior art, one is provided
The preparation method for the phosphatization cobalt that kind is synthesized with Prussian blue derivative.Provided by the invention preparation method is simple, repeatability
Good, raw materials are cheap and easy to get, and product is stablized；It is anti-to analysis oxygen that the phosphatization cobalt being prepared can give full play of phosphatization cobalt material
The satisfactory electrical conductivity of the electro catalytic activity and phosphide material answered has good catalytic performance to oxygen evolution reaction, anti-in analysis oxygen
Ying Zhong, 10mA/cm2Current potential corresponding to current density is lower than 1.6000V vs.RHE.
Another object of the present invention is to provide the phosphatization cobalts that above-mentioned preparation method is prepared.
Application another object of the present invention is to provide above-mentioned phosphatization cobalt as catalyst in oxygen evolution reaction.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of the phosphatization cobalt with the synthesis of Prussian blue derivative, includes the following steps：
S1：Dispersion stabilizer, potassium cobalticyanide and cobalt salt are mixed, stand reaction, drying to obtain is Prussian blue spreads out for washing
Eobiont body；The dispersion stabilizer is one or more of polyvinylpyrrolidone or neopelex；Institute
The molar ratio for stating potassium cobalticyanide and cobalt salt is 1 ~ 2:3；
S2：Prussian blue derivative presoma in S1 is warming up under air conditions with the heating rate of 1 ~ 5 DEG C/min
1 ~ 3 h is roasted after 350 ~ 450 DEG C up to cobaltosic oxide particle；
S3：Cobaltosic oxide particle and phosphorus source are warming up to 285 under inert gas conditions with the heating rate of 1 ~ 5 DEG C/min ~
1 ~ 5h is roasted after 350 DEG C to get phosphatization cobalt；The molar ratio of the cobaltosic oxide particle and phosphorus source is 1:18~36.
The present invention promotes Prussian blue derivative presoma preferably to disperse using dispersion stabilizer, avoids reuniting.With
The pattern of cobaltosic oxide is regulated and controled, is removed by roasting dispersion stabilizer, forms porous pattern, so that final
The phosphatization cobalt pattern arrived is uniform, is class cubic granules, homogeneity is preferable；Also, the phosphatization cobalt can give full play of routine
The phosphatization cobalt material of non-Prussian blue similar object is to the electro catalytic activity of oxygen evolution reaction and phosphatization derived from Prussian blue similar object
The satisfactory electrical conductivity of object material has good catalytic performance, in oxygen evolution reaction, 10mA/cm to oxygen evolution reaction2Current density
Corresponding current potential is lower than 1.6000V vs.RHE.
Method provided by the invention is simple and easy, reproducible, and raw materials are cheap and easy to get, and product is stablized.
Polyvinylpyrrolidone conventional in the art（If molecular weight is 40000 ~ 360000）It is used equally in the present invention.
Preferably, polyvinylpyrrolidone described in S1 is polyvinylpyrrolidone 40 000 or polyvinylpyrrolidone
It is one or more of in 360000.
Preferably, cobalt salt described in S1 is one or more of cobaltous sulfate, cobalt nitrate or cobalt acetate.
Preferably, the molar ratio of potassium cobalticyanide described in S1 and cobalt salt is 1:2.
Preferably, the temperature that reaction is stood described in S1 is 25 ~ 80 DEG C, and the time is 18 ~ 30h.
Preferably, the process of washing described in S1 is successively to use deionized water and ethanol washing, centrifugation to neutrality；Institute in S1
Stating dry temperature is 60 DEG C, time 12h.
The dosage of dispersion stabilizer, which is subject to, realizes that potassium cobalticyanide and cobalt salt are uniformly dispersed.Under normal circumstances, stably dispersing
When the quality of agent is 0.2g ~ 0.5g, the preferable dispersion of the two can be realized.
Preferably, 1h is roasted after being warming up to 350 DEG C in S2 with 1 DEG C/min heating rate.
Preferably, phosphorus source described in S3 is the one or two of sodium hypophosphite or Diammonium phosphate (DAP).
Preferably, the molar ratio of cobaltosic oxide particle described in S3 and phosphorus source is 1:36.
Preferably, in S3 with 1 DEG C/min heating rate to roasting 1h after 285 DEG C.
A kind of phosphatization cobalt synthesized with Prussian blue derivative is also claimed in the present invention, and the phosphatization cobalt is according to above-mentioned
One preparation method obtains.
Preferably, the pattern of the phosphatization cobalt is class cubic granules, and partial size is 100 ~ 200nm.
Above-mentioned phosphatization cobalt is also within the scope of the present invention as application of the catalyst in oxygen evolution reaction.
Compared with prior art, the present invention has the advantages that：
Provided by the invention preparation method is simple, reproducible, and raw materials are cheap and easy to get, and product is stablized；It is prepared into
To phosphatization cobalt can give full play of phosphatization cobalt material to the electro catalytic activity of oxygen evolution reaction and the good conductive of phosphide material
Property, there is good catalytic performance to oxygen evolution reaction, in oxygen evolution reaction, 10mA/cm2Current potential corresponding to current density is lower than
1.6000V vs.RHE。
Detailed description of the invention
Fig. 1 is the XRD diagram for the phosphatization cobalt with the synthesis of Prussian blue derivative that embodiment 1 provides；
Fig. 2 is the SEM figure with the phosphatization cobalt of Prussian blue derivative synthesis when multiple is 30K that embodiment 1 provides；
Fig. 3 is the SEM figure with the phosphatization cobalt of Prussian blue derivative synthesis when multiple is 50K that embodiment 1 provides；
Fig. 4 is the catalysis oxygen using the phosphatization cobalt that Prussian blue derivative synthesizes as oxygen evolution reaction catalysts prepared by embodiment 1
The performance map of precipitation.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of phosphatization cobalt synthesized with Prussian blue derivative, which can be used as oxygen evolution reaction catalysis
Agent is prepared via a method which to obtain.
0.3g polyvinylpyrrolidone 360000 and 0.04mmol potassium cobalticyanide are uniformly mixed in 50ml deionized water,
0.08mmol cobalt acetate is scattered in 50ml deionized water, and the above solution is evenly mixed in beaker, then under the conditions of 25 DEG C
18h is stood, spends ionic hydration ethyl alcohol centrifuge washing, then at 60 DEG C, freeze-day with constant temperature for 24 hours, obtains Prussian blue derivative
Presoma.
The Prussian blue derivative presoma of 200mg is placed in Muffle furnace, under air conditions, is heated up with 1 DEG C/min fast
To 350 DEG C, constant temperature 1h is cooled to room temperature to get cobaltosic oxide particle rate.
0.10g cobaltosic oxide particle and 1.58g sodium hypophosphite are respectively put at the downstream in tube furnace and upper
At air-flow, under inert gas conditions, with 1 DEG C/min heating rate to 285 DEG C, constant temperature 1h is cooled to room temperature to get phosphatization cobalt
Material.
Phosphatization cobalt oxide evolution reaction catalyst derived from resulting Prussian blue similar object is passed through into X-ray diffraction characterization point
Analysis, as a result as shown in FIG. 1, FIG. 1 is phosphatization cobalt oxide evolution reaction catalysts derived from the Prussian blue similar object of the preparation of embodiment 1
XRD diagram.Product made from the preparation method and phosphatization cobalt standard card coincide as can be known from Fig. 1, to prove obtained
Catalyst is phosphatization cobalt oxide evolution reaction catalyst derived from Prussian blue similar object.
Phosphatization cobalt oxide evolution reaction catalyst derived from resulting Prussian blue similar object is scanned electron-microscope scanning point
Analysis, as a result as shown in Figures 2 and 3, Fig. 2 are phosphatization cobalt oxide evolution reaction derived from the Prussian blue similar object of the preparation of embodiment 1
SEM figure of the catalyst when multiple is 30K.Fig. 3 is that phosphatization cobalt oxide derived from the Prussian blue similar object of the preparation of embodiment 1 is precipitated
SEM figure of the catalysts when multiple is 50K.From Fig. 2 in Fig. 3 it can be seen that Prussian blue similar object derived from phosphatization cobalt
The pattern of oxygen evolution reaction catalyst is uniform, is particle, and partial size is 100 ~ 200nm, illustrates to prepare by this method general
Phosphatization cobalt oxide evolution reaction catalyst derived from the scholar's indigo plant analog of Shandong has preferable homogeneity.
The catalytic activity of phosphatization cobalt oxide evolution reaction catalyst derived from resulting Prussian blue similar object is detected, as a result such as
Shown in Fig. 4, Fig. 4 is the catalysis oxygen of phosphatization cobalt oxide evolution reaction catalyst derived from the Prussian blue similar object of the preparation of embodiment 1
The performance map of precipitation.As can be known from Fig. 4, the 10mA/cm of phosphatization cobalt oxide evolution reaction catalyst derived from Prussian blue similar object2
Current potential corresponding to current density is 1.5700V vs.RHE, illustrates that the phosphatization cobalt oxygen evolution reaction synthesized with Prussian blue derivative is urged
Agent is precipitated with preferably catalytic performance to catalysis oxygen.
Embodiment 2
The present embodiment provides a kind of phosphatization cobalts synthesized with Prussian blue derivative, are prepared via a method which to obtain.
0.5g polyvinylpyrrolidone 40 000 and 0.04mmol potassium cobalticyanide are uniformly mixed in 50ml deionized water,
0.06mmol cobaltous sulfate is scattered in 50ml deionized water, and the above solution is evenly mixed in beaker, then under the conditions of 60 DEG C
30h is stood, spends ionic hydration ethyl alcohol centrifuge washing, then at 60 DEG C, freeze-day with constant temperature for 24 hours, obtains Prussian blue derivative
Presoma.
The Prussian blue derivative presoma of 200mg is placed in Muffle furnace, under air conditions, is heated up with 1 DEG C/min fast
To 350 DEG C, constant temperature 1h is cooled to room temperature to get cobaltosic oxide particle rate.
0.10g cobaltosic oxide particle cobalt oxide and 1.19g Diammonium phosphate (DAP) are respectively put at the downstream in tube furnace
At overdraught, under inert gas conditions, with 1 DEG C/min heating rate to 285 DEG C, constant temperature 1h is cooled to room temperature to get phosphorus
Change cobalt material.
Detect the resulting catalytic performance for having preferably catalytic performance to catalysis analysis oxygen, it is known that, Prussian blue similar object spreads out
The 10mA/cm of raw phosphatization cobalt oxide evolution reaction catalyst2Current potential corresponding to current density is 1.5800V vs.RHE.
Embodiment 3
The present embodiment provides a kind of phosphatization cobalts synthesized with Prussian blue derivative, are prepared via a method which to obtain.
0.3g polyvinylpyrrolidone 360000 and 0.04mmol potassium cobalticyanide are uniformly mixed in 50ml deionized water,
0.12mmol cobaltous sulfate is scattered in 50ml deionized water, and the above solution is evenly mixed in beaker, then under the conditions of 25 DEG C
18h is stood, spends ionic hydration ethyl alcohol centrifuge washing, then at 60 DEG C, freeze-day with constant temperature for 24 hours, obtains Prussian blue derivative
Presoma.
The Prussian blue derivative presoma of 200mg is placed in Muffle furnace, under air conditions, is heated up with 5 DEG C/min fast
To 450 DEG C, constant temperature 5h is cooled to room temperature to get cobaltosic oxide particle rate.
0.10g cobaltosic oxide particle and 1.32g sodium hypophosphite are respectively put at the downstream in tube furnace and upper
At air-flow, under inert gas conditions, with 5 DEG C/min heating rate to 350 DEG C, constant temperature 5h is cooled to room temperature to get phosphatization cobalt
Material.
Detect the resulting catalytic performance for having preferably catalytic performance to catalysis analysis oxygen, it is known that, Prussian blue similar object spreads out
The 10mA/cm of raw phosphatization cobalt oxide evolution reaction catalyst2Current potential corresponding to current density is 1.5750V vs.RHE.
Embodiment 4
The present embodiment provides a kind of phosphatization cobalts synthesized with Prussian blue derivative, are prepared via a method which to obtain.
0.5g neopelex and 0.04mmol potassium cobalticyanide are uniformly mixed in 50ml deionized water,
0.06mmol cobalt nitrate is scattered in 50ml deionized water, and the above solution is evenly mixed in beaker, then under the conditions of 60 DEG C
30h is stood, spends ionic hydration ethyl alcohol centrifuge washing, then at 60 DEG C, freeze-day with constant temperature for 24 hours, obtains Prussian blue derivative
Presoma.
The Prussian blue derivative presoma of 200mg is placed in Muffle furnace, under air conditions, is heated up with 5 DEG C/min fast
To 450 DEG C, constant temperature 5h is cooled to room temperature to get cobaltosic oxide particle rate.
0.10g cobaltosic oxide particle and 1.06g Diammonium phosphate (DAP) are respectively put at the downstream in tube furnace and upper gas
At stream, under inert gas conditions, with 5 DEG C/min heating rate to 350 DEG C, constant temperature 5h, it is cooled to room temperature to get phosphatization cobalt material
Material.
Detect the resulting catalytic performance for having preferably catalytic performance to catalysis analysis oxygen, it is known that, Prussian blue similar object spreads out
The 10mA/cm of raw phosphatization cobalt oxide evolution reaction catalyst2Current potential corresponding to current density is 1.5850V vs.RHE.
Claims (10)
1. a kind of preparation method of the phosphatization cobalt with the synthesis of Prussian blue derivative, which is characterized in that include the following steps：
S1：Dispersion stabilizer, potassium cobalticyanide and cobalt salt are mixed, stand reaction, washing, drying to obtain is Prussian blue to spread out
Eobiont body；The dispersion stabilizer is one or more of polyvinylpyrrolidone or neopelex；Institute
The molar ratio for stating potassium cobalticyanide and cobalt salt is 1 ~ 2:3；
S2：Prussian blue derivative presoma in S1 is warming up under air conditions with the heating rate of 1 ~ 5 DEG C/min
1 ~ 3 h is roasted after 350 ~ 450 DEG C up to cobaltosic oxide particle；
S3：Cobaltosic oxide particle and phosphorus source are warming up to 285 under inert gas conditions with the heating rate of 1 ~ 5 DEG C/min ~
1 ~ 5h is roasted after 350 DEG C to get phosphatization cobalt；The molar ratio of the cobaltosic oxide particle and phosphorus source is 1:18~36.
2. preparation method according to claim 1, which is characterized in that polyvinylpyrrolidone described in S1 is polyvinyl pyrrole
One or more of alkanone 40000 or polyvinylpyrrolidone 360000.
3. preparation method according to claim 1, which is characterized in that cobalt salt described in S1 is cobaltous sulfate, cobalt nitrate or acetic acid
One or more of cobalt.
4. preparation method according to claim 1, which is characterized in that the molar ratio of potassium cobalticyanide described in S1 and cobalt salt is 1:
2。
5. preparation method according to claim 1, which is characterized in that after being warming up to 350 DEG C in S2 with 1 DEG C/min heating rate
Roast 1h.
6. preparation method according to claim 1, which is characterized in that phosphorus source described in S3 is sodium hypophosphite or Diammonium phosphate (DAP)
One or both of.
7. preparation method according to claim 1, which is characterized in that mole of cobaltosic oxide particle described in S3 and phosphorus source
Than being 1:36.
8. preparation method according to claim 1, which is characterized in that with 1 DEG C/min heating rate to roasting after 285 DEG C in S3
1h。
9. a kind of phosphatization cobalt synthesized with Prussian blue derivative, which is characterized in that the phosphatization cobalt is according to claim 1 ~ 8 times
One preparation method obtains.
10. application of any phosphatization cobalt of claim 8 ~ 9 as catalyst in oxygen evolution reaction.
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