CN106784902A - Load type platinum porpezite ternary alloy nano catalyst and its preparation method and application - Google Patents
Load type platinum porpezite ternary alloy nano catalyst and its preparation method and application Download PDFInfo
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- CN106784902A CN106784902A CN201611222405.5A CN201611222405A CN106784902A CN 106784902 A CN106784902 A CN 106784902A CN 201611222405 A CN201611222405 A CN 201611222405A CN 106784902 A CN106784902 A CN 106784902A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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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
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a kind of load type platinum porpezite ternary alloy nano catalyst and its preparation method and application, preparation method is comprised the following steps:S01, measures appropriate PdCl2HCl solution a certain amount of ammoniacal liquor is slowly added in beaker, under agitation, until system is in colourless, continue to stir at least 30min, it is stand-by;S02, weighs a certain amount of pretreated carbon carrier in another beaker, adds appropriate H2PtCl6And H2AuCl6The aqueous solution, be uniformly dispersed in low temperature ultrasonic machine;S03, by the beaker of the solution addition S02 in S01, be uniformly dispersed to obtain carbon mud at room temperature;S04, the carbon mud of S03 is stirred at a certain temperature and is evaporated in carbon mud without obvious liquid.The method is simple to operate, pollution-free without any surfactant, environmentally friendly, and catalyst performance stabilised prepared by the method, reproducible, can be mass-produced.
Description
Technical field
The present invention relates to a kind of load type platinum porpezite ternary alloy nano catalyst and its preparation method and application, belong to combustion
Material cell art.
Background technology
Due to burning mineral fuel, global warming increasingly accelerates, the air quality in many cities in the world declining, and
Hydrogen energy source is totally pollution-free, the energy policy of various countries is turned to hydrogen energy source.Fuel cell is a kind of efficient, environment-friendly generating
Device, it can will directly be stored in fuel and be converted into electric energy with the chemical energy in oxidant.The elctro-catalyst of fuel cell is played the part of
The effect of electrochemical reaction " factory " is drilled, is battery core critical material.Fuel cell will turn into real commodity, it is necessary to solve
Certainly problems such as performance, cost, stability, durability, environmental suitability, wherein the most key is that performance and cost are asked
Topic.But the reserves as the platinum of elctro-catalyst are limited, expensive, the commercialization of fuel cell is constrained.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method simply and entirely without waste gas and waste liquid discharge, performance
The preparation method of excellent load type platinum porpezite ternary alloy nano catalyst;Further, the present invention provides a kind of support type
Platinum porpezite ternary alloy nano catalyst, the catalyst can be greatly lowered Pt consumptions, catalysis is improved while reduces cost and is lived
Property and anti-toxic effects;Further, the present invention provides a kind of application of load type platinum porpezite ternary alloy nano catalyst.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
The preparation method of load type platinum porpezite ternary alloy nano catalyst, comprises the following steps:
S01, measures appropriate PdCl2HCl solution a certain amount of ammoniacal liquor is slowly added in beaker, under agitation,
Until system continues to stir at least 30min in colourless, it is stand-by;
S02, weighs a certain amount of pretreated carbon carrier in another beaker, adds appropriate H2PtCl6And H2AuCl6
The aqueous solution, be uniformly dispersed in low temperature ultrasonic machine;
S03, by the beaker of the solution addition S02 in S01, be uniformly dispersed to obtain carbon mud at room temperature;
S04, the carbon mud of S03 is stirred at a certain temperature and is evaporated in carbon mud without obvious liquid;
S05, lyophilized overnight is carried out by the carbon mud of S04;
S06, the carbon mud after freezing is placed in ball grinder after taking out, and adds appropriate ball milling pearl, is carried out ball milling and is obtained treating also
Raw sample;
S07, obtains final load type platinum porpezite ternary alloy nano and urges after sample to be restored is reduced in tube furnace
Agent.
The preprocess method of the carbon carrier is comprised the following steps:
A, weighs a certain amount of specific surface area at least 20g/m2Carbon carrier in beaker, by the quality of carbon carrier and urea
Than being 1:The proportioning of (0.5~3) adds urea, adds ultra-pure water to not having carbon carrier, 10~60min of ultrasonic disperse;
B, heating stirring is evaporated to without clearly visible water at 50~80 DEG C;
C, the carbon carrier that step b is obtained is dried overnight for 80 DEG C in vacuum drying chamber;
D, 2~5h is calcined by dried carbon carrier under 300~800 DEG C of nitrogen atmospheres in tube furnace.
Evaporating temperature is 40~80 DEG C in S04.
The ball grinder be zirconia ball grinding jar, ball milling pearl be zirconium oxide ball milling pearl, zirconium oxide ball milling pearl a diameter of 3~
8mm, selected during ball milling single diameter or many diameter mix and match zirconium oxide ball milling pearl, Ball-milling Time is 1~4h, and ball milling turns
Speed is 100~500rpm/min.
Reducing atmosphere in S07 is H2/ Ar atmosphere, reduction temperature is 120~300 DEG C, and the recovery time is 60~180min.
Stirring in S01 and S04 is magnetic agitation.
The temperature range of the low temperature ultrasonic machine is 0~10 DEG C.
The preparation method of load type platinum porpezite ternary alloy nano catalyst of the invention, the method is simple to operate, and nothing is appointed
What surfactant, it is pollution-free, it is environmentally friendly, and catalyst performance stabilised prepared by the method, it is reproducible, can high-volume
Production.
The load type platinum porpezite ternary alloy nano catalyst that preparation method of the invention is obtained.The catalyst deposits Pt
On Pd (111) crystal face, Pt consumptions can be not only greatly lowered, while ORR activity can also be improved.Meanwhile, in catalyst system
Middle introducing transition metal Au, substantially increases the anti-toxic effects of catalyst.The present invention is beneficial to using pretreated carbon carrier
The combination of metal ion and carrier, catalyst precursor (i.e. PdCl can be made through ball-milling technology2、H2PtCl6And H2AuCl6And its water
Compound) being more evenly distributed on carrier, and then influence the activity of catalyst.
Application of the load type platinum porpezite ternary alloy nano catalyst of the invention in fuel-cell catalyst.The present invention
When the load type platinum porpezite ternary alloy nano catalyst of preparation is used as fuel-cell catalyst, platinum utilization is improved, reduced
The carrying capacity of platinum, so as to effectively improve the performance of catalyst.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of carrier carbon of the present invention;
Fig. 2 is the preparation technology flow chart of load type platinum porpezite ternary alloy nano catalyst of the present invention.
Specific embodiment
The present invention is further described below in conjunction with the accompanying drawings.
Embodiment 1:
As shown in Fig. 1~Fig. 2, the preparation method of load type platinum porpezite ternary alloy nano catalyst is comprised the following steps:
S01, measures 1.3mLPdCl2HCl solution in beaker, wherein HCl solution be 0.5mol/L, after preparation
PdCl2Solution is 5wt%;Then a certain amount of ammoniacal liquor is slowly added under magnetic stirring, until system continues to stir in colourless
30min, it is stand-by;
S02, weighs the pretreated carbon carriers of 0.5g in another beaker, adds 2mL H2PtCl6With
0.9mLH2AuCl6The aqueous solution, the aqueous solution after preparation contains 2wt%H2PtCl6And 5wt%H2AuCl6, in low temperature ultrasonic machine
In 2 DEG C of ultrasonic disperse 40min;
S03, S02 is added by the solution in S01, and 30min is disperseed at room temperature;
S04, by the mixed solution of S03 in magnetic agitation is evaporated to carbon mud at a temperature of 40 DEG C on magnetic stirring apparatus without bright
Aobvious liquid;
S05, lyophilized overnight is carried out by carbon mud prepared by S04;
S06, carbon mud of the S05 after lyophilized is taken out after in 0.1L ball grinders, adds 50 zirconium oxide ball millings of 3mm diameters
Pearl, 300rpm/min rotating speeds, ball milling 2h obtains sample to be restored;
S07, by the sample to be restored in S06 in tube furnace, with H2/ Ar is reducing atmosphere, and 120~150 DEG C of reduction are gone back
The former time is 120min, obtains final load type platinum porpezite ternary alloy nano catalyst.
The preprocess method of carbon carrier is comprised the following steps:
A, weighs a certain amount of 20g/m2The carbon carrier of specific surface is 1 by the mass ratio of carbon carrier and urea in beaker:
0.5 proportioning adds urea, adds ultra-pure water to not having carbon carrier, ultrasonic disperse 10min;
B, heating stirring is evaporated to without clearly visible water at 50 DEG C;
C, the carbon carrier that step b is obtained is dried overnight for 80 DEG C in vacuum drying chamber;
D, calcines dried carbon carrier 2h and obtains carrier carbon under 300 DEG C of nitrogen atmospheres in tube furnace.
The present embodiment also protects load type platinum porpezite ternary alloy nano catalyst and catalysis of above method preparation
Application of the agent in fuel-cell catalyst.
Embodiment 2:
As shown in Fig. 1~Fig. 2, the preparation method of load type platinum porpezite ternary alloy nano catalyst is comprised the following steps:
S01, measures 2mLPdCl2HCl solution in beaker, wherein HCl solution be 0.1mol/L, the PdCl after preparation2
Solution is 3wt%;Then a certain amount of ammoniacal liquor is slowly added under magnetic stirring, until system continues to stir 30min in colourless,
It is stand-by;
S02, weighs the pretreated 50g/m of 0.5g2Specific surface carbon carrier adds 1.5mL in another beaker
H2PtCl6And 0.8mLH2AuCl6The aqueous solution, the aqueous solution after preparation contains 1wt%H2PtCl6And 2wt%H2AuCl6, in low temperature
In 10 DEG C of ultrasonic disperse 40min in ultrasonic machine;
S03, S02 is added by the solution in S01, and 40min is disperseed at room temperature;
S04, by the mixed solution of S03 in magnetic agitation is evaporated to carbon mud at a temperature of 80 DEG C on magnetic stirring apparatus without bright
Aobvious liquid;
S05, lyophilized overnight is carried out by carbon mud prepared by S04;
S06, carbon mud of the S05 after lyophilized is taken out after in 0.1L ball grinders, and 40 3mm diameters of addition and 20 5mm are straight
The zirconium oxide ball milling pearl in footpath, 100rpm/min rotating speeds, ball milling 4h obtains sample to be restored;
S07, by the sample to be restored in S06 in tube furnace, with H2/ Ar is reducing atmosphere, 200 DEG C of reduction, during reduction
Between be 60~80min, obtain final load type platinum porpezite ternary alloy nano catalyst.
The preprocess method of carbon carrier is comprised the following steps:
A, weighs a certain amount of 50g/m2The carbon carrier of specific surface is 1 by the mass ratio of carbon carrier and urea in beaker:3
Proportioning add urea, add ultra-pure water to not having carbon carrier, ultrasonic disperse 60min;
B, heating stirring is evaporated to without clearly visible water at 80 DEG C;
C, the carbon carrier that step b is obtained is dried overnight for 80 DEG C in vacuum drying chamber;
D, calcines dried carbon carrier 5h and obtains carrier carbon under 800 DEG C of nitrogen atmospheres in tube furnace.
The present embodiment also protects load type platinum porpezite ternary alloy nano catalyst and catalysis of above method preparation
Application of the agent in fuel-cell catalyst.
Embodiment 3:
As shown in Fig. 1~Fig. 2, the preparation method of load type platinum porpezite ternary alloy nano catalyst is comprised the following steps:
S01, measures 1.6mLPdCl2HCl solution in beaker, wherein HCl solution be 0.1mol/L, after preparation
PdCl2Solution is 3wt%;Then a certain amount of ammoniacal liquor is slowly added under magnetic stirring, until system continues to stir in colourless
30min, it is stand-by;
S02, weighs the pretreated carbon carriers of 0.5g in another beaker, adds 2.2mL H2PtCl6With
1.0mLH2AuCl6The aqueous solution, the aqueous solution after preparation contains 1wt%H2PtCl6And 2wt%H2AuCl6, in low temperature ultrasonic machine
In 0~1 DEG C of ultrasonic disperse 50min;
S03, S02 is added by the solution in S01, and 50min is disperseed at room temperature;
S04, by the mixed solution of S03 in magnetic agitation is evaporated to carbon mud at a temperature of 60 DEG C on magnetic stirring apparatus without bright
Aobvious liquid;
S05, lyophilized overnight is carried out by carbon mud prepared by S04;
S06, carbon mud of the S05 after lyophilized is taken out after in 0.1L ball grinders, and 15 8mm diameters of addition and 30 5mm are straight
The zirconium oxide ball milling pearl in footpath, 500rpm/min rotating speeds, ball milling 1h obtains sample to be restored;
S07, by the sample to be restored in S06 in tube furnace, with H2/ Ar is reducing atmosphere, 300 DEG C of reduction, during reduction
Between be 180min, obtain final load type platinum porpezite ternary alloy nano catalyst.
The preprocess method of carbon carrier is comprised the following steps:
A, weighs a certain amount of 50g/m2The carbon carrier of specific surface is 1 by the mass ratio of carbon carrier and urea in beaker:2
Proportioning add urea, add ultra-pure water to not having carbon carrier, ultrasonic disperse 30min;
B, heating stirring is evaporated to without clearly visible water at 60 DEG C;
C, the carbon carrier that step b is obtained is dried overnight for 80 DEG C in vacuum drying chamber;
D, calcines dried carbon carrier 3h and obtains carrier carbon under 600 DEG C of nitrogen atmospheres in tube furnace.
The present embodiment also protects load type platinum porpezite ternary alloy nano catalyst and catalysis of above method preparation
Application of the agent in fuel-cell catalyst.
The above is only the preferred embodiment of the present invention, it should be pointed out that:For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. the preparation method of load type platinum porpezite ternary alloy nano catalyst, it is characterised in that:Comprise the following steps:
S01, measures appropriate PdCl2HCl solution a certain amount of ammoniacal liquor is slowly added in beaker, under agitation, until body
System continues to stir at least 30min in colourless, stand-by;
S02, weighs a certain amount of pretreated carbon carrier in another beaker, adds appropriate H2PtCl6And H2AuCl6It is water-soluble
Liquid, is uniformly dispersed in low temperature ultrasonic machine;
S03, by the beaker of the solution addition S02 in S01, be uniformly dispersed to obtain carbon mud at room temperature;
S04, the carbon mud of S03 is stirred at a certain temperature and is evaporated in carbon mud without obvious liquid;
S05, lyophilized overnight is carried out by the carbon mud of S04;
S06, the carbon mud after freezing is placed in ball grinder after taking out, and adds appropriate ball milling pearl, is carried out ball milling and is obtained sample to be restored
Product;
S07, final load type platinum porpezite ternary alloy nano catalyst is obtained after sample to be restored is reduced in tube furnace.
2. the preparation method of load type platinum porpezite ternary alloy nano catalyst according to claim 1, it is characterised in that:
The preprocess method of the carbon carrier is comprised the following steps:
A, weighs a certain amount of specific surface area at least 20g/m2Carbon carrier in beaker, be with the mass ratio of urea by carbon carrier
1:The proportioning of (0.5~3) adds urea, adds ultra-pure water to not having carbon carrier, 10~60min of ultrasonic disperse;
B, heating stirring is evaporated to without clearly visible water at 50~80 DEG C;
C, the carbon carrier that step b is obtained is dried overnight for 80 DEG C in vacuum drying chamber;
D, 2~5h is calcined by dried carbon carrier under 300~800 DEG C of nitrogen atmospheres in tube furnace.
3. the preparation method of load type platinum porpezite ternary alloy nano catalyst according to claim 1, it is characterised in that:
Evaporating temperature is 40~80 DEG C in S04.
4. the preparation method of load type platinum porpezite ternary alloy nano catalyst according to claim 1, it is characterised in that:
The ball grinder is zirconia ball grinding jar, and ball milling pearl is zirconium oxide ball milling pearl, a diameter of 3~8mm of zirconium oxide ball milling pearl, ball milling
When select single diameter or many diameter mix and match zirconium oxide ball milling pearl, Ball-milling Time is 1~4h, and rotational speed of ball-mill is 100
~500rpm/min.
5. the preparation method of load type platinum porpezite ternary alloy nano catalyst according to claim 1, it is characterised in that:
Reducing atmosphere in S07 is H2/ Ar atmosphere, reduction temperature is 120~300 DEG C, and the recovery time is 60~180min.
6. the preparation method of load type platinum porpezite ternary alloy nano catalyst according to claim 1, it is characterised in that:
Stirring in S01 and S04 is magnetic agitation.
7. the preparation method of load type platinum porpezite ternary alloy nano catalyst according to claim 1, it is characterised in that:
The temperature range of the low temperature ultrasonic machine is 0~10 DEG C.
8. the load type platinum porpezite ternary alloy nano catalysis that the preparation method according to claim any one of 1-7 is obtained
Agent.
9. the load type platinum porpezite ternary alloy nano catalyst that the preparation method according to claim any one of 1-7 is obtained
Application in fuel-cell catalyst.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109065903A (en) * | 2018-09-17 | 2018-12-21 | 苏州擎动动力科技有限公司 | A kind of preparation method of high activity loading type octahedron ternary alloy catalyst |
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CN103928691A (en) * | 2014-04-10 | 2014-07-16 | 哈尔滨工业大学 | Platinum-based catalyst carrier of direct methanol fuel cell and preparation method thereof |
CN106058277A (en) * | 2016-08-13 | 2016-10-26 | 三峡大学 | PdAu electrocatalyst for fuel cell and preparation method thereof |
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CN101612566A (en) * | 2009-07-14 | 2009-12-30 | 复旦大学 | A kind of low-platinum carbon-supported nanometer Pd-Pt alloy catalyst, preparation method and application thereof |
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