CN101087022A - Making method for dual-function catalyzer of recycling fuel battery - Google Patents

Making method for dual-function catalyzer of recycling fuel battery Download PDF

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CN101087022A
CN101087022A CNA2006100272868A CN200610027286A CN101087022A CN 101087022 A CN101087022 A CN 101087022A CN A2006100272868 A CNA2006100272868 A CN A2006100272868A CN 200610027286 A CN200610027286 A CN 200610027286A CN 101087022 A CN101087022 A CN 101087022A
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preparation
dual
fuel battery
ptcl
polyalcohol
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CN101087022B (en
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田丙伦
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Beijing Zhongchuang Panye New Energy Technology Co., Ltd.
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DANYE HYDROGEN ENERGY-SOURCE SCIENCE-TECHNOLOGY Co Ltd SHANGHAI
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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 provides a preparing method of regeneration fuel battery double-function activator; the method includes decentralization liquid which is used to produce electrolysis active component carrier, polyatomic alcohol and water solution which are used to produce generating electricity active component precursor, revivification sedimentation Pt, producing double-function activator grain. The double-function activator produced by the method in the invention such as Pt/IrO2, Pt/IrO2-RuO2, and Pt is dispersed well, and grain is easy to be dispersed. Stability of activator is well, performance of battery produced is well, and it also possesses perfect electroanalysis. It can be used in URFC battery, the performance of generating electricity is better than activator produced by traditional mechanical mixing method.

Description

The preparation method of dual-function catalyzer of recycling fuel battery
Technical field
The present invention relates to a kind of Preparation of catalysts method, relate in particular to a kind of preparation method of dual-function catalyzer of recycling fuel battery.
Background technology
Regenerative fuel cell (united regenerative fuel cell) is a kind of battery energy storage system that brine electrolysis can generate electricity again that gets final product.It is compared with secondary cells such as traditional lead acid accumulator, Ni-Cd batteries as energy-storage system, have higher theoretical specific energy and theoretical specific power, do not have self discharge in the use, not limited by depth of discharge, and corrosion and pollute very lowly, be a kind of rising novel energy storage cell.
Research about the brine electrolysis galvanic anode is many, and the much more general method that is coated with one or more layers conduction catalytic membrane above the material at Titanium etc. that adopts is made electrolytic anode.This electrolytic anode is mainly used in the alkaline electrolysis battery structure.In the alkaline electrolysis battery, the current density of electrolytic cell is generally 0.2A/cm 2Little because of its electrolysis internal resistance as the acid solid polymer electrolytic battery of PEM, catalyst performance is good etc., and characteristics can be worked it under higher electrolytic current density.Under same decomposition voltage, the electrolytic current density of PEM system is generally at 1A/cm 2More than, and system is pollution-free.High performance electrolytic cell anode catalyst is bigger to the electrolysis Effect on Performance.
In application number is the Chinese patent of CN85107320, a kind of electrolytic cell Preparation of catalysts method that is particularly suitable for has been proposed.Provided a kind of porous high surface composite conducting catalysis material in the patent, it contain the pre-mold base of a kind of porous and after the make-up catalyst that is coated with, be characterized in that this porous matrix contains at least a platinum metal oxide and at least a non-noble metal oxide and catalysis material, is blended among the porous high surface area structure densely.The described material of this patent is the anode catalyst that is used as electrolytic cell.Proposed a kind of preparation method of electrolytic catalyst in the patent No. is the international monopoly of WO2005049199, the preparation method described in this patent mainly is that oxide surfaces such as the nano silicon, titanium dioxide at high-ratio surface support IrO 2, RuO 2Stablize the IrO of high-ratio surface Deng electrolytic catalyst 2, RuO 2Deng particle, improve the electrolysis performance of battery by the specific grain surface that improves catalyst.
For fuel cell, the Preparation of catalysts method is a lot, as application number is the preparation method that the Chinese patent of CN200310121180.0 has provided a kind of proton membrane fuel battery cathod eelctro-catalyst, is to utilize liquid-phase reduction that palladium or palladium and platinum isoreactivity component are supported the conductive porous material carrier for being prepared from activated carbon, carbon nano-tube, carbon fiber, mesopore charcoal, carbosphere, the conducting polymer.A kind of proton exchange membrane fuel cell electrode Preparation of catalysts method that Chinese patent CN01138909.5 mentions is that the method that adopts dihydroxylic alcohols to add thermal reduction is deposited to metal precursor on the carrier.
Application number is the preparation method that the Chinese patent of CN03127432.3 is mentioned a kind of fuel-cell catalyst; be with I; V; VI; VII; VIII subgroup and III; the mixture of IV main group metal or its mixture or their alloy or metal and metal oxide is an active constituent; with aluminium oxide; silica; active carbon; carbon black; CNT (carbon nano-tube); carbon fiber; molecular sieve; titanium oxide or cerium oxide are carrier; with the microwave radiation is heating source; with ethylene glycol; glycerol; butanediol; triethanolamine; binary such as trishydroxymethylaminomethane; ternary; tetrahydroxy alcohol is reducing agent and protective agent; to contain I; V; VI; VII; VIII subgroup and III; the salt of IV main group metal or its mixture are precursor; under microwave radiation, can obtain the metal loading fast is one of 1wt%～99wt%; two; ternary and polynary supported metal catalyst.
Application number is that the active component that the Chinese patent " a kind of solid supported noble metal catalyst " of CN01144123.2 is mentioned is metal Ru, Rh, Pd, Os, Ir, Pt, Au, Ag, Cu or Ni, and carrier is active carbon, graphite charcoal, CNT (carbon nano-tube), Al 2O 3, SiO 2, molecular sieve, MgO or TiO 2, active constituent and alkali metal or alkaline-earth metal and carrier are scattered in respectively in the solvent, mix heated solution, sedimentation, oven dry preparation in proportion.
Research for the regenerative fuel cell catalyst is fewer, and the anode catalyst of regenerative fuel cell should have dissolved oxygen and analyse the double function characteristic of oxygen, the preparation conventional machinery mixed method preparation of anode catalyst.As Ioroi T. etc. (J.Power sources[J], 2003,124:385-389) adopt the method preparation of mechanical mixture Pt powder-Ir powder; Swette L L etc. (Proton-exchange membrane regenerative fuel cells[J] .J.Power Sources, 1994,47:343-351), Hao liu etc. (Electrochemical andSolid-State Letters, 7 (3) A56-A59 (2004)) adopts the black and IrO of mechanical mixture Pt 2Method preparation.But said method is unfavorable for Pt and Ir, IrO 2Perhaps RuO 2Effective combination, be unfavorable for bringing into play the anode-catalyzed performance of oxygen electrode catalyst.
Ioroi etc. (J.Appl.Electrochem., 2001,31:1179-1183) report utilizes gluey predecessor (Ir (OH) 3(H 2O) 3) deposit to Pt and make oxygen electrode catalyst IrO on black 2/ Pt can make the black and IrO of Pt 2Organically combine, its performance is better than the Pt-IrO of mechanical mixing preparation 2The performance of electrode catalyst.Adopting Pt black in the said method is carrier, because the black particle of Pt is assembled than being easier in the normal state, usually connecting together is difficult for disperseing, thereby utilance is not very high.The catalyst of making in this way is applied on the URFC, and its power generation performance is compared slightly inferior properties with PEMFC, and the black loading of Pt is than higher.
Summary of the invention
Purpose of the present invention provides a kind of preparation method of dual-function catalyzer of recycling fuel battery exactly in order to address the above problem.
The object of the present invention is achieved like this: a kind of preparation method of dual-function catalyzer of recycling fuel battery may further comprise the steps:
The dispersion liquid of a, preparation carrier
With high-ratio surface electrolysis active component IrO 2, IrO 2-RuO 2Or IrO 2/ TiO 2Be carrier, it be distributed in the mixed liquor of polynary alcohol and water that ultrasonic concussion is even, makes the dispersion liquid of carrier;
The polyalcohol and the aqueous solution of b, preparation precursor
With H 2PtCl 6, (NH 4) 2PtCl 6, PtCl 4Or its mixture makes the polyalcohol and the aqueous solution as cell power generation active component precursor, and to regulate pH be 2-14.5;
C, reduction sedimentation Pt particle
The polyalcohol and the aqueous solution that regulate the cell power generation active component precursor of pH value are joined in the dispersion liquid of electrolysis active component carrier, ultrasonic concussion evenly and add thermal response, make electrolysis active component precursor restore Pt and deposit on the carrier, form the bifunctional catalyst particle.
D, preparation bifunctional catalyst
The suspension-turbid liquid that comprises the bifunctional catalyst particle that step c is made makes electrolysis-generating bifunctional catalyst product through steps such as cooling, filtration, washing, vacuum dryings.
The specific surface of the carrier described in the step a is 10-100m 2/ g.
In the mixed liquor of the polynary alcohol and water described in the step a, the weight ratio of polyalcohol and water is 1: 2-2: 1.
In the polyalcohol and the aqueous solution of the precursor described in the step b, the weight ratio of polyalcohol and water is 1: 5-5: 1.
Heating reaction temperature described in the step c is controlled at 40-100 ℃.
Polyalcohol described in step a and the step b is an ethylene glycol.
Precursor H described in the step b 2PtCl 6, (NH 4) 2PtCl 6, PtCl 4Or its mixture is its ethylene glycol solution.
The bifunctional catalyst such as the Pt/IrO of preparation method's preparation of dual-function catalyzer of recycling fuel battery of the present invention 2, Pt/IrO 2-RuO 2, Pt disperses relatively good on particle, and the particle ratio is easier to disperse difficult the gathering.The good stability of catalyst, the cell power generation performance of making is good, and has good electrolysis performance.Be used for the URFC battery, its power generation performance is better than the catalyst of traditional mechanical mixture method preparation.
Embodiment
The preparation method of dual-function catalyzer of recycling fuel battery of the present invention is described below by several embodiment.
Embodiment 1
Get the commercially available IrO of 1.2g 2Pressed powder, its specific area is greater than 20m 2/ g is distributed to it in 10g ethylene glycol and the 5g water, and ultrasonic concussion is even, makes IrO 2Dispersion liquid.
Get the H that 41.4g concentration is 20g/L 2PtCl 6Ethylene glycol solution adds 20.7g water, adds Na again 2CO 3Solid 0.6g regulates its pH value, makes H 2PtCl 6The ethylene glycol and the aqueous solution.
The H of pH value will be regulated 2PtCl 6The ethylene glycol and the aqueous solution join IrO 2Dispersion liquid in, behind the ultrasonic concussion 10min, put into microwave oven and be heated to boiling.After the taking-up, the room temperature cooling, suction filtration, washing 60 ℃ of bakings 12 hours, promptly makes 20%Pt/IrO 2The dual-function catalyzer of recycling fuel battery product.
Embodiment 2
Get the commercially available IrO of 1.2g 2Pressed powder, its specific area is greater than 20m 2/ g is distributed to it in 10g ethylene glycol and the 10g water, and ultrasonic concussion is even, makes IrO 2Dispersion liquid.
Get the H that 41.4g concentration is 20g/L 2PtCl 6Ethylene glycol solution adds 41.4g water, adds Na again 2CO 3Solid 2g regulates its pH value, makes H 2PtCl 6The ethylene glycol and the aqueous solution.
The H of pH value will be regulated 2PtCl 6The ethylene glycol and the aqueous solution add IrO 2Dispersion liquid in, behind the ultrasonic concussion 10min, put into microwave oven and be heated to boiling.After the taking-up, the room temperature cooling, suction filtration, washing, 120 ℃ of vacuum were dried by the fire 12 hours, promptly made 20%Pt/IrO 2The dual-function catalyzer of recycling fuel battery product.
Embodiment 3
Get the commercially available Ir0 of 1.2g 2Pressed powder, its specific area is greater than 20m 2/ g is distributed to it in 10g ethylene glycol and the 20g water, and ultrasonic concussion is even, makes IrO 2Dispersion liquid.
Get the H that 41.4g concentration is 20g/L 2PtCl 6Ethylene glycol solution adds 82.8g water, makes H 2PtCl 6The ethylene glycol and the aqueous solution.
With H 2PtCl 6The ethylene glycol and the aqueous solution add IrO 2Dispersion liquid in, behind the ultrasonic concussion 10min, put into microwave oven and be heated to boiling.After the taking-up, the room temperature cooling, suction filtration, washing, 120 ℃ of vacuum were dried by the fire 12 hours, promptly made 20%Pt/IrO 2The dual-function catalyzer of recycling fuel battery product.
Embodiment 4
Get the commercially available IrO of 0.6g 2Pressed powder, its specific area is greater than 20m 2/ g is distributed to it in 5g ethylene glycol and the 5g water, and ultrasonic concussion is even, makes IrO 2Dispersion liquid.
Get the H that 55.2g concentration is 20g/L 2PtCl 6Ethylene glycol solution adds 55.2g water, adds Na again 2CO 3Solid 0.6g regulates its pH value, makes H 2PtCl 6The ethylene glycol and the aqueous solution.
With H 2PtCl 6The ethylene glycol and the aqueous solution add IrO 2Dispersion liquid in, behind the ultrasonic concussion 10min, put into microwave oven and be heated to boiling.After the taking-up, the room temperature cooling, suction filtration, washing, 60 ℃ were dried by the fire 12 hours, and promptly made 40%Pt/IrO 2The dual-function catalyzer of recycling fuel battery product.
Embodiment 5
Get the commercially available IrO of 0.5g 2Pressed powder, its specific area is greater than 20m 2/ g is distributed to it in 5g ethylene glycol and the 5g water, and ultrasonic concussion is even, makes IrO 2Dispersion liquid.
Get the H that 68.75g concentration is 20g/L 2PtCl 6Ethylene glycol solution adds 68.75g water, adds Na again 2CO 3Solid 1.2g regulates its pH value, makes H 2PtCl 6The ethylene glycol and the aqueous solution.
With H 2PtCl 6The ethylene glycol and the aqueous solution add IrO 2Dispersion liquid in, behind the ultrasonic concussion 10min, will put into microwave oven and be heated to boiling.After the taking-up, the room temperature cooling, suction filtration, washing, 60 ℃ were dried by the fire 12 hours, and promptly made 50%Pt/IrO 2The dual-function catalyzer of recycling fuel battery product.
Prepared catalyst among the embodiment 4 is taken out 0.05 gram, add entry, pure equal solvent, add the NAFION resin then, wherein NAFION: catalyst=1: 4 is coated in 36cm with its slurry that makes 2On NR211 (dupont) proton exchange membrane, be used as electrolytic anode.0.05 gram 20%Pt/C is mixed with 0.2 gram 10%NAFION solution, make slurry, be coated in the another side of proton exchange membrane, be used as electrolysis cathode.Make battery No. 1.
Get black 0.02 gram of JM (JOHNSON METTHEY company) Pt, directly add 0.03 gram IrO 2, making its mixed proportion is 4: 6, adds entry, pure equal solvent, and making its total amount is 0.1 gram, and add NAFION (DUPONT company product) resin, wherein NAFION then: catalyst=1: 4 is coated in 36cm with its slurry that makes 2On NR211 (dupont) proton exchange membrane, be used as electrolytic anode.0.05 gram 20%Pt/C is mixed with 0.2 gram 10%NAFION solution, make slurry, be coated in the another side of proton exchange membrane, be used as electrolysis cathode.Make battery No. 2.
1, No. 2 battery is carried out the electrolysis generator experimental after with the assembling of materials such as carbon paper, and the result is as shown in table 1.(wherein electrolysis and generating temperature are all carried out at 60 ℃, and pressure is 1atm.)
Table 1
The battery label 1 2
Electrolysis (voltage 1.7V) 500mA/cm 2 520mA/cm 2
Generating (voltage 0.6V) 950mA/cm 2 820mA/cm 2
By the correction data of table 1 as can be seen, the electrolysis performance of No. 2 batteries slightly is better than battery No. 1, but its power generation performance is starkly lower than battery No. 1.Therefore we think that the catalyst Pt in No. 1 battery is supported on IrO more dispersedly 2On, so Pt/IrO 2The utilization ratio of catalyst is higher.

Claims (7)

1, a kind of preparation method of dual-function catalyzer of recycling fuel battery is characterized in that, may further comprise the steps:
The dispersion liquid of a, preparation carrier
With high-ratio surface electrolysis active component IrO 2, IrO 2-RuO 2Or IrO 2/ TiO 2Be carrier, it be distributed in the mixed liquor of polynary alcohol and water that ultrasonic concussion is even, makes the dispersion liquid of carrier;
The polyalcohol and the aqueous solution of b, preparation precursor
With H 2PtCl 6, (NH 4) 2PtCl 6, PtCl 4Or its mixture makes the polyalcohol and the aqueous solution as cell power generation active component precursor, and to regulate pH be 2-14.5;
C, reduction sedimentation Pt particle
The polyalcohol and the aqueous solution that regulate the cell power generation active component precursor of pH value are joined in the dispersion liquid of electrolysis active component carrier, ultrasonic concussion evenly and add thermal response, make electrolysis active component precursor restore Pt and deposit on the carrier, form the bifunctional catalyst particle.
D, preparation bifunctional catalyst
The suspension-turbid liquid that comprises the bifunctional catalyst particle that step c is made makes electrolysis-generating bifunctional catalyst product through steps such as cooling, filtration, washing, vacuum dryings.
2, the preparation method of dual-function catalyzer of recycling fuel battery as claimed in claim 1 is characterized in that: the specific surface of the carrier described in the step a is 10-100m 2/ g.
3, the preparation method of dual-function catalyzer of recycling fuel battery as claimed in claim 1 is characterized in that: in the mixed liquor of the polynary alcohol and water described in the step a, the weight ratio of polyalcohol and water is 1: 2-2: 1.
4, the preparation method of dual-function catalyzer of recycling fuel battery as claimed in claim 1 is characterized in that: in the polyalcohol and the aqueous solution of the precursor described in the step b, the weight ratio of polyalcohol and water is 1: 5-5: 1.
5, the preparation method of dual-function catalyzer of recycling fuel battery as claimed in claim 1 is characterized in that: the heating reaction temperature described in the step c is controlled at 40-100 ℃.
6, the preparation method of dual-function catalyzer of recycling fuel battery as claimed in claim 1 is characterized in that: the polyalcohol described in step a and the step b is an ethylene glycol.
7, the preparation method of dual-function catalyzer of recycling fuel battery as claimed in claim 1 is characterized in that: the precursor H described in the step b 2PtCl 6, (NH 4) 2PtCl 6, PtCl 4Or its mixture is its ethylene glycol solution.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101325266B (en) * 2008-07-24 2010-06-02 华南理工大学 Power supply system for minisize composite regenerative fuel battery
WO2012107738A1 (en) * 2011-02-08 2012-08-16 Johnson Matthey Public Limited Company Catalyst for fuel cells
CN101773826B (en) * 2009-01-14 2013-01-30 中国科学院大连化学物理研究所 Catalyst using metal oxide as carrier for fuel cells and application thereof
CN101983450B (en) * 2009-04-28 2015-01-07 松下电器产业株式会社 Electrode for fuel cell, method for manufacturing the electrode, and fuel cell using the electrode
CN107195910A (en) * 2017-06-03 2017-09-22 上海博暄能源科技有限公司 One kind can discharge and recharge metal air battery cathodes and preparation method thereof
CN110416561A (en) * 2019-06-25 2019-11-05 华北电力大学 A kind of bifunctional electrocatalyst Pt-IrO2, preparation method
JP2023545163A (en) * 2020-10-13 2023-10-26 グリナリティ・ゲーエムベーハー Oxygen evolution catalysts, their production and use, membrane electrode arrangements, and fuel cells or electrolytic cells

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JP4625658B2 (en) * 2004-07-21 2011-02-02 株式会社東芝 Fuel cell electrode, membrane electrode composite, and fuel cell

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101325266B (en) * 2008-07-24 2010-06-02 华南理工大学 Power supply system for minisize composite regenerative fuel battery
CN101773826B (en) * 2009-01-14 2013-01-30 中国科学院大连化学物理研究所 Catalyst using metal oxide as carrier for fuel cells and application thereof
CN101983450B (en) * 2009-04-28 2015-01-07 松下电器产业株式会社 Electrode for fuel cell, method for manufacturing the electrode, and fuel cell using the electrode
WO2012107738A1 (en) * 2011-02-08 2012-08-16 Johnson Matthey Public Limited Company Catalyst for fuel cells
EP3187262A1 (en) * 2011-02-08 2017-07-05 Johnson Matthey Fuel Cells Limited Catalyst for fuel cells
CN107195910A (en) * 2017-06-03 2017-09-22 上海博暄能源科技有限公司 One kind can discharge and recharge metal air battery cathodes and preparation method thereof
CN110416561A (en) * 2019-06-25 2019-11-05 华北电力大学 A kind of bifunctional electrocatalyst Pt-IrO2, preparation method
CN110416561B (en) * 2019-06-25 2020-12-01 华北电力大学 Bifunctional Pt-IrO2Nano-wire electro-catalyst, preparation method thereof and fuel cell
JP2023545163A (en) * 2020-10-13 2023-10-26 グリナリティ・ゲーエムベーハー Oxygen evolution catalysts, their production and use, membrane electrode arrangements, and fuel cells or electrolytic cells

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