CN105327700A - Method for preparing electrocatalysts through liquid-phase reduction of hydrogen at room temperature - Google Patents
Method for preparing electrocatalysts through liquid-phase reduction of hydrogen at room temperature Download PDFInfo
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- CN105327700A CN105327700A CN201510802112.3A CN201510802112A CN105327700A CN 105327700 A CN105327700 A CN 105327700A CN 201510802112 A CN201510802112 A CN 201510802112A CN 105327700 A CN105327700 A CN 105327700A
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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 method for preparing electrocatalysts through liquid-phase reduction of hydrogen at the room temperature. The method comprises steps as follows: firstly, platinum, palladium or platinum-palladium precious metal precursors are dissolved in ethylene glycol or a mixed solvent of ethylene glycol and water, the mixture and carbon supports are subjected to alternate ultrasonic treatment and stirring to form a suspension, and the pH value is adjusted to range from 9 to 10; then hydrogen is introduced into the suspension at the room temperature; suction filtration is performed finally, a filter cake is washed clean, vacuum-dried and ground, the carbon-supported fuel cell precious metal electrocatalysts are obtained, and the percentage of precious metal active components in the final carbon-supported fuel cell precious metal electrocatalysts is up to 10%-40%. The precious metal electrocatalysts prepared with the method have the small particle size and are evenly dispersed on the carbon supports; the preparation process is simple, environment-friendly, rapid and low in cost and is conducted at the room temperature, heating is not required, and industrial batch production is easy to realize.
Description
Technical field
The invention belongs to fuel cell electro-catalyst field, be specifically related to the preparation method that a kind of room temperature hydrogen liquid-phase reduction prepares eelctro-catalyst.
Background technology
In a fuel cell, eelctro-catalyst plays the effect of electrochemical reaction " factory ", is the core material in battery, and the development of eelctro-catalyst is one of key of fuel cell.Noble metal platinum, palladium or platinum-nickel alloys all have very high catalytic activity to the oxidation reaction of the fuel molecules such as hydrogen, formic acid, methyl alcohol, ethanol and redox reaction, therefore present stage business and the practical eelctro-catalyst overwhelming majority carries platinum for carbon or carbon carries palladium eelctro-catalyst.Commercialization eelctro-catalyst must ensure that particle diameter is enough little and be uniformly dispersed on the carbon carrier, to ensure to utilize noble metal active component to greatest extent.
Eelctro-catalyst preparation method has a lot, and the most frequently used has immersion reduction method and polyol reduction method.Solid phase immersion reduction method first noble metal precursor body and carbon carrier is flooded, and after drying and grinding, high temperature (being generally greater than 200 DEG C) is logical hydrogen reducing in tube furnace, and this method energy consumption is high, and noble metal skewness on the carbon carrier; Liquid infiltration and reduction method first noble metal precursor body and carbon carrier is flooded, then the reduction of the strong reductant such as boron hydride, formic acid room temperature is added, although this method is simple, fast and Non-energy-consumption, prepared eelctro-catalyst particle diameter is large and domain size distribution is uneven.Polyol reduction method makes the polyalcohols such as spent glycol simultaneously as solvent and reducing agent; heating (120 ~ 160 DEG C) 3 ~ 8 hours; noble metal precursor body is reduced to eelctro-catalyst; because polyalcohol plays protectant effect simultaneously; eelctro-catalyst particle diameter prepared by this method is little and be uniformly dispersed, and its shortcoming is that energy consumption is high, and the oxidation in course of reaction of the polyalcohols such as ethylene glycol itself; can not recycle, cost is high.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation process low energy consumption, simple, environmental protection, quick, with low cost, is easy to the preparation method realizing the noble metal electrocatalyst that bulk industrial is produced.
The present invention is achieved through the following technical solutions.
Room temperature hydrogen liquid-phase reduction prepares a preparation method for eelctro-catalyst, and concrete steps are as follows:
1) noble metal precursor body is dissolved in the mixed solvent of pure ethylene glycol solvent or ethylene glycol and water, with carbon carrier alternately ultrasonic, stir into suspension, adjust ph is 9 ~ 10;
2), then under room temperature, in suspension, hydrogen is passed into 1 ~ 10 minute;
3) last suction filtration, Washing of Filter Cake is clean, and vacuum drying, obtains carbon and carries fuel cell noble metal eelctro-catalyst after grinding;
Described noble metal precursor body is platinum or palladium or platinum palladium mixing presoma; The volume ratio of described ethylene glycol and water is 1:9 ~ 9:1; Described carbon carries noble metal active constituent mass in fuel cell noble metal eelctro-catalyst and accounts for 10 ~ 40% of eelctro-catalyst quality; Described carbon carrier is XC-72 carbon carrier or CNT.
Further, described noble metal precursor body is one or more in chloroplatinic acid, potassium chloroplatinate, platinic sodium chloride, the acid of chlorine palladium, chlorine palladium acid sodium and potassium chloropalladate.
With prior art ratio, tool of the present invention has the following advantages and technique effect:
1, reduction reaction preparation process of the present invention is at room temperature carried out, without the need to energy consumption, and the reaction time short (reduction reaction only needs 1 ~ 10 minute), significantly reduce the cost of preparation process;
2, the ethylene glycol that the present invention uses is solvent, itself does not participate in reaction, can recycle, completely different from common polyol reduction method;
3, the eelctro-catalyst particle diameter prepared of the present invention is little and be uniformly dispersed on the carbon carrier.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of platinum eelctro-catalyst prepared by embodiment 1.
Fig. 2 is the electromicroscopic photograph of palladium eelctro-catalyst prepared by embodiment 2.
Fig. 3 is the electromicroscopic photograph of platinum eelctro-catalyst prepared by embodiment 3.
Detailed description of the invention
Embodiment 1
74mg potassium chloroplatinate is dissolved in 50ml ethylene glycol, then adds 120mgXC-72 carbon carrier, alternately ultrasonic, stir into even prepared Chinese ink shape suspension, regulate the pH value of suspension to be 9.5; Then room temperature passes into hydrogen 10 minutes; Last suction filtration, Washing of Filter Cake is clean, and vacuum drying, obtain carbon after grinding and carry fuel cell platinum eelctro-catalyst, in eelctro-catalyst, the mass ratio of platinum is 20%.Fig. 1 is the transmission electron microscope photo of prepared platinum eelctro-catalyst, and the average grain diameter of platinum is 3.1nm.
Embodiment 2
111mg chlorine palladium acid sodium is dissolved in 75ml ethylene glycol, then adds 60mgXC-72 carbon carrier, alternately ultrasonic, stir into even prepared Chinese ink shape suspension, regulate the pH value of suspension to be 9.0; Then room temperature passes into hydrogen 1 minute; Last suction filtration, Washing of Filter Cake is clean, and vacuum drying, obtain carbon after grinding and carry fuel cell palladium eelctro-catalyst, in eelctro-catalyst, the mass ratio of palladium is 40%.Fig. 2 is the transmission electron microscope photo of prepared palladium eelctro-catalyst, and the average grain diameter of palladium is 3.6nm.
Embodiment 3
40mg six hydration chloroplatinic acid being dissolved in 50ml volume ratio is, in the ethylene glycol of 1:1 and the mixed solvent of water, then add 135mg CNT, alternately ultrasonic, stir into even prepared Chinese ink shape suspension, the pH value regulating suspension is 10.0; Then room temperature passes into hydrogen 6 minutes; Last suction filtration, Washing of Filter Cake is clean, and vacuum drying, obtain carbon nanotube loaded fuel cell platinum eelctro-catalyst after grinding, in eelctro-catalyst, the mass ratio of platinum is 10%.Fig. 3 is the transmission electron microscope photo of prepared platinum eelctro-catalyst, and the average grain diameter of platinum is 2.0nm.
Claims (2)
1. room temperature hydrogen liquid-phase reduction prepares a preparation method for eelctro-catalyst, it is characterized in that, concrete steps are as follows:
1) noble metal precursor body is dissolved in the mixed solvent of pure ethylene glycol solvent or ethylene glycol and water, with carbon carrier alternately ultrasonic, stir into suspension, adjust ph is 9 ~ 10;
2), then under room temperature, in suspension, hydrogen is passed into 1 ~ 10 minute;
3) last suction filtration, Washing of Filter Cake is clean, and vacuum drying, obtains carbon and carries fuel cell noble metal eelctro-catalyst after grinding;
Described noble metal precursor body is platinum or palladium or platinum palladium mixing presoma; The volume ratio of described ethylene glycol and water is 1:9 ~ 9:1; Described carbon carries noble metal active constituent mass in fuel cell noble metal eelctro-catalyst and accounts for 10 ~ 40% of eelctro-catalyst quality; Described carbon carrier is XC-72 carbon carrier or CNT.
2. a kind of room temperature hydrogen liquid-phase reduction according to claim 1 prepares the preparation method of eelctro-catalyst, it is characterized in that, described noble metal precursor body be chloroplatinic acid, potassium chloroplatinate, platinic sodium chloride, chlorine palladium acid, chlorine palladium acid sodium and potassium chloropalladate in one or more.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058272A (en) * | 2016-07-25 | 2016-10-26 | 北京工业大学 | Environmentally friendly one-step synthesis method of small-grain-size uniformly dispersed noble metal nanoparticle electro-catalyst |
| CN109289836A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of production hydrogen Pd process for synthetic catalyst |
| CN109289835A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of Pt process for synthetic catalyst of hydrogen evolution reaction |
| CN110612159A (en) * | 2017-05-01 | 2019-12-24 | 帝斯曼知识产权资产管理有限公司 | Improved method for depositing PD nanoparticles |
| CN112023977A (en) * | 2020-08-17 | 2020-12-04 | 西安交通大学 | Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst and preparation method thereof |
| CN112687895A (en) * | 2020-12-25 | 2021-04-20 | 苏州擎动动力科技有限公司 | Catalyst and preparation method thereof |
| CN114976078A (en) * | 2022-06-28 | 2022-08-30 | 中南大学 | Platinum-carbon catalyst for proton exchange membrane fuel cell and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106058272A (en) * | 2016-07-25 | 2016-10-26 | 北京工业大学 | Environmentally friendly one-step synthesis method of small-grain-size uniformly dispersed noble metal nanoparticle electro-catalyst |
| CN110612159A (en) * | 2017-05-01 | 2019-12-24 | 帝斯曼知识产权资产管理有限公司 | Improved method for depositing PD nanoparticles |
| CN109289836A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of production hydrogen Pd process for synthetic catalyst |
| CN109289835A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of Pt process for synthetic catalyst of hydrogen evolution reaction |
| CN112023977A (en) * | 2020-08-17 | 2020-12-04 | 西安交通大学 | Y-type molecular sieve packaged platinum group noble metal nanoparticle catalyst and preparation method thereof |
| CN112687895A (en) * | 2020-12-25 | 2021-04-20 | 苏州擎动动力科技有限公司 | Catalyst and preparation method thereof |
| CN114976078A (en) * | 2022-06-28 | 2022-08-30 | 中南大学 | Platinum-carbon catalyst for proton exchange membrane fuel cell and preparation method thereof |
| CN114976078B (en) * | 2022-06-28 | 2024-02-27 | 中南大学 | Platinum-carbon catalyst for proton exchange membrane fuel cell and preparation method thereof |
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Application publication date: 20160217 |