CN1698962A - Preparation method for loading platinum nanoparticles on carbon carrier - Google Patents
Preparation method for loading platinum nanoparticles on carbon carrier Download PDFInfo
- Publication number
- CN1698962A CN1698962A CN 200510049593 CN200510049593A CN1698962A CN 1698962 A CN1698962 A CN 1698962A CN 200510049593 CN200510049593 CN 200510049593 CN 200510049593 A CN200510049593 A CN 200510049593A CN 1698962 A CN1698962 A CN 1698962A
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- Prior art keywords
- carbon
- carbon carrier
- preparation
- platinum nanoparticles
- acetate
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 44
- 229910052697 platinum Inorganic materials 0.000 title claims description 27
- 239000002105 nanoparticle Substances 0.000 title claims description 24
- 238000002360 preparation method Methods 0.000 title claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical group [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 229920005862 polyol Polymers 0.000 claims description 5
- 150000003077 polyols Chemical class 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000969 carrier Substances 0.000 claims description 2
- 239000008240 homogeneous mixture Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- CTUFHBVSYAEMLM-UHFFFAOYSA-N acetic acid;platinum Chemical compound [Pt].CC(O)=O.CC(O)=O CTUFHBVSYAEMLM-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 15
- 239000003223 protective agent Substances 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000012190 activator Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000002082 metal nanoparticle Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 150000005846 sugar alcohols Polymers 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000002638 heterogeneous catalyst Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 150000003057 platinum Chemical class 0.000 description 1
- QCSGLAMXZCLSJW-UHFFFAOYSA-L platinum(2+);diacetate Chemical compound [Pt+2].CC([O-])=O.CC([O-])=O QCSGLAMXZCLSJW-UHFFFAOYSA-L 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
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- Catalysts (AREA)
- Inert Electrodes (AREA)
Abstract
This invention discloses a method for loading platinum metal nanometer particles in the carbon carrier surface, which comprises the following steps: a) scattering carbon carrier on the polyatomic alcohol liquid with platinum metal salt and acetate; b) heating to 160-180 Deg.c, stirring and refluxing 2-3 hours; wherein each liter liquid has 1.2-15 g carbon carrier, 0.01-0.04 mole metal salt, 0-0.01 mole acetate. The loading quantity of platinum metal nanometer particles in the carbon carrier surface is 2%-40%. The particles have fine and even grain size, and the average size is about 3.0nm; besides, the method does not need any surface activator or polyaromatics protecting agent.
Description
Technical field
The present invention relates to the preparation of nano metal particles, relate in particular to the preparation method of loading platinum nanoparticles on carbon carrier, belong to the eelctro-catalyst field of catalyst preparation technical field and fuel cell.
Background technology
The platinum nanoparticles of carbon load has obtained using widely as heterogeneous catalyst in the chemical and fuel cell electro-catalyst with its excellent catalytic performance.But this carbon loading platinum nanoparticles catalyst traditional preparation process method mainly is based on dipping-reduction technique, just at first carbon carrier is immersed in the solution that contains slaine, make slaine be adsorbed on the carbon carrier surface, make its high temperature reduction under reducing atmosphere then.But thisly be difficult to the size of control load platinum particle on carbon carrier, and the dispersion of platinum particle on carbon carrier neither be very even, especially for the Pt/C catalyst of preparation high capacity amount based on traditional dipping-method of reducing.Document (Xue B for example, Chen P, Hong Q, etc., Growth of Pd, Pt, Ag and Au nanoparticles on carbon nanotubes, J.of Materials Chemistry, 2001,11 (19): 2378-2381) report employing immersion-reduction technique is 8nm in the average grain diameter of the ripple nano particle of carbon nano tube surface load, and particle size distribution is between 2-12nm.Also can adopt surfactant or polymer to prepare the nano metal particles of high degree of dispersion in addition, support on the carrier then as protective agent.But this method is very high to solvent, surfactant or protective agent and operating condition requirement, while complicated operation, cost height.And dispersed catalytic performance to catalyst has great influence on the size of platinum particle and uniformity and year carrier thereof.So the tiny and even also method of the nano metal particles of high degree of dispersion of a kind of simple and effective preparation load on carbon carrier has great importance for high performance Preparation of Catalyst.
Recently, the polyalcohol method is proved to be to prepare a kind of effective ways of metal nanoparticle.In this method, polyalcohol is as the solvent and the reducing agent of slaine.At high temperature polyalcohol makes the solution metal ion be reduced into metal nanoparticle as reducing agent.Can prepare the metal nanoparticle of particle diameter with polymer as protectant polyalcohol method at 1～2nm.But the metal nanoparticle of the polymer that this method obtains protection is difficult to directly load on the carbon carrier.As the application in catalyst field, the polymer protective agent must at high temperature be removed simultaneously, and metal nanoparticle can be reunited once more in the high-temperature process.
Summary of the invention
The purpose of this invention is to provide a kind of on carbon carrier the preparation method of loading platinum nanoparticles.
It is that carbon carrier is evenly dispersed in the liquid polyol that contains platinum salt and acetate, then said homogeneous mixture is heated to 160-180 ℃, and under constantly stirring backflow 2-3 hour; Contain 1.2～15 gram carbon carriers in every liter of liquid polyol, metalline is 0.01～0.04 mole, contains 0～0.01 mole of acetate.
The present invention has tiny and uniform particle diameter by the platinum nanoparticles of load on carbon carrier that this method obtains, and high degree of dispersion is on carbon carrier, and its average grain diameter is at 3.0nm.The load capacity of platinum particle on carbon carrier can reach 40%.Method of the present invention does not need to use any surfactant or polymer protective agent, has simple and the high characteristics of efficient.The Pt/C catalyst for preparing by method of the present invention has widely as the electrode catalyst of heterogeneous catalyst in the chemical and fuel cell to be used.
The specific embodiment
Embodiment 1:
The business-like XC-72 nano-sized carbon of 0.16 gram is evenly dispersed in 100 milliliters the ethylene glycol solution that contains 0.002 mole of chloroplatinic acid, the SAS that adds 0,0.25,0.5 and 0.7 milliliter 1 mol respectively, be heated to 170 ℃ then, and refluxed 3 hours.Get product to the end after washing after filtration and fully.The load capacity of platinum nanoparticles on carbon is 20%.Transmission electron microscope observing is the result show: do not add sodium acetate and add 0.25 in synthetic solvent, 0.5 and the SAS of 0.7 milliliter 1 mol resulting on the XC-72 nano-sized carbon average grain diameter of the platinum particle of load be respectively 4.5,3.4,3.1 and 2.9nm.
Embodiment 2:
The business-like XC-72 nano-sized carbon of 0.12 gram is evenly dispersed in 100 milliliters the ethylene glycol solution that contains 0.004 mole of chloroplatinic acid, adds the SAS of 0,0.5 and 1.0 milliliter 1 mol respectively, be heated to 175 ℃ then, and refluxed 3 hours.Get product to the end after washing after filtration and fully.The load capacity of platinum nanoparticles on carbon is 40%.Transmission electron microscope observing is the result show: in synthetic solvent, do not add sodium acetate and add 0.5 and 1.0 milliliter the SAS of 1 mol resulting on the XC-72 nano-sized carbon average grain diameter of the platinum particle of load be respectively 5.9,3.7 and 3.0nm.
Embodiment 3:
With 0.18 the gram even carbon nanotube be dispersed in 100 milliliters the ethylene glycol solution that contains 0.001 mole of potassium chloroplatinate, add the SAS of 0 and 0.5 milliliter 1 mol respectively, be heated to 170 ℃ then, and refluxed 3 hours.Get product to the end after washing after filtration and fully.The load capacity of platinum nanoparticles on carbon is 10%.Transmission electron microscope observing is the result show: in synthetic solvent, do not add sodium acetate and add 0.5 milliliter the SAS of 1 mol resulting on CNT the average grain diameter of the platinum particle of load be respectively 3.9 and 2.8nm.
Embodiment 4:
The active carbon of 1.52 grams is evenly dispersed in 100 milliliters the ethylene glycol solution that contains 0.004 molar acetate platinum, adds the SAS of 0 and 1.0 milliliter 1 mol respectively, be heated to 170 ℃ then, and refluxed 3 hours.Get product to the end after washing after filtration and fully.The load capacity of platinum nanoparticles on active carbon is 5%.Transmission electron microscope observing is the result show: in synthetic solvent, do not add sodium acetate and add 1.0 milliliters the SAS of 1 mol resulting on active carbon the average grain diameter of the platinum particle of load be respectively 3.3 and 2.7nm.
Embodiment 5:
The active carbon of 0.98 gram is evenly dispersed in 100 milliliters the ethylene glycol solution that contains 0.001 mole of chloroplatinic acid, adds the SAS of 0 and 0.5 milliliter 1 mol respectively, be heated to 170 ℃ then, and refluxed 2 hours.Get product to the end after washing after filtration and fully.The load capacity of platinum nanoparticles on active carbon is 2%.Transmission electron microscope observing is the result show: in synthetic solvent, do not add sodium acetate and add 0.5 milliliter the SAS of 1 mol resulting on active carbon the average grain diameter of the platinum particle of load be respectively 3.4 and 2.8nm.
Claims (5)
1. preparation method at carbon carrier area load platinum nanoparticles, it is characterized in that carbon carrier is dispersed in the liquid polyol that contains slaine and acetate, then this homogeneous mixture is heated to 160-180 ℃, and under constantly stirring backflow 2-3 hour; Contain 1.2～15 gram carbon carriers in every liter of liquid polyol, metalline is 0.01～0.04 mole, contains 0～0.01 mole of acetate.
2. according to the described a kind of preparation method of claim 1, it is characterized in that said slaine is: chloroplatinic acid, potassium chloroplatinate or platinum acetate at carbon carrier area load platinum nanoparticles.
3. according to the described a kind of preparation method of claim 1, it is characterized in that said acetate is sodium acetate at carbon carrier area load platinum nanoparticles.
4. according to the described a kind of preparation method of claim 1, it is characterized in that said liquid polyol is an ethylene glycol at carbon carrier area load platinum nanoparticles.
5. according to the described a kind of preparation method of claim 1, it is characterized in that said carrier carbon is: active carbon, XC-72 nano-sized carbon or CNT at carbon carrier area load platinum nanoparticles.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100495931A CN100336596C (en) | 2005-04-08 | 2005-04-08 | Preparation method for loading platinum nanoparticles on carbon carrier |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100495931A CN100336596C (en) | 2005-04-08 | 2005-04-08 | Preparation method for loading platinum nanoparticles on carbon carrier |
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| Publication Number | Publication Date |
|---|---|
| CN1698962A true CN1698962A (en) | 2005-11-23 |
| CN100336596C CN100336596C (en) | 2007-09-12 |
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| CNB2005100495931A Expired - Fee Related CN100336596C (en) | 2005-04-08 | 2005-04-08 | Preparation method for loading platinum nanoparticles on carbon carrier |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371079C (en) * | 2005-12-05 | 2008-02-27 | 浙江大学 | Method for preparing platinum/carbon nano electro catalyst by microwave synthesis |
| CN100428989C (en) * | 2006-09-06 | 2008-10-29 | 大连理工大学 | Method for preparing loading type nano Pd/C catalyst from colloidal solution |
| CN101192628B (en) * | 2006-11-30 | 2010-10-13 | 比亚迪股份有限公司 | Semi-conductor electrode and method for making and solar cell containing the semiconductor electrode |
| CN102687320A (en) * | 2009-06-10 | 2012-09-19 | 丰田自动车株式会社 | Electrode catalyst for fuel cell |
| CN103316669A (en) * | 2012-03-20 | 2013-09-25 | 上饶师范学院 | Construction method of Pt particle-loaded water dispersion carbon nanotubes by using phenol as predecessor |
| CN114904516A (en) * | 2021-02-06 | 2022-08-16 | 中国科学院青岛生物能源与过程研究所 | Method for preparing carbon carrier supported platinum-based nanoparticle catalyst by aid of functional small molecules |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150997C (en) * | 2002-12-27 | 2004-05-26 | 浙江大学 | Method for coating mono-metal particles on carbon nano tube surface |
| CN1253245C (en) * | 2004-03-04 | 2006-04-26 | 厦门大学 | Method of depositing high density loading metal platinum on carbon nanometer pipe surface using oriented chemistry |
-
2005
- 2005-04-08 CN CNB2005100495931A patent/CN100336596C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371079C (en) * | 2005-12-05 | 2008-02-27 | 浙江大学 | Method for preparing platinum/carbon nano electro catalyst by microwave synthesis |
| CN100428989C (en) * | 2006-09-06 | 2008-10-29 | 大连理工大学 | Method for preparing loading type nano Pd/C catalyst from colloidal solution |
| CN101192628B (en) * | 2006-11-30 | 2010-10-13 | 比亚迪股份有限公司 | Semi-conductor electrode and method for making and solar cell containing the semiconductor electrode |
| CN102687320A (en) * | 2009-06-10 | 2012-09-19 | 丰田自动车株式会社 | Electrode catalyst for fuel cell |
| CN103316669A (en) * | 2012-03-20 | 2013-09-25 | 上饶师范学院 | Construction method of Pt particle-loaded water dispersion carbon nanotubes by using phenol as predecessor |
| CN114904516A (en) * | 2021-02-06 | 2022-08-16 | 中国科学院青岛生物能源与过程研究所 | Method for preparing carbon carrier supported platinum-based nanoparticle catalyst by aid of functional small molecules |
| CN114904516B (en) * | 2021-02-06 | 2024-04-26 | 中国科学院青岛生物能源与过程研究所 | Method for preparing carbon carrier supported platinum-based nanoparticle catalyst with assistance of functional micromolecules |
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| CN100336596C (en) | 2007-09-12 |
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