CN100371079C - Method for preparing platinum/carbon nano electro catalyst by microwave synthesis - Google Patents
Method for preparing platinum/carbon nano electro catalyst by microwave synthesis Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 238000000034 method Methods 0.000 title abstract description 25
- 239000010411 electrocatalyst Substances 0.000 title abstract description 11
- 230000015572 biosynthetic process Effects 0.000 title abstract description 5
- 238000003786 synthesis reaction Methods 0.000 title abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 44
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 33
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000001632 sodium acetate Substances 0.000 claims abstract description 24
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims description 65
- 239000002904 solvent Substances 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002048 multi walled nanotube Substances 0.000 claims description 17
- 239000012265 solid product Substances 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 239000002041 carbon nanotube Substances 0.000 claims description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- CTUFHBVSYAEMLM-UHFFFAOYSA-N acetic acid;platinum Chemical compound [Pt].CC(O)=O.CC(O)=O CTUFHBVSYAEMLM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052799 carbon Inorganic materials 0.000 abstract description 17
- 239000003381 stabilizer Substances 0.000 abstract description 17
- 150000003057 platinum Chemical class 0.000 abstract description 5
- 239000000446 fuel Substances 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 60
- 239000002105 nanoparticle Substances 0.000 description 13
- 230000005540 biological transmission Effects 0.000 description 12
- 238000006056 electrooxidation reaction Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000002109 single walled nanotube Substances 0.000 description 6
- 150000005846 sugar alcohols Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000002082 metal nanoparticle Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003223 protective agent Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical group Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The present invention discloses a preparation method of nanometer platinum/carbon electrocatalysts by microwave synthesis. Platinum salts are dissolved in ethylene glycol, the concentration of the platinum salts in a solution is from 0.001 to 0.008 mol/L, a sodium acetate solution is added as stabilizing agents, and the concentration of sodium acetate in the synthesized solution is from 0.005 to 0.03 mol/L. Nanometer carbon carriers are added and are sufficiently dispersed by ultrasonic waves in the solution, the uniform mixtures are heated in a microwave oven, and the nanometer platinum/carbon electrocatalysts whose mass percent of platinum is from 10 to 40% are obtained through filtration, wash and drying. Nanometer platinum particles in the Pt/C electrocatalysts synthesized by the method of the present invention have uniform particle size, and the Pt/C electrocatalysts synthesized by the method of the present invention have good electrocatalytic performance and can be extensively applied to fuel cells.
Description
Technical field
The present invention relates to the preparation of nano material, relate in particular to a kind of preparation method of platinum/carbon nano electro catalyst by microwave synthesis.
Background technology
Platinum/the material with carbon element of the platinum nanoparticles of carbon load is with its excellent catalytic performance, and as the catalyst in the chemical, the eelctro-catalyst in the battery that especially acts as a fuel has obtained using widely.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 etc. for example, Growthof 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 platinum nanoparticles 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 the size of platinum particle has great influence to the electrocatalysis characteristic of Pt/C catalyst.The particle diameter of general platinum nanoparticles is about 3 nanometers, and the Pt/C catalyst has higher electrocatalysis characteristic.
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, influences the electrocatalysis characteristic of catalyst.
The inventor disclosed in the past and had a kind ofly added a spot of SAS as stabilizing agent in synthetic solvent, method (the Chen Weixiang etc. that in the liquid polyhydric alcoholic solution, directly synthesize the Pt/C catalyst, a kind of on carbon carrier the preparation method of loading platinum nanoparticles, application number: 200510049593.1).Adopted traditional heat conduction heating means in this building-up process, heat time heating time is generally at 2～3 hours.Owing to need the heating of long period, consumed a large amount of electric energy, also reduced combined coefficient.
Heating using microwave has fast, evenly, and energy-conservation and high efficiency advantage.Be used widely in microwave heating technique synthetic and nano material at organic chemistry synthetic recently, it can make reaction speed improve about 10～100 times.Replace traditional heat conduction heating means with heating using microwave, can shorten heat time heating time greatly, thereby reduce the consumption of electric energy and improve combined coefficient.But up to the present, in synthetic solvent, add SAS, yet there are no the report of pertinent literature with the synthetic platinum/carbon nano electro catalyst of the polyalcohol technology of heating using microwave as stabilizing agent.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of platinum/carbon nano electro catalyst by microwave synthesis.
It is that platinum salt is dissolved in the ethylene glycol, the concentration of platinum salt in solution is 0.001～0.008mol/L, add SAS as stabilizing agent, the concentration of sodium acetate in synthetic solvent is 0.005～0.03mol/L, add the nano-sized carbon carrier, with the ultrasonic wave processing nano-carbon material is fully disperseed in solution, should in micro-wave oven, heat 2.0～4.0 minutes by uniform mixture.Through overanxious, washing, oven dry, the mass percent that obtains platinum is 10～40% platinum/carbon nano electro catalyst.
Described platinum salt is chloroplatinic acid, potassium chloroplatinate or platinum acetate.Have reflux during heating using microwave.The nano-sized carbon carrier is XC-72 nano-sized carbon or CNT.CNT is multi-walled carbon nano-tubes or SWCN.CNT is reflow treatment 3 hours in red fuming nitric acid (RFNA) before use, and reflux temperature is 100 ℃.
Method of the present invention compared with the prior art has following outstanding advantage:
Advantage of the present invention is to add a spot of SAS as stabilizing agent in synthetic solvent, with the synthetic platinum/carbon nano electro catalyst of the polyalcohol technology of microwave assistant heating.Nano platinum particle has tiny and uniform particle diameter in the catalyst that is synthesized, and average grain diameter can be regulated and control about 3.0nm, and nano platinum particle is uniformly dispersed at the nano-sized carbon carrier.
Method of the present invention can be synthesized the Pt/C nanometer electrical catalyst of high capacity amount, and the load capacity of platinum can reach 40% (mass fraction).
Compare with traditional heat conduction heating technique synthetic method, the present invention has adopted microwave heating technique, have fast, evenly, the energy-conservation and high advantage of efficient.
The synthetic Pt/C nanometer electrical catalyst of the inventive method has good catalytic action, and the eelctro-catalyst of the battery that acts as a fuel has widely to be used.
The specific embodiment
Embodiment 1:
Chloroplatinic acid is dissolved in the ethylene glycol, is mixed with the solution that concentration is 0.002mol/L.Get 100 milliliters of these solution, add the SAS of 1.0 milliliters of 1mol/L then, sodium acetate concentration in synthetic solvent is 0.01mol/L.The XC-72 nano-sized carbon that in this synthetic solvent, adds 160 milligrams again, and handle with ultrasonic wave it is mixed.At last will this uniform mixture transfer in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, add reflux after, heating using microwave 2.5 minutes.After the cooling, solid product passes through overanxious and fully washs with acetone and deionized water, 90 ℃ of oven dry, obtains Pt/XC-72 nanometer electrical catalyst (mass fraction of platinum is 20%).Nano platinum particle has uniform particle diameter in the transmission electron microscope observing Pt/XC-72 nanometer electrical catalyst, and average grain diameter is 2.8 nanometers.
As a comparison, in synthetic solvent, do not add SAS, with the synthetic Pt/XC-72 nanometer electrical catalyst (mass fraction of platinum is 20%) of same condition.The particle diameter of nano platinum particle is inhomogeneous in the transmission electron microscope observing Pt/XC-72 nanometer electrical catalyst, and average grain diameter is 5.1 nanometers.
The electrocatalysis characteristic compare test is relatively: the Nafion solution and the deionized water of a little P t/XC-72 nanometer electrical catalyst and an amount of 5% are mixed under the ultrasonic wave effect, should be coated on the glassy carbon electrode by uniform mixture, dry the back down as measuring working electrode at 80 ℃.Reference electrode is saturated calomel electrode (SCE) during measurement, and electrolyte is 2M CH
3OH+1M H
2SO
4, platinized platinum is to electrode.Estimate the electro catalytic activity of Pt/XC-72 nanometer electrical catalyst with cyclic voltammetry experiment to methanol electrooxidation.The peak current that records methanol electro-oxidizing on the above-mentioned Pt/XC-72 nanometer electrical catalyst that synthesizes as the stabilizing agent microwave with sodium acetate under the same terms is 10.3mA; Do not add sodium acetate as the stabilizing agent situation under on the synthetic Pt/XC-72 nanometer electrical catalyst of microwave the peak current of methanol electro-oxidizing be 5.2mA.Illustrate that the former has more high electrocatalytic active than the latter to the electrochemical oxidation of methyl alcohol.
Embodiment 2:
Potassium chloroplatinate is dissolved in the ethylene glycol, is mixed with the solution that concentration is 0.001mol/L.Get 100 milliliters of these solution, add the SAS of 0.6 milliliter of 1mol/L then, sodium acetate concentration in synthetic solvent is 0.006mol/L.The multi-walled carbon nano-tubes that in this synthetic solvent, adds 80 milligrams again, and handle with ultrasonic wave it is mixed.At last will this uniform mixture transfer in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, add reflux after, heating using microwave 2.5 minutes.After the cooling, solid product passes through overanxious and fully washs with acetone and deionized water, 90 ℃ of oven dry, obtains Pt/CNTs nanometer electrical catalyst (mass fraction of platinum is 20%).Nano platinum particle has uniform particle diameter in the transmission electron microscope observing Pt/MWCNTs nanometer electrical catalyst, and average grain diameter is 3.0 nanometers.
As a comparison, in synthetic solvent, do not add SAS, with the synthetic Pt/MWCNTs nanometer electrical catalyst (mass fraction of platinum is 20%) of same condition.The average grain diameter of nano platinum particle is 4.9 nanometers in the transmission electron microscope observing Pt/MWCNTs nanometer electrical catalyst.
The electrocatalysis characteristic of two kinds of Pt/MWCNTs nanometer electrical catalysts is compared in the method test of pressing embodiment 1.The peak current that records methanol electro-oxidizing on the Pt/MWCNTs nanometer electrical catalyst that synthesizes as the stabilizing agent microwave with sodium acetate under the same terms is 10.6mA; Do not add sodium acetate as the stabilizing agent situation under on the synthetic Pt/C nanometer electrical catalyst of microwave the peak current of methanol electro-oxidizing be 5.4mA.Illustrate that the former has more high electrocatalytic active than the latter to the electrochemical oxidation of methyl alcohol.
Embodiment 3:
Chloroplatinic acid is dissolved in the ethylene glycol, is mixed with the solution that concentration is 0.001mol/L.Get 100 milliliters of these solution, add the SAS of 0.5 milliliter of 1mol/L then, sodium acetate concentration in synthetic solvent is 0.005mol/L.The SWCN that in this synthetic solvent, adds 80 milligrams again, and handle with ultrasonic wave it is mixed.At last will this uniform mixture transfer in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, add reflux after, heating using microwave 2.5 minutes.After the cooling, solid product passes through overanxious and fully washs with acetone and deionized water, 90 ℃ of oven dry, obtains Pt/SWCNTs nanometer electrical catalyst (mass fraction of platinum is 20%).The nano platinum particle particle diameter is even in the transmission electron microscope observing Pt/SWCNTs nanometer electrical catalyst, and average grain diameter is 3.1 nanometers.
As a comparison, in synthetic solvent, do not add SAS, with the synthetic Pt/SWCNTs nanometer electrical catalyst (mass fraction of platinum is 20%) of same condition.The average grain diameter of nano platinum particle is 4.7 nanometers in the transmission electron microscope observing Pt/SWCNTs nanometer electrical catalyst.
The electrocatalysis characteristic of two kinds of Pt/SWCNTs nanometer electrical catalysts is compared in the method test of pressing embodiment 1.The peak current that records methanol electro-oxidizing on the Pt/SWCNTs nanometer electrical catalyst that synthesizes as the stabilizing agent microwave with sodium acetate under the same terms is 9.8mA; Do not add sodium acetate as the stabilizing agent situation under on the synthetic Pt/C nanometer electrical catalyst of microwave the peak current of methanol electro-oxidizing be 4.7mA.Illustrate that the former has more high electrocatalytic active than the latter to the electrochemical oxidation of methyl alcohol.
Embodiment 4:
Platinum acetate is dissolved in the ethylene glycol, is mixed with the solution that concentration is 0.002mol/L.Get 100 milliliters of these solution, add the SAS of 0.8 milliliter of 1mol/L then, sodium acetate concentration in synthetic solvent is 0.008mol/L.The multi-walled carbon nano-tubes that in this synthetic solvent, adds 160 milligrams again, and handle with ultrasonic wave it is mixed.At last will this uniform mixture transfer in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, add reflux after, heating using microwave 3.0 minutes.After the cooling, solid product passes through overanxious and fully washs with acetone and deionized water, 90 ℃ of oven dry, obtains Pt/CNTs nanometer electrical catalyst (mass fraction of platinum is 20%).Nano platinum particle has uniform particle diameter in the transmission electron microscope observing Pt/MWCNTs nanometer electrical catalyst, and average grain diameter is 2.9 nanometers.
As a comparison, in synthetic solvent, do not add SAS, with the synthetic Pt/MWCNTs nanometer electrical catalyst (mass fraction of platinum is 20%) of same condition.The average grain diameter of nano platinum particle is 3.8 nanometers in the transmission electron microscope observing Pt/MWCNTs nanometer electrical catalyst.
The electrocatalysis characteristic of two kinds of Pt/MWCNTs nanometer electrical catalysts is compared in the method test of pressing embodiment 1.The peak current that records methanol electro-oxidizing on the Pt/MWCNTs nanometer electrical catalyst that synthesizes as the stabilizing agent microwave with sodium acetate under the same terms is 10.1mA; Do not add sodium acetate as the stabilizing agent situation under on the synthetic Pt/C nanometer electrical catalyst of microwave the peak current of methanol electro-oxidizing be 6.8mA.Illustrate that the former has more high electrocatalytic active than the latter to the electrochemical oxidation of methyl alcohol.
Embodiment 5:
Chloroplatinic acid is dissolved in the ethylene glycol, is mixed with the solution that concentration is 0.008mol/L.Get 100 milliliters of these solution, add the SAS of 3.0 milliliters of 1mol/L then, sodium acetate concentration in synthetic solvent is 0.03mol/L.The XC-72 nano-sized carbon that in this synthetic solvent, adds 240 milligrams again, and handle with ultrasonic wave it is mixed.At last will this uniform mixture transfer in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, add reflux after, heating using microwave 4.0 minutes.After the cooling, solid product passes through overanxious and fully washs with acetone and deionized water, 90 ℃ of oven dry, obtains Pt/XC-72 nanometer electrical catalyst (mass fraction of platinum is 40%).Nano platinum particle has uniform particle diameter in the transmission electron microscope observing Pt/XC-72 nanometer electrical catalyst, and average grain diameter is 3.4 nanometers.
As a comparison, in synthetic solvent, do not add SAS, with the synthetic Pt/C nanometer electrical catalyst (mass fraction of platinum is 40%) of same condition.The particle diameter of nano platinum particle is inhomogeneous in the transmission electron microscope observing Pt/XC-72 nanometer electrical catalyst, and average grain diameter is 6.2 nanometers.
The electrocatalysis characteristic of two kinds of Pt/XC-72 nanometer electrical catalysts is compared in the method test of pressing embodiment 1.The peak current that records methanol electro-oxidizing on the Pt/XC-72 nanometer electrical catalyst that synthesizes as the stabilizing agent microwave with sodium acetate under the same terms is 15.2mA; Do not add sodium acetate as the stabilizing agent situation under on the synthetic Pt/C nanometer electrical catalyst of microwave the peak current of methanol electro-oxidizing be 7.1mA.Illustrate that the former has more high electrocatalytic active than the latter to the electrochemical oxidation of methyl alcohol.
Embodiment 6:
Chloroplatinic acid is dissolved in the ethylene glycol, is mixed with the solution that concentration is 0.002mol/L.Get 100 milliliters of these solution, add the SAS of 1.0 milliliters of 1mol/L then, sodium acetate concentration in synthetic solvent is 0.01mol/L.The XC-72 nano-sized carbon that in this synthetic solvent, adds 180 milligrams again, and handle with ultrasonic wave it is mixed.At last will this uniform mixture transfer in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, add reflux after, heating using microwave 2 minutes.After the cooling, solid product passes through overanxious and fully washs with acetone and deionized water, 90 ℃ of oven dry, obtains Pt/XC-72 nanometer electrical catalyst (mass fraction of platinum is 10%).Nano platinum particle has uniform particle diameter in the transmission electron microscope observing Pt/XC-72 nanometer electrical catalyst, and average grain diameter is 3.2 nanometers.
As a comparison, in synthetic solvent, do not add SAS, with the synthetic Pt/C nanometer electrical catalyst (mass fraction of platinum is 10%) of same condition.The particle diameter of nano platinum particle is inhomogeneous in the transmission electron microscope observing Pt/XC-72 nanometer electrical catalyst, and average grain diameter is 4.5 nanometers.
The electrocatalysis characteristic of two kinds of Pt/XC-72 nanometer electrical catalysts is compared in the method test of pressing embodiment 1.The peak current that records methyl alcohol methanol electro-oxidizing on the Pt/XC-72 nanometer electrical catalyst that synthesizes as the stabilizing agent microwave with sodium acetate under the same terms is 6.3mA; Do not add sodium acetate as the stabilizing agent situation under on the synthetic Pt/C nanometer electrical catalyst of microwave the peak current of methanol electro-oxidizing be 3.8mA.Illustrate that the former has more high electrocatalytic active than the latter to the electrochemical oxidation of methyl alcohol.
Claims (3)
1. the preparation method of the synthetic platinum/carbon nano-tube eelctro-catalyst of a microwave, it is characterized in that chloroplatinic acid is dissolved in and be mixed with solution in the ethylene glycol, the concentration of chloroplatinic acid in above-mentioned solution is 0.001mol/L, the SAS that adds 0.5 milliliter of 1mol/L in 100 milliliters of above-mentioned solution constitutes synthetic solvent, the concentration of sodium acetate in above-mentioned synthetic solvent is 0.005mol/L, add 80 milligrams of SWCNs then, make SWCN in above-mentioned synthetic solvent, fully disperse to obtain uniform mixture with the ultrasonic wave processing, described uniform mixture transferred in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, after adding reflux, heating using microwave 2.5 minutes, cool off then, filter then and obtain solid product, and fully wash described solid product, 90 ℃ of oven dry with acetone and deionized water, obtain described eelctro-catalyst, the mass percent of the platinum in the wherein said eelctro-catalyst is 20%.
2. the preparation method of the synthetic platinum/carbon nano-tube eelctro-catalyst of a microwave, it is characterized in that potassium chloroplatinate is dissolved in and be mixed with solution in the ethylene glycol, the concentration of potassium chloroplatinate in above-mentioned solution is 0.001mol/L, the SAS that adds 0.6 milliliter of 1mol/L in 100 milliliters of above-mentioned solution constitutes synthetic solvent, the concentration of sodium acetate in above-mentioned synthetic solvent is 0.006mol/L, add 80 milligrams of multi-walled carbon nano-tubes then, make multi-walled carbon nano-tubes in above-mentioned synthetic solvent, fully disperse to obtain uniform mixture with the ultrasonic wave processing, described uniform mixture transferred in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, after adding reflux, heating using microwave 2.5 minutes, cool off then, filter then and obtain solid product, and fully wash described solid product, 90 ℃ of oven dry with acetone and deionized water, obtain described eelctro-catalyst, the mass percent of the platinum in the wherein said eelctro-catalyst is 20%.
3. the preparation method of the synthetic platinum/carbon nano-tube eelctro-catalyst of a microwave, it is characterized in that platinum acetate is dissolved in and be mixed with solution in the ethylene glycol, the concentration of platinum acetate in above-mentioned solution is 0.002mol/L, the SAS that adds 0.8 milligram of 1mol/L in 100 milliliters of above-mentioned solution constitutes synthetic solvent, sodium acetate is 0.008mol/L in above-mentioned concentration in above-mentioned synthetic solvent, add 160 milligrams of multi-walled carbon nano-tubes then, make multi-walled carbon nano-tubes in above-mentioned synthetic solvent, fully disperse to obtain uniform mixture with the ultrasonic wave processing, described uniform mixture transferred in 250 milliliters the round-bottomed flask, and be placed in the micro-wave oven, after adding reflux, heating using microwave 3.0 minutes, cool off then, filter then and obtain solid product, and fully wash described solid product, 90 ℃ of oven dry with acetone and deionized water, obtain described eelctro-catalyst, the mass percent of the platinum in the wherein said eelctro-catalyst is 20%.
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| CN100531901C (en) * | 2008-05-08 | 2009-08-26 | 郴州高鑫铂业有限公司 | Preparation method of high-activity nanocrystalline platinum carbon catalyst |
| CN103372429B (en) * | 2013-07-04 | 2015-04-22 | 南京大学昆山创新研究院 | Preparation method of Pt/C (platinum/carbon) catalyst for fuel cell |
| CN105327700A (en) * | 2015-11-18 | 2016-02-17 | 华南理工大学 | Method for preparing electrocatalysts through liquid-phase reduction of hydrogen at room temperature |
| CN105363435B (en) * | 2015-12-09 | 2018-03-27 | 广东南海普锐斯科技有限公司 | A kind of preparation method of oxygen reduction electro-catalyst Pt/N carbon nanocoils |
| CN109755602A (en) * | 2018-12-26 | 2019-05-14 | 武汉喜玛拉雅光电科技股份有限公司 | A kind of platinum carbon catalyst and preparation method thereof for fuel cell manufacture |
| CN116072897A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Platinum carbon catalyst, preparation method and application thereof and hydrogen fuel cell |
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| Pt/CNT纳米催化剂的微波快速合成及其对甲醇电化学氧化的电催化性能。. 陈卫祥等。.高等学校化学学报，第24卷第12期. 2003 * |
| 微波合成碳负载纳米铂催化剂及其对甲醇氧化的电催化性能。. 陈卫祥等。.化学学报，第62卷第1期. 2004 * |
| 醋酸盐稳定的Pt/C纳米粒子的微波合成及其对甲醇的电催化氧化。. 赵杰等。.第十三次全国电化学会议论文摘要集(下集). 2005 * |
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