CN101716507A - Preparation method of platiniridium/carbon-electro catalyst by using microwave synthesis - Google Patents
Preparation method of platiniridium/carbon-electro catalyst by using microwave synthesis Download PDFInfo
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- CN101716507A CN101716507A CN200910153973A CN200910153973A CN101716507A CN 101716507 A CN101716507 A CN 101716507A CN 200910153973 A CN200910153973 A CN 200910153973A CN 200910153973 A CN200910153973 A CN 200910153973A CN 101716507 A CN101716507 A CN 101716507A
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Abstract
The invention discloses a preparation method of a platiniridium/carbon-electro catalyst by using microwave synthesis. The preparation method comprises the following steps of: evenly distributing nanometer carbon carriers in ethylene glycol solution containing both platinum metal salt and iridium metal salt at the same time, wherein the concentration of the platinum salt and the iridium salt is 0.001 to 0.01 mol/L; adding sodium acetate as a stabilizer, wherein the concentration of the sodium acetate in the resulting solution is 0.005 to 0.03 mol/L; then heating the well-distributed mixture of the nanometer carbon carriers and the metal salt ethylene glycol solution for 2 to 4 minutes by microwave radiation, and then filtering, washing and drying to obtain the platiniridium/carbon-electro catalysts. The atomic composition ratio of a platinum iridium alloy is PtxIry, wherein x is 0.1 to 1, and y is 0.1 to 1. The invention has the advantages that the nano-particles of the platinum iridium alloy, which are loaded on the surfaces of the carbon carriers, have small grain diameter averagely from 3 to 4 nm, and the grain diameter distribution is narrow, and the loading capacity of the alloy nano particles on the surface of the carbon carrier is 5% to 30%. The invention also has the advantages of high speed, simple process, high efficiency and energy saving. The platiniridium/carbon-electro catalyst is widely used in the field of electrochemical energy conversion.
Description
Technical field
That the present invention relates to is the preparation method of the synthetic platinoiridita of a kind of microwave/carbon eelctro-catalyst, belongs to catalyst preparation technical field and electrochemical energy technical field.
Background technology
DMFC (DMFCs) has high energy density and energy conversion efficiency, and low advantages such as operating temperature, has widely as small-sized portable power source and uses.Platinum has very high catalytic activity to methanol electrooxidation, poisons but the strong absorption of the intermediate product of methanol oxidation (CO etc.) on the platinum surface can make catalyst produce.In order to improve the anti-CO poisoning capability of platinum, the alloy that forms with platinum and other transition metal (as ruthenium, nickel, iridium etc.) replaces the anode catalyst of pure platinum as DMFCs, can improve the anti-CO poisoning capability of catalyst.
The particle size of metallic catalyst, uniformity and the dispersiveness on carrier thereof have material impact to its performance.And be difficult to be controlled at the size and the uniformity coefficient of metallic particles on the carbon carrier surface by traditional dipping-method of reducing.As a kind of fast, equal even energy-conservation heating means, carry out microwave radiation heating has been widely used for organic chemical reactions and nano material is synthetic.Because polyalcohols such as ethylene glycol have high dielectric constant, under the microwave radiation by Fast Heating, the synthetic solvent that makes polyalcohol at high temperature original position produces reducing agent, with the reduction of the precious metal ion in the solution, thereby can effectively control the particle size and the uniformity of metallic particles.Up to the present, utilizing the microwave polyol method to synthesize platinoiridita/carbon eelctro-catalyst does not also appear in the newspapers as yet.
Summary of the invention
The preparation method who the purpose of this invention is to provide the synthetic platinoiridita of a kind of microwave/carbon eelctro-catalyst.The preparation method of platinoiridita of the present invention/carbon eelctro-catalyst, be that the nano-sized carbon carrier is evenly dispersed in the ethylene glycol solution that contains platinum and two kinds of slaines of iridium simultaneously, the concentration of platinum salt and iridium salt is 0.001～0.01mol/L, add sodium acetate as stabilizing agent, the concentration of sodium acetate in synthetic solvent is 0.005～0.03mol/L, then with the homogeneous mixture 2～4min of this nano-sized carbon carrier of heating using microwave and slaine ethylene glycol solution, after filtration, wash, dry, acquisition platinoiridita/carbon eelctro-catalyst.The atom ratio of components of platinumiridio is Pt
xIr
y, x=0.1～1 wherein, y=0.1～1.
Wherein a kind of slaine in the said two kinds of slaines of the present invention is: chloroplatinic acid, potassium chloroplatinate; Another slaine is: chloro-iridic acid.Said heating using microwave has reflux.Said nano-sized carbon carrier is XC-72 carbon or CNT.
Advantage of the present invention is tiny at the platinumiridio nano particle diameter of nano-sized carbon carrier surface load, and average grain diameter is 3～4nm, and has narrow particle diameter distribution.The carrying capacity of alloy nano particle on the carbon carrier surface is 5%～30%.The present invention also has fast, simple, efficient and energy-saving advantages.This platinoiridita/carbon eelctro-catalyst has in electrochemical energy conversion field widely to be used.
The specific embodiment
Embodiment 1:
Chloroplatinic acid and chloro-iridic acid are dissolved in respectively in the ethylene glycol, are mixed with the solution that concentration is 0.002mol/L.Respectively get this solution of 50mL, it is 0.006mol/L that the adding sodium acetate makes its concentration in solution, in this solution, add 160mg XC-72 carbon again, mixture is transferred in the round-bottomed flask of 250mL after ultrasonic being uniformly dispersed, placed micro-wave oven, load onto reflux, heating using microwave 3min, after the cooling, solid product after filtration, the washing, 80 ℃ of oven dry.Obtain platinoiridita/XC-72 C catalyst (mass fraction of platinumiridio is 19.8%).Platinumiridio consist of Pt
1.0Ir
1.0The average grain diameter of transmission electron microscope observing platinumiridio nano particle is 3.2nm, particle diameter distribution 1～5nm.And with the platinumiridio nano particle average grain diameter 4.3nm of the XC-72 carbon load of traditional dipping-method of reducing preparation, particle diameter is distributed as 1～12nm.
Embodiment 2:
Chloroplatinic acid and chloro-iridic acid are dissolved in respectively in the ethylene glycol, are mixed with the solution that concentration is 0.002mol/L.Respectively get this solution of 50mL, it is 0.006mol/L that the adding sodium acetate makes its concentration in solution, in this solution, add the 160mg CNT again, mixture is transferred in the round-bottomed flask of 250mL after ultrasonic being uniformly dispersed, placed micro-wave oven, load onto reflux, heating using microwave 3min, after the cooling, solid product after filtration, the washing, 80 ℃ of oven dry.Obtain platinoiridita/carbon nano-tube catalyst (mass fraction of platinumiridio is 19.8%).Platinumiridio consist of Pt
1.0Ir
1.0The average grain diameter of transmission electron microscope observing platinumiridio nano particle is 3.2nm, particle diameter distribution 1～5nm.And with the carbon nanotube loaded platinumiridio nano particle average grain diameter 4.1nm of traditional dipping-method of reducing preparation, particle diameter is distributed as 1～11nm.
Embodiment 3:
Potassium chloroplatinate and chloro-iridic acid are dissolved in respectively in the ethylene glycol, are mixed with the solution that concentration is 0.002mol/L.Respectively get this solution of 50mL, it is 0.006mol/L that the adding sodium acetate makes its concentration in solution, in this solution, add the 160mg CNT again, mixture is transferred in the round-bottomed flask of 250mL after ultrasonic being uniformly dispersed, placed micro-wave oven, load onto reflux, heating using microwave 3min, after the cooling, solid product after filtration, the washing, 80 ℃ of oven dry.Obtain platinoiridita/carbon nano-tube catalyst (mass fraction of platinumiridio is 19.8%).Platinumiridio consist of Pt
1.0Ir
1.0The average grain diameter of transmission electron microscope observing platinumiridio nano particle is 3.3nm, particle diameter distribution 1～5nm.And with the carbon nanotube loaded platinumiridio nano particle average grain diameter 4.2nm of traditional dipping-method of reducing preparation, particle diameter is distributed as 1～12nm.
Embodiment 4:
Chloroplatinic acid and chloro-iridic acid are dissolved in respectively in the ethylene glycol, are mixed with the solution that concentration is 0.002mol/L.Respectively get this solution of 50mL, it is 0.006mol/L that the adding sodium acetate makes its concentration in solution, in this solution, add the 120mg CNT again, mixture is transferred in the round-bottomed flask of 250mL after ultrasonic being uniformly dispersed, placed micro-wave oven, load onto reflux, heating using microwave 3min, after the cooling, solid product after filtration, the washing, 80 ℃ of oven dry.Obtain platinoiridita/carbon nano-tube catalyst (mass fraction of platinumiridio is 24.7%).Platinumiridio consist of Pt
1.0Ir
1.0The average grain diameter of transmission electron microscope observing platinumiridio nano particle is 3.4nm, particle diameter distribution 1～5nm.And with the carbon nanotube loaded platinumiridio nano particle average grain diameter 4.4nm of traditional dipping-method of reducing preparation, particle diameter is distributed as 1～13nm.
Embodiment 5:
Chloroplatinic acid and chloro-iridic acid are dissolved in respectively in the ethylene glycol, are mixed with the solution that concentration is 0.002mol/L.Getting 75mL platinum acid chloride solution and 25mL Chloroiridic Acid solution mixes, adding sodium acetate then, to make its concentration in solution be 0.006mol/L, in this solution, add 160mg XC-72 carbon again, mixture is transferred in the round-bottomed flask of 250mL after ultrasonic being uniformly dispersed, placed micro-wave oven, load onto reflux, heating using microwave 3min, after the cooling, solid product after filtration, the washing, 80 ℃ of oven dry.Obtain platinoiridita/XC-72 C catalyst (mass fraction of platinumiridio is 19.9%).Platinumiridio consist of Pt
3.0Ir
1.0The average grain diameter of transmission electron microscope observing platinumiridio nano particle is 3.3nm, particle diameter distribution 1～5nm.And with the platinumiridio nano particle average grain diameter 4.4nm of the XC-72 carbon load of traditional dipping-method of reducing preparation, particle diameter is distributed as 1～12nm.
Embodiment 6:
Chloroplatinic acid and chloro-iridic acid are dissolved in respectively in the ethylene glycol, are mixed with the solution that concentration is 0.002mol/L.Getting 25mL platinum acid chloride solution and 75mL Chloroiridic Acid solution mixes, adding sodium acetate then, to make its concentration in solution be 0.006mol/L, in this solution, add 160mg XC-72 carbon again, mixture is transferred in the round-bottomed flask of 250mL after ultrasonic being uniformly dispersed, placed micro-wave oven, load onto reflux, heating using microwave 3min, after the cooling, solid product after filtration, the washing, 80 ℃ of oven dry.Obtain platinoiridita/XC-72 C catalyst (mass fraction of platinumiridio is 19.5%).Platinumiridio consist of Pt
3.0Ir
1.0The average grain diameter of transmission electron microscope observing platinumiridio nano particle is 3.2nm, particle diameter distribution 1～5nm.And with the platinumiridio nano particle average grain diameter 4.3nm of the XC-72 carbon load of traditional dipping-method of reducing preparation, particle diameter is distributed as 1～12nm.
Claims (4)
1. the preparation method of the synthetic platinoiridita of a microwave/carbon eelctro-catalyst, it is characterized in that the nano-sized carbon carrier is evenly dispersed in the ethylene glycol solution that contains platinum and two kinds of slaines of iridium simultaneously, the concentration of platinum salt and iridium salt is 0.001～0.01mol/L, add sodium acetate as stabilizing agent, the concentration of sodium acetate in synthetic solvent is 0.005～0.03mol/L, then with the homogeneous mixture 2～4min of this nano-sized carbon carrier of heating using microwave and slaine ethylene glycol solution, after filtration, wash, dry, acquisition platinoiridita/carbon eelctro-catalyst.The atom ratio of components of platinumiridio is Pt
xIr
y, x=0.1～1 wherein, y=0.1～1.
2. a kind of microwave according to claim 1 synthesizes the preparation method of platinoiridita/carbon eelctro-catalyst, it is characterized in that the wherein a kind of slaine in said two kinds of slaines is: chloroplatinic acid, potassium chloroplatinate; Another slaine is: chloro-iridic acid.
3. a kind of microwave according to claim 1 synthesizes the preparation method of platinoiridita/carbon eelctro-catalyst, it is characterized in that said heating using microwave has reflux.
4. a kind of microwave according to claim 1 synthesizes the preparation method of platinoiridita/carbon eelctro-catalyst, it is characterized in that said nano-sized carbon carrier is XC-72 carbon or CNT.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966458A (en) * | 2010-09-30 | 2011-02-09 | 昆明理工大学 | Preparation method of Ir and Ir-Pt/C alloy nano-catalyst with high dispersion and high load capacity |
| CN105214653A (en) * | 2015-08-28 | 2016-01-06 | 北京化工大学 | A kind of preparation method of carbon nanotube loaded nanoparticle catalyst |
| CN109226740A (en) * | 2018-09-30 | 2019-01-18 | 青岛科技大学 | A kind of iridium nanoparticle and its application in catalytic growth carbon nanotube |
| CN111554946A (en) * | 2020-04-23 | 2020-08-18 | 广东道氏云杉氢能科技有限公司 | Pt alloy with high HOR catalytic activity and preparation method and application thereof |
| CN113368852A (en) * | 2021-06-10 | 2021-09-10 | 中山大学 | Preparation method and application of carbon-supported Ir-based alloy catalyst with high hydrogenation selectivity |
| CN113546622A (en) * | 2021-06-03 | 2021-10-26 | 南京大学 | Catalyst for catalytic oxidation of toluene at low temperature and high activity, and preparation method and application thereof |
| CN115156546A (en) * | 2021-03-19 | 2022-10-11 | 北京化工大学 | Preparation method of monodisperse PtM alloy nanoparticles or nanoclusters |
-
2009
- 2009-11-30 CN CN200910153973A patent/CN101716507A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966458A (en) * | 2010-09-30 | 2011-02-09 | 昆明理工大学 | Preparation method of Ir and Ir-Pt/C alloy nano-catalyst with high dispersion and high load capacity |
| CN105214653A (en) * | 2015-08-28 | 2016-01-06 | 北京化工大学 | A kind of preparation method of carbon nanotube loaded nanoparticle catalyst |
| CN109226740A (en) * | 2018-09-30 | 2019-01-18 | 青岛科技大学 | A kind of iridium nanoparticle and its application in catalytic growth carbon nanotube |
| CN111554946A (en) * | 2020-04-23 | 2020-08-18 | 广东道氏云杉氢能科技有限公司 | Pt alloy with high HOR catalytic activity and preparation method and application thereof |
| CN111554946B (en) * | 2020-04-23 | 2022-05-17 | 广东泰极动力科技有限公司 | Pt alloy with high HOR catalytic activity and preparation method and application thereof |
| CN115156546A (en) * | 2021-03-19 | 2022-10-11 | 北京化工大学 | Preparation method of monodisperse PtM alloy nanoparticles or nanoclusters |
| CN113546622A (en) * | 2021-06-03 | 2021-10-26 | 南京大学 | Catalyst for catalytic oxidation of toluene at low temperature and high activity, and preparation method and application thereof |
| CN113368852A (en) * | 2021-06-10 | 2021-09-10 | 中山大学 | Preparation method and application of carbon-supported Ir-based alloy catalyst with high hydrogenation selectivity |
| CN113368852B (en) * | 2021-06-10 | 2022-07-12 | 中山大学 | Preparation method and application of carbon-supported Ir-based alloy catalyst with high hydrogenation selectivity |
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Open date: 20100602 |