CN102205252B - Method for synthesizing nano palladium particles with superactivity - Google Patents
Method for synthesizing nano palladium particles with superactivity Download PDFInfo
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- CN102205252B CN102205252B CN201010136791.2A CN201010136791A CN102205252B CN 102205252 B CN102205252 B CN 102205252B CN 201010136791 A CN201010136791 A CN 201010136791A CN 102205252 B CN102205252 B CN 102205252B
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Abstract
The invention provides a method for synthesizing nano palladium particles with superactivity and widens a method for preparing relevant nano particles. By creatively using iodobenzene as a surface modifying agent and adopting the characteristics that metal nano particles can be effectively absorbed and an effective steric hindrance effect can be provided by using phenyl of the iodobenzene, more stable nano palladium particles with high-content defects at the inner part and the surface are formed under the combined action of sudden reduction of reaction liquid temperature and polyvinyl pyrrolidone solubility caused by freezing acetone. The method has the characteristics of simple process, convenience for operation, controllable feature, wide application range and the like, and has a potential application value.
Description
Technical field
The present invention relates to a kind of preparation method of palladium nanoparticle catalyst, specifically, the method of utilizing exactly the agent of nano particle outer wrapping and temperature control to match, prepare a kind of internal structure and be rich in defect and comparatively stable palladium nano-particles, this nano particle is owing to having the defect of high-load, so there is potential using value at aspects such as electro-catalysis, belong to catalyst material field.
Background technology
Nearly ten years, the form controlledly synthesis of palladium nano-particles is caused to a lot of concerns in scientific circles, main because by metamorphosis, can effectively control the character such as catalysis, optics, electricity, magnetics of nano particle.Template guided synthetic, electrochemistry synthetic and the technology such as chemical synthesis is all applied to this, that but the pattern of palladium nano-particles is confined to is spherical, cube, tetrahedron, octahedron, line or bar structure etc., the achievement of radiation structure is little, the research of the higher internal energy more not also not causing due to a large amount of defects in radiation inside configuration.
Radiation structure, because it exists a large amount of crystal lattice boundaries, has a large amount of specific surface energies on surface, and due to relaxation and crystallization again, often this structure is difficult to maintain the long period, so aspect practical application, especially catalysis aspect shorter mention.In this patent, the temperature of acetone comes into question as forming the key factor of superactivity nano particle.Former reactant liquor reduces suddenly and the unexpected decline of the PVP solubility that acetone causes in temperature, makes PVP be coherent condition, and the while also makes to form because crystallization is imperfect in nano particle the defect of high-load.The gathering of PVP has caused the accumulation of the nano particle of parcel therein.Meanwhile, because nano grain surface has the iodobenzene of steric restriction effect, make this sedimentation more obvious.In research before, the iodo in iodobenzene has been found effectively to combine with palladium nano-particles, thereby in this patent, iodobenzene also can be protected the defect sturcture having formed in the accumulation that is used for promoting nano particle.
Summary of the invention
The invention provides a kind of method of preparing the method for palladium nanoparticle catalyst and having widened the relevant nano particle of preparation.
Creative use iodobenzene of the present invention is as coating material, utilize its effectively adsorbing metal nano particle, can utilize again its phenyl that effective steric restriction effect is provided, under the acting in conjunction that the reacting liquid temperature causing at freezing acetone and PVP solubility decline suddenly, form comparatively stablely, inner and surface all has the palladium nano-particles of high-load defect.The features such as it is simple that this method has technique, easy to operate, and pattern is controlled, applied range, have potential using value.
The present invention adopts following technical scheme:
1. prepare a method for Pd nanoparticle catalyst, comprise preparation, product separation, the washing process process of catalyst carrier, it is characterized in that comprising following step:
(1) first PVP and iodobenzene are dissolved in the ethylene glycol solution of 100 DEG C;
(2) then in reaction system, add K
2pdCl
4the aqueous solution;
(3) after reaction, reaction solution is poured in DEG C acetone of preprepared-30 while hot, centrifugation subsequently, then the mixed solution washing precipitation of using ethanol/acetone is for several times, to remove remaining ethylene glycol and excessive PVP, then precipitation is dissolved in ethanol again.
2. the method for preparing Pd nanoparticle catalyst as described in item 1, is characterized in that using iodobenzene as coating material, control its addition and be coating agent PVP 250 times.
3. as described in item 1, prepare the method for Pd nanoparticle catalyst, it is characterized in that by the addition control of metal be 1/100 of iodobenzene addition.
4. as described in item 1, prepare the method for Pd nanoparticle catalyst, it is characterized in that the solution after 3 hours adds in-30 DEG C of acetone while hot by reaction.
The preparation method of nanoparticle palladium catalyst provided by the present invention has the following advantages:
(1) metal nanoparticle of preparing is not easy to reunite, and monodispersity is fine.
(2) all there is the defect of high-load on inner and surface in the palladium nano-particles of preparing gained, and these defects keep chronic, can utilize with actual production in.
(3) with the breakthrough utilization of the method iodobenzene as coating material, later relevant nano particle preparation is had to reference function.
The present invention can be applicable at aspects such as electro-catalysis.
Brief description of the drawings
Fig. 1 superactivity palladium nano-particles is prepared schematic diagram.
Fig. 2 superactivity palladium nano-particles projection electromicroscopic photograph.
Fig. 3 superactivity palladium nano-particles high-resolution projection electromicroscopic photograph.
Fig. 4 superactivity palladium nano-particles EDS elementary analysis.
The superactivity palladium nano-particles projection electromicroscopic photograph that Fig. 5 places in normal temperature air.
Detailed description of the invention
1. first by a certain amount of 0.4g PVP, 0.28mL iodobenzene is dissolved in the 40mL ethylene glycol solution of 100 DEG C.
2. then in reaction system, dropwise add 0.025M K
2pdCl
4aqueous solution 1mL.
3. after reacting 3 hours, reaction solution is poured in DEG C acetone of preprepared-30 while hot, centrifugation subsequently, then the mixed solution washing precipitation of using ethanol/acetone is for several times, to remove remaining ethylene glycol and excessive PVP, then precipitation is dissolved in ethanol again.
Claims (4)
1. prepare a method for Pd nanoparticle catalyst, comprise preparation, product separation, the washing process process of catalyst carrier, it is characterized in that comprising following step:
(1) first PVP and iodobenzene are dissolved in the ethylene glycol solution of 100 DEG C;
(2) then in reaction system, add K
2pdCl
4the aqueous solution;
(3) after reaction, reaction solution is poured in DEG C acetone of preprepared-30 while hot, centrifugation subsequently, then the mixed solution washing precipitation of using ethanol/acetone is for several times, to remove remaining ethylene glycol and excessive PVP, then precipitation is dissolved in ethanol again.
2. the method for preparing as claimed in claim 1 Pd nanoparticle catalyst, is characterized in that using iodobenzene as coating material, control its addition and be coating agent PVP 250 times.
3. the method for preparing as claimed in claim 1 Pd nanoparticle catalyst, is characterized in that K
2pdCl
4add mole control be iodobenzene add mole 1/100.
4. prepare as claimed in claim 1 the method for Pd nanoparticle catalyst, it is characterized in that the solution after 3 hours adds in-30 DEG C of acetone while hot by reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010136791.2A CN102205252B (en) | 2010-03-31 | 2010-03-31 | Method for synthesizing nano palladium particles with superactivity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010136791.2A CN102205252B (en) | 2010-03-31 | 2010-03-31 | Method for synthesizing nano palladium particles with superactivity |
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| Publication Number | Publication Date |
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| CN102205252A CN102205252A (en) | 2011-10-05 |
| CN102205252B true CN102205252B (en) | 2014-06-11 |
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| CN201010136791.2A Active CN102205252B (en) | 2010-03-31 | 2010-03-31 | Method for synthesizing nano palladium particles with superactivity |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103909272B (en) * | 2012-12-31 | 2016-02-24 | 浙江海洋学院 | A kind of preparation method of multiway shape platinum nano material |
| CN104493153A (en) * | 2014-12-08 | 2015-04-08 | 中国科学院深圳先进技术研究院 | Palladium nanoparticles and preparation method thereof |
| CN110842212A (en) * | 2019-11-07 | 2020-02-28 | 南京师范大学 | Superfine Pd tetrahedral nano material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817458A (en) * | 2005-02-11 | 2006-08-16 | 罗门哈斯公司 | Method for preparing catalysts and the catalysts produced thereby |
| CN1972750A (en) * | 2004-02-18 | 2007-05-30 | 卢塞特国际英国有限公司 | A catalyst system |
| EP1840130A1 (en) * | 2005-01-21 | 2007-10-03 | Riken | Metal complex containing tridentate ligand, and polymerization catalyst comprising the same |
-
2010
- 2010-03-31 CN CN201010136791.2A patent/CN102205252B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1972750A (en) * | 2004-02-18 | 2007-05-30 | 卢塞特国际英国有限公司 | A catalyst system |
| EP1840130A1 (en) * | 2005-01-21 | 2007-10-03 | Riken | Metal complex containing tridentate ligand, and polymerization catalyst comprising the same |
| CN1817458A (en) * | 2005-02-11 | 2006-08-16 | 罗门哈斯公司 | Method for preparing catalysts and the catalysts produced thereby |
Non-Patent Citations (3)
| Title |
|---|
| Platinum Nanoparticles Stabilized by Polyvinylpyrrolidone for Hydrogenation;Nelly ZAKARINA 等;《Chinese Journal of Catalysis》;20081130;第29卷(第11期);第1165-1168页 * |
| Synthesis of Palladium Nanobricks with Atomic-Step Defects;Akrajas Ali Umar 等;《CRYSTAL GROWTH & DESIGN》;20081231;第8卷(第6期);第1808-1811页 * |
| 不使用保护气氛和还原剂超声制备纳米钯颗粒;王艳丽等;《材料研究学报》;20070630;第21卷(第3期);第329-332页 * |
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| CN102205252A (en) | 2011-10-05 |
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