CN102205252A - Method for synthesizing nano palladium particles with superactivity - Google Patents

Method for synthesizing nano palladium particles with superactivity Download PDF

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Publication number
CN102205252A
CN102205252A CN2010101367912A CN201010136791A CN102205252A CN 102205252 A CN102205252 A CN 102205252A CN 2010101367912 A CN2010101367912 A CN 2010101367912A CN 201010136791 A CN201010136791 A CN 201010136791A CN 102205252 A CN102205252 A CN 102205252A
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iodobenzene
particles
preparing
acetone
nano
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CN102205252B (en
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曹荣
郑兆亮
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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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

A kind of synthetic method of superactivity nanometer palladium particle
Technical field
The present invention relates to a kind of preparation method of palladium nanoparticle catalyst, specifically, the method of utilizing the control of agent of nano particle outer wrapping and temperature to match exactly, prepare a kind of internal structure and be rich in defective and comparatively stable palladium nano-particles, this nano particle is owing to have the defective of high-load, so have potential using value at aspects such as electro-catalysis, belong to the catalyst material field.
Background technology
Over past ten years, the form controlledly synthesis of palladium nano-particles has been caused 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 technology such as chemical synthesis all is applied to this, but the pattern of palladium nano-particles is confined to sphere, cube, tetrahedron, octahedron, line or bar structure or the like, the achievement of radiation structure does not seldom more also exist because the research of the higher internal energy that a large amount of defective causes in the radiation inside configuration.
The radiation structure because there is a large amount of crystal lattice boundaries in it, has a large amount of specific surface energies on the surface, and because relaxation and crystallization effect again, often this structure is difficult to keep the long period, so aspect practical application, especially catalysis aspect shorter mention.In this patent, the temperature of acetone comes into question as the key factor that forms the 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 the defective that forms high-load in the nano particle owing to crystallization is imperfect.The gathering of PVP has caused the accumulation of the nano particle of portion's parcel within it.Simultaneously, because nano grain surface has the iodobenzene of steric restriction effect, make that this sedimentation is more obvious.In research before, the iodo in the iodobenzene has been found can effectively combine with palladium nano-particles, thereby in this patent, iodobenzene also can be protected the defect sturcture that has formed in the accumulation that is used for promoting nano particle.
Summary of the invention
The invention provides a kind of method for preparing the method for palladium nanoparticle catalyst and widened the relevant nano particle of preparation.
The present invention innovates and uses iodobenzene as coating material, utilize its effectively ADSORPTION OF GOLD metal nano-particle, can utilize its phenyl that effective steric restriction effect is provided again, under the acting in conjunction of freezing reacting liquid temperature that acetone caused and the decline suddenly of PVP solubility, form comparatively stable, inner and palladium nano-particles that the surface all has the high-load defective.It is simple that this method has technology, easy to operate, and pattern is controlled, and characteristics such as applied range have potential using value.
The present invention adopts following technical scheme:
1. a method for preparing the Pd nanoparticle catalyst comprises that the preparation of catalyst carrier, product separate, the washing process process, it is characterized in that comprising following step:
(1) at first PVP and iodobenzene are dissolved in 100 ℃ the ethylene glycol solution;
(2) in reaction system, add K then 2PdCl 4The aqueous solution;
(3) after the reaction, reaction solution is poured in the preprepared-30 ℃ acetone while hot, centrifugation subsequently, the mixed solution washing precipitation of using ethanol/acetone again is for several times, be dissolved in the ethanol to remove remaining ethylene glycol and excessive PVP, will precipitate again again.
2. as preparing the method for Pd nanoparticle catalyst as described in the item 1, it is characterized in that with iodobenzene as coating material control its addition and be the coating agent PVP 250 times.
3. as preparing the method for Pd nanoparticle catalyst as described in the item 1, it is characterized in that the addition of metal is controlled to be 1/100 of iodobenzene addition.
4. as preparing the method for Pd nanoparticle catalyst as described in the item 1, it is characterized in that the solution of reaction after 3 hours is added in-30 ℃ of acetone while hot.
The preparation method of nanometer palladium beaded catalyst provided by the present invention has the following advantages:
(1) Zhi Bei metal nanoparticle is not easy to reunite, and monodispersity is fine.
(2) all there is the defective of high-load in the palladium nano-particles of preparation gained on inner and surface, and these defectives keep chronic, can utilize with actual production in.
(3) with the breakthrough utilization of the method iodobenzene as coating material, later relevant preparation of nanoparticles is had reference function.
The present invention can be applicable at aspects such as electro-catalysis.
Description of drawings
Fig. 1 superactivity palladium nano-particles prepares 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.
The specific embodiment
1. at first with a certain amount of 0.4g PVP, the 0.28mL iodobenzene is dissolved in 100 ℃ the 40mL ethylene glycol solution.
2. in reaction system, dropwise add 0.025M K then 2PdCl 4Aqueous solution 1mL.
3. after reacting 3 hours, reaction solution is poured in the preprepared-30 ℃ acetone while hot, centrifugation subsequently, the mixed solution washing precipitation of using ethanol/acetone again is for several times, be dissolved in the ethanol to remove remaining ethylene glycol and excessive PVP, will precipitate again again.

Claims (4)

1. a method for preparing the Pd nanoparticle catalyst comprises that the preparation of catalyst carrier, product separate, the washing process process, it is characterized in that comprising following step:
(1) at first PVP and iodobenzene are dissolved in 100 ℃ the ethylene glycol solution;
(2) in reaction system, add K then 2PdCl 4The aqueous solution;
(3) after the reaction, reaction solution is poured in the preprepared-30 ℃ acetone while hot, centrifugation subsequently, the mixed solution washing precipitation of using ethanol/acetone again is for several times, be dissolved in the ethanol to remove remaining ethylene glycol and excessive PVP, will precipitate again again.
2. the method for preparing the Pd nanoparticle catalyst according to claim 1 is characterized in that iodobenzene as coating material, control its addition and be the coating agent PVP 250 times.
3. the method for preparing the Pd nanoparticle catalyst according to claim 1 is characterized in that the addition of metal is controlled to be 1/100 of iodobenzene addition.
4. the method for preparing the Pd nanoparticle catalyst according to claim 1 is characterized in that the solution of reaction after 3 hours is added in-30 ℃ of acetone while hot.
CN201010136791.2A 2010-03-31 2010-03-31 Method for synthesizing nano palladium particles with superactivity Active CN102205252B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103909272A (en) * 2012-12-31 2014-07-09 浙江海洋学院 Preparation method for multi-foot-shaped platinum nano materials
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
WO2021088956A1 (en) * 2019-11-07 2021-05-14 南京师范大学 Ultra-fine pd tetrahedron nanomaterial, preparation method therefor and use thereof

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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

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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
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NELLY ZAKARINA 等: "Platinum Nanoparticles Stabilized by Polyvinylpyrrolidone for Hydrogenation", 《CHINESE JOURNAL OF CATALYSIS》, vol. 29, no. 11, 30 November 2008 (2008-11-30), pages 1165 - 1168, XP025861141, DOI: doi:10.1016/S1872-2067(09)60019-X *
王艳丽等: "不使用保护气氛和还原剂超声制备纳米钯颗粒", 《材料研究学报》, vol. 21, no. 3, 30 June 2007 (2007-06-30), pages 329 - 332 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103909272A (en) * 2012-12-31 2014-07-09 浙江海洋学院 Preparation method for multi-foot-shaped platinum nano materials
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
WO2021088956A1 (en) * 2019-11-07 2021-05-14 南京师范大学 Ultra-fine pd tetrahedron nanomaterial, preparation method therefor and use thereof

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