CN100488675C - Nanometer Pd material and its preparation process - Google Patents
Nanometer Pd material and its preparation process Download PDFInfo
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- CN100488675C CN100488675C CNB2007100554163A CN200710055416A CN100488675C CN 100488675 C CN100488675 C CN 100488675C CN B2007100554163 A CNB2007100554163 A CN B2007100554163A CN 200710055416 A CN200710055416 A CN 200710055416A CN 100488675 C CN100488675 C CN 100488675C
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Abstract
The present invention provides one kind of cuboidal nanometer Pd material and its preparation process. The preparation process includes the following steps: mixing 10 mM concentration water solution of chloropalladic acid and 12.5-25 mM concentration water solution of ammonium hexadecyl trimethyl bride in the volume ratio of 1 to 20, heating to 65-95 deg.c, adding 100 mM concentration water solution of ascorbic acid in the volume ratio to the water solution of chloropalladic acid of 0.16 to 1 to react for 30 min, centrifugal separation to collect precipitate, water washing, and drying to obtain cuboidal nanometer Pd material. The process is simple, and the prepared cuboidal nanometer Pd material is used in catalyzing, preparing nanometer material and other fields.
Description
Technical field
The present invention relates to technical field of nano material.
Background technology
Metal nano material has the character of many uniquenesses and causes people's extensive concern.And their character and its shape and size are closely bound up.Therefore produced the preparation method of nano material of the method for the metal nano material of many preparation specific dimensions and shape, particularly gold and silver.Palladium is a kind of important catalyst, has participated in many important catalytic reactions.Therefore, the preparation method of nanometer Pd material causes people's attention day by day in recent years.Prepared the nanometer Pd material of many different structures, reported that the 4817th page of the 19th volume of Langmuir the employing hydrazine reduces potassium chloropalladate and prepares palladium nanometer octahedron in the presence of TTAB as Veisz etc. 2003; Xiong etc. 2005 have reported that the 1237th page of the 5th volume of Nano.Lett. there is under the situation reduction palladium bichloride in employing ethylene glycol and reduces nano particle quantity with the iron chloride oxidation at polyvinylpyrrolidone, thereby prepare the palladium nanocube of large-size; They had reported that the employing citric acid existed under the situation reduction chlorine palladium acid sodium can prepare palladium nanometer icosahedron at polyvinylpyrrolidone for the 790th page at the 46th volume of Angew.Chem.Int.Ed. in 2007.Yet at present also not about the synthetic report of palladium nanometer cuboid.
Summary of the invention
The purpose of this invention is to provide a kind of nanometer Pd material and preparation method thereof.
A kind of nanometer Pd material provided by the invention is characterized in that, it is a palladium nanometer cuboid.
A kind of palladium nanometer cuboid preparation methods of the present invention, step and condition method are as follows:
Is volume ratio 10mM chlorine palladium aqueous acid and the 12.5-25mM softex kw aqueous solution of 1:20, be heated to 65-95 ℃, adding is the 100mM aqueous ascorbic acid of 0.16:1 with the volume ratio of 10mM chlorine palladium aqueous acid then, reacted 30 minutes, solution centrifugal is separated, the precipitation of collecting washes with water, and drying obtains palladium nanometer cuboid.
Palladium nanometer cuboid preparation method of the present invention is simple, and prepared palladium nanometer cuboid is expected to be used for fields such as catalysis and nano material preparation.
Description of drawings
The sem photograph of the cuboid of palladium nanometer described in Fig. 1: the embodiment 1.
The sem photograph of the cuboid of palladium nanometer described in Fig. 2: the embodiment 2.
The sem photograph of the cuboid of palladium nanometer described in Fig. 3: the embodiment 3.
The sem photograph of the cuboid of palladium nanometer described in Fig. 4: the embodiment 4.
The specific embodiment
By following examples to inventing further elaboration.
Embodiment 1
12.5mM softex kw aqueous solution with the 10mM chlorine palladium aqueous acid and 20 volumes of 1 volume, be heated to 95 ℃, adding is the 100mM aqueous ascorbic acid of 0.16:1 with the volume ratio of 10mM chlorine palladium aqueous acid then, react after 30 minutes, solution centrifugal is separated, the precipitation of collecting washes with water, and drying obtains palladium nanometer cuboid material.
Embodiment 2
15mM softex kw aqueous solution with the 10mM chlorine palladium aqueous acid and 20 volumes of 1 volume, be heated to 65 ℃, adding is the 100mM aqueous ascorbic acid of 0.16:1 with the volume ratio of 10mM chlorine palladium aqueous acid then, react after 30 minutes, solution centrifugal is separated, the precipitation of collecting washes with water, and drying obtains palladium nanometer cuboid.
Embodiment 3
25mM softex kw aqueous solution with the 10mM chlorine palladium aqueous acid and 20 volumes of 1 volume, be heated to 95 ℃, adding is the 100mMM aqueous ascorbic acid of 0.16:1 with the volume ratio of 10mM chlorine palladium aqueous acid then, react after 30 minutes, solution centrifugal is separated, the precipitation of collecting washes with water, and drying obtains palladium nanometer cuboid material.
Embodiment 4
25mM softex kw aqueous solution with the 10mM chlorine palladium aqueous acid and 20 volumes of 1 volume, be heated to 85 ℃, adding is the 100mM aqueous ascorbic acid of 0.16:1 with the volume ratio of 10mM chlorine palladium aqueous acid then, react after 30 minutes, solution centrifugal is separated, the precipitation of collecting washes with water, and drying obtains palladium nanometer cuboid material.
Claims (2)
1, a kind of nanometer Pd material is characterized in that, it is a palladium nanometer cuboid.
2, a kind of palladium nanometer cuboid preparation methods as claimed in claim 1, step and condition are as follows:
Is volume ratio 10mM chlorine palladium aqueous acid and the 12.5-25mM softex kw aqueous solution of 1:20, be heated to 65-95 ℃, adding is the 100mM aqueous ascorbic acid of 0.16:1 with the volume ratio of 10mM chlorine palladium aqueous acid then, reacted 30 minutes, solution centrifugal is separated, the precipitation of collecting washes with water, and drying obtains palladium nanometer cuboid material.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100554163A CN100488675C (en) | 2007-03-16 | 2007-03-16 | Nanometer Pd material and its preparation process |
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| CNB2007100554163A CN100488675C (en) | 2007-03-16 | 2007-03-16 | Nanometer Pd material and its preparation process |
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| CN101020243A CN101020243A (en) | 2007-08-22 |
| CN100488675C true CN100488675C (en) | 2009-05-20 |
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| CNB2007100554163A Expired - Fee Related CN100488675C (en) | 2007-03-16 | 2007-03-16 | Nanometer Pd material and its preparation process |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775638A (en) * | 2010-03-24 | 2010-07-14 | 中国科学院长春应用化学研究所 | Preparation method of palladium nano crystal |
| CN102172776A (en) * | 2011-01-25 | 2011-09-07 | 西安凯立化工有限公司 | Method for preparing metal palladium powder |
| CN102744416B (en) * | 2011-04-19 | 2013-12-25 | 同济大学 | Preparation method of icosahedron crystalline nano nickel-cobalt alloy |
| CN102699347B (en) * | 2012-06-25 | 2014-04-30 | 安徽理工大学 | Method for preparing palladium nanometer sheet with optical property |
| CN102794172B (en) * | 2012-07-26 | 2014-09-17 | 安徽理工大学 | Photosynthesis preparation method of nano palladium catalyst |
| CN102847952B (en) * | 2012-10-22 | 2014-11-05 | 安徽理工大学 | Method for preparing polyhedral nano palladium material through ethanol reduction |
| CN104209530B (en) * | 2013-05-30 | 2016-05-04 | 国家纳米科学中心 | A kind of PdPt core-shell nano material and preparation method thereof |
| CN104841948B (en) * | 2015-05-15 | 2016-10-05 | 燕山大学 | A kind of method preparing starlike Pd nano particle for template with lanreotide acetate |
| CN106732556B (en) * | 2016-11-25 | 2019-11-26 | 安徽师范大学 | A kind of porous platinum/palldium alloy nanoparticle catalyst, preparation method and applications |
| CN108031834B (en) * | 2017-12-15 | 2019-07-05 | 复旦大学 | The in-situ synthetic method of different-shape chiral zinc porphyrin nanometer Pd material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020194958A1 (en) * | 2001-06-08 | 2002-12-26 | Chien-Liang Lee | Process for preparing noble metal nanoparticles |
| CN1485171A (en) * | 2002-09-24 | 2004-03-31 | 中国科学技术大学 | Granular nanometer amorphous metal Pd and the preparation thereof |
| EP1627699A1 (en) * | 2004-08-16 | 2006-02-22 | Dowa Mining Co., Ltd. | Face-centered cubic structure alloy particles and method of manufacturing |
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2007
- 2007-03-16 CN CNB2007100554163A patent/CN100488675C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020194958A1 (en) * | 2001-06-08 | 2002-12-26 | Chien-Liang Lee | Process for preparing noble metal nanoparticles |
| CN1485171A (en) * | 2002-09-24 | 2004-03-31 | 中国科学技术大学 | Granular nanometer amorphous metal Pd and the preparation thereof |
| EP1627699A1 (en) * | 2004-08-16 | 2006-02-22 | Dowa Mining Co., Ltd. | Face-centered cubic structure alloy particles and method of manufacturing |
Non-Patent Citations (1)
| Title |
|---|
| 溶剂稳定的钯金属纳米颗粒的制备. 何武强，何宝林，陈益贤，廖小娟，刘汉范.中南民族大学学报（自然科学版），第23卷第4期. 2004 * |
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Owner name: CHANGZHOU INSTITUTE OF ENERGY STORAGE MATERIALS + Free format text: FORMER OWNER: CHANGCHUN INSTITUTE OF APPLIED CHEMISTRY HINESE ACADEMY OF SCIENCES Effective date: 20121231 |
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Effective date of registration: 20121231 Address after: Changzhou City, Jiangsu province Hehai road 213000 No. 9 Patentee after: Changzhou Institute of Energy Storage Materials & Devices Address before: 130022 Changchun people's street, Jilin, No. 5625 Patentee before: Changchun Institue of Applied Chemistry, Chinese Academy of Sciences |
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