CN105148936A - Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles - Google Patents
Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles Download PDFInfo
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Abstract
The invention relates to a method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles. The method comprises the following steps: (1) respectively dissolving 0.1-1.0 part (by mass) of CTAB (Cetyl Trimethyl Ammonium Bromide) and 1-5 parts (by mass) of glucose in 1-10 parts (by mass) of pure water and 10-50 parts (by mass) of pure water, so as to prepare a CTAB solution and a glucose solution; (2) respectively weighing 0.1-1 part (by mass) of the glucose solution prepared in the step (1) and 0.03-1 part (by mass) of the CTAB solution prepared in the step (1), adding the weighed glucose solution and the weighed CTAB solution into a beaker, and carrying out stirring, so as to form a uniform mixed solution; (3) adding 0.5-5.0 parts (by mass) of sodium tetrachloropalladate and 0.01-0.5 part (by mass) of ferric chloride into the mixed solution formed in the step (2), carrying out stirring until the solution is mixed uniformly, putting the mixture in a reaction kettle for hydrothermal reaction, heating the mixture to the temperature of 100-200 DEG C, and carrying out reaction for 0.5-5 hours; and (4) after the reaction ends, naturally cooling the reactant to room temperature, finally, pouring the reactant into a clean centrifuge tube, carrying out centrifuge washing for several times with anhydrous ethanol and ultrapure water, and baking obtained precipitates at the temperature of 25-80 DEG C, thereby obtaining a black powdered product. The product prepared by the method is regular in morphology, uniform in size, good in dispersity, high in electrocatalytic oxidation capacity, simple in preparation process and easy in condition control, so that scale production is facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of palladium Fe nanometer particles, especially a kind of preparation method of straight-chain arrangement cube palladium Fe nanometer particles.
Technical background
Noble metal nano particles has the ins and outs such as catalysis, plasma resonance, spectroscopy due to it and becomes in inorganic nano material studies one of system the most widely.Along with nano material technology development and renewal, research pattern (size, shape etc.) controlled nano material is subject to people and pays close attention to widely.At present, large area, accurately control synthesis noble metal nanometer material, remain focus and the difficult point of current nano materials research.As everyone knows, hydrothermal reduction method is utilized to be a kind of typical Nobel-metal catalyst preparation method by noble metal such as Pd, Au.
Summary of the invention
For overcoming above-mentioned the deficiencies in the prior art, a kind of straight-chain is the object of the present invention is to provide to arrange the preparation method of cube palladium Fe nanometer particles, utilize surfactant softex kw (CTAB), the week reduction of glucose and Morphological control effect, under the synergy of CTAB and glucose, prepare have catenation, compound with regular structure, size uniformity, there is good crystallinity and (100) crystal face expose cube nanometer Pd material, improve the various performances of precious metal material, particularly greatly improve its catalytic performance.
For achieving the above object, present invention employs following technical scheme:
A preparation method for straight-chain arrangement cube palladium Fe nanometer particles, it comprises the steps:
1) by mass fraction, 0.1 ~ 1.0 part of CTAB and 1 ~ 5 part glucose is dissolved in 1-10 part and 10-50 part pure water respectively, is made into CTAB solution and glucose solution.
2) by mass fraction, the CTAB solution of the glucose solution and 0.03-1 part step 1) gained of getting 0.1-1 part step 1) gained respectively adds jar agitation, forms uniform mixed solution.
3) by mass fraction, by 0.5-5.0 part tetrachloro-palladium acid sodium (Na
2pdCl
4) and 0.01-0.5 part iron chloride (FeCl
3) join step 2) and mixed solution in, stir until solution mixes, put into reactor and carry out hydro-thermal reaction, be warming up to 100 ~ 200 DEG C reaction 0.5 ~ 5 hour.
4), after reaction terminates, room temperature is naturally cooled to.Finally by the centrifuge tube of reactant impouring cleaning, with absolute ethyl alcohol and ultra-pure water centrifuge washing several, gained is deposited in 25-80 DEG C of oven dry and obtains black powder product.
The invention has the beneficial effects as follows:
1) the cube palladium ferrum nano material of the regular arrangement of one dimension straight-chain that what the present invention prepared have, regular appearance, size uniformity, and favorable dispersibility.
2) product that prepared by the present invention has higher catalytic oxidation ability.
3) product preparation process of the present invention is simple, and condition is easy to control, and is convenient to large-scale production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of straight-chain of the present invention arrangement cube palladium Fe nanometer particles.
Detailed description of the invention
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The present invention, by the standby cube palladium Fe nanometer particles going out to have catenation of simple hydrothermal reduction legal system, improves electrocatalytic oxidation property.As shown in Figure 1.
A preparation method for straight-chain arrangement cube palladium Fe nanometer particles, it comprises the steps:
1) by mass fraction, 0.1 ~ 1.0 part of CTAB and 1 ~ 5 part glucose is dissolved in 1-10 part and 10-50 part pure water respectively, is made into CTAB solution and glucose solution.
2) by mass fraction, the CTAB solution of the glucose solution and 0.03-1 part step 1) gained of getting 0.1-1 part step 1) gained respectively adds jar agitation, forms uniform mixed solution.
3) by mass fraction, by 0.5-5.0 part tetrachloro-palladium acid sodium (Na
2pdCl
4) and 0.01-0.5 part iron chloride (FeCl
3) join step 2) and mixed solution in, stir until solution mixes, put into reactor and carry out hydro-thermal reaction, be warming up to 100 ~ 200 DEG C reaction 0.5 ~ 5 hour.
4), after reaction terminates, room temperature is naturally cooled to.Finally by the centrifuge tube of reactant impouring cleaning, with absolute ethyl alcohol and ultra-pure water centrifuge washing several, gained is deposited in 25-80 DEG C of oven dry and obtains black powder product.
Embodiment 1:
A preparation method for straight-chain arrangement cube palladium Fe nanometer particles, it comprises the steps:
1) by mass fraction, 0.1 part of CTAB and 1 part glucose is dissolved in 1 part and 10 parts of pure water respectively, is made into CTAB solution and glucose solution.
2) by mass fraction, the CTAB solution of the glucose solution and 0.03 part of step 1) gained of getting 0.1 part of step 1) gained respectively adds jar agitation, forms uniform mixed solution.
3) by mass fraction, by 0.5 part of tetrachloro-palladium acid sodium (Na
2pdCl
4) and 0.01 part of iron chloride (FeCl
3) join step 2) and mixed solution in, stir until solution mixes, put into reactor and carry out hydro-thermal reaction, be warming up to 100 DEG C reaction 0.5 hour.
4), after reaction terminates, room temperature is naturally cooled to.Finally by the centrifuge tube of reactant impouring cleaning, with absolute ethyl alcohol and ultra-pure water centrifuge washing several, gained is deposited in 25 DEG C of oven dry and obtains black powder product.
Embodiment 2:
A preparation method for straight-chain arrangement cube palladium Fe nanometer particles, it comprises the steps:
1) by mass fraction, 0.5 part of CTAB and 3 part glucose is dissolved in 5 parts and 30 parts of pure water respectively, is made into CTAB solution and glucose solution.
2) by mass fraction, the CTAB solution of the glucose solution and 0.5 part of step 1) gained of getting 0.5 part of step 1) gained respectively adds jar agitation, forms uniform mixed solution.
3) by mass fraction, by 3 parts of tetrachloro-palladium acid sodium (Na
2pdCl
4) and 0.3 part of iron chloride (FeCl
3) join step 2) and mixed solution in, stir until solution mixes, put into reactor and carry out hydro-thermal reaction, be warming up to 150 DEG C reaction 3 hours.
4), after reaction terminates, room temperature is naturally cooled to.Finally by the centrifuge tube of reactant impouring cleaning, with absolute ethyl alcohol and ultra-pure water centrifuge washing several, gained is deposited in 50 DEG C of oven dry and obtains black powder product.
Embodiment 3:
A preparation method for straight-chain arrangement cube palladium Fe nanometer particles, it comprises the steps:
1) by mass fraction, 1.0 parts of CTAB and 5 part glucose are dissolved in 10 parts and 50 parts of pure water respectively, are made into CTAB solution and glucose solution.
2) by mass fraction, the CTAB solution of the glucose solution and 1 part of step 1) gained of getting 1 part of step 1) gained respectively adds jar agitation, forms uniform mixed solution.
3) by mass fraction, by 5.0 parts of tetrachloro-palladium acid sodium (Na
2pdCl
4) and 0.5 part of iron chloride (FeCl
3) join step 2) and mixed solution in, stir until solution mixes, put into reactor and carry out hydro-thermal reaction, be warming up to 200 DEG C reaction 5 hours.
4), after reaction terminates, room temperature is naturally cooled to.Finally by the centrifuge tube of reactant impouring cleaning, with absolute ethyl alcohol and ultra-pure water centrifuge washing several, gained is deposited in 80 DEG C of oven dry and obtains black powder product.
Claims (1)
1. a preparation method for straight-chain arrangement cube palladium Fe nanometer particles, is characterized in that it comprises the steps:
1) by mass fraction, 0.1 ~ 1.0 part of CTAB and 1 ~ 5 part glucose is dissolved in 1-10 part and 10-50 part pure water respectively, is made into CTAB solution and glucose solution;
2) by mass fraction, the CTAB solution of the glucose solution and 0.03-1 part step 1) gained of getting 0.1-1 part step 1) gained respectively adds jar agitation, forms uniform mixed solution;
3) by mass fraction, by 0.5-5.0 part tetrachloro-palladium acid sodium (Na
2pdCl
4) and 0.01-0.5 part iron chloride (FeCl
3) join step 2) and mixed solution in, stir until solution mixes, put into reactor and carry out hydro-thermal reaction, be warming up to 100 ~ 200 DEG C reaction 0.5 ~ 5 hour;
4), after reaction terminates, room temperature is naturally cooled to;
5) finally by the centrifuge tube of reactant impouring cleaning, with absolute ethyl alcohol and ultra-pure water centrifuge washing several, gained is deposited in 25-80 DEG C of oven dry and obtains black powder product.
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| CN201510449935.2A CN105148936B (en) | 2015-07-29 | 2015-07-29 | Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles |
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| CN201510449935.2A CN105148936B (en) | 2015-07-29 | 2015-07-29 | Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989450A (en) * | 2012-12-03 | 2013-03-27 | 中国科学院大连化学物理研究所 | Preparation method, structural feature and application of carrying type nanometer electrocatalyst |
| US20140235428A1 (en) * | 2011-07-21 | 2014-08-21 | Nanjing University | Supported bimetallic nanocomposite catalyst and the preparation method thereof |
| CN104174392A (en) * | 2013-05-27 | 2014-12-03 | 中国科学院大连化学物理研究所 | One-step preparation method and application of supported platinum-based multi-metal catalysts |
-
2015
- 2015-07-29 CN CN201510449935.2A patent/CN105148936B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140235428A1 (en) * | 2011-07-21 | 2014-08-21 | Nanjing University | Supported bimetallic nanocomposite catalyst and the preparation method thereof |
| CN102989450A (en) * | 2012-12-03 | 2013-03-27 | 中国科学院大连化学物理研究所 | Preparation method, structural feature and application of carrying type nanometer electrocatalyst |
| CN104174392A (en) * | 2013-05-27 | 2014-12-03 | 中国科学院大连化学物理研究所 | One-step preparation method and application of supported platinum-based multi-metal catalysts |
Non-Patent Citations (3)
| Title |
|---|
| QIANG YUAN ET AL.: "Pd-Pt random alloy nanocubes with tunable compositions and their enhanced electrocatalytic activities", 《CHEM.COMMUN.》 * |
| SHUIFEN XIE ET AL.: "Atomic Layer-by-layer deposition of Pt on Pd nanocubes for catalysts with enhanced activity and durability toward oxygen reduction", 《NANO LETTERS》 * |
| XIANGYU WANG ET AL.: "Modification of Pd-Fe nanoparticles for catalytic dechlorination of 2,4-dichlorophenol", 《SCIENCE OF THE TOTAL ENVIRONMENT》 * |
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