CN102847952B - Method for preparing polyhedral nano palladium material through ethanol reduction - Google Patents
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Abstract
The invention relates to a method for preparing a polyhedral nano palladium material through ethanol reduction, which is characterized in that the polyhedral nano palladium material is prepared through one-step synthesis at 65-80 DEG C by taking water as main solvent in normal-pressure environment and adding a small amount of ethanol as cosolvent and reducer through the use of a simple heating device; and the nano palladium material having polyhedral morphology is prepared through low-temperature synthesis by taking a surfactant-macromolecule composite system as a soft template. According to the invention, the method is a convenient and environment-friendly technology, and has the advantages of mild process conditions, no need of complicated equipment, simple operation process and no need of a toxic organic phase used as solvent or assistant; the prepared polyhedral nano palladium material is high in yield, the polyhedral morphology yield is 83-94%, the particle size is within the range of 10-35nm, and the size distribution is concentrated; and mass production can be realized. Thus, the invention has favorable application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of nano particle, being specifically related to one is soft template with surfactant-macromolecule complex, utilizes ethanol reduction to prepare the method for polyhedron Technique of Nano Pd material.
Background technology
Metal nanoparticle is different from the performances such as special electricity, magnetics, optics, calorifics and the mechanics of reguline metal owing to having, and is expected to be widely used in biology, medical science, information storage, chemistry, sensor field.The property that metal nanoparticle has is by the size of metal nanoparticle, shape, component, crystal formation and structures shape, and therefore synthetic shape is single, size is controlled, crystal formation and the clear and definite metal nanoparticle of structure are research and apply the vital first step of its character.Compared with the common polycrystalline ball-type nano particle synthesizing, there is polyhedron-shaped nano particle and often show unique character and application widely.But synthetic have polyhedron-shaped will be a kind of huge challenge with these controlled nano particles of size.Because from thermodynamic (al) angle, the growth of nano particle will be followed the principle of minimum energy principle and surface area minimum.So prepare the growing environment that the three-dimensional nano particle of complicated shape generally need to be more special.
In recent years, the shape control of metal nano palladium particle is synthesized under difficult prerequisite and is still made some progress.2005, Xia seminar delivered one section of synthetic about cube Pd nano particle on JACS, experiment be ethylene glycol solution in, spent glycol is reducing agent and solvent, chlorine palladium acid sodium (Na
2pdCl
4) do palladium salt precursor, polyvinylpyrrolidone (PVP) does dispersant and coating agent, inject chlorine palladium using ethylene glycol as solvent acid sodium and PVP solution in reaction bulb with certain speed with two pass injector simultaneously, in 110 DEG C of back flow reaction 9h synthesized the rescinded angle monocrystalline palladium nanocube that the length of side is 8 nm (
j. Am. Chem. Soc,2005,
127,7332-7333).2007, Berhault seminar utilized the crystal seed method first step using softex kw (CTAB) as surfactant, adopted NaBH
4for reducing agent, electronation Na
2pdCl
4obtain little Pd nano particle; Second step utilizes this Pd Nano sol to join by Na as crystal seed
2pdCl
4in the growth solution of the weak vitamin C composition of reproducibility, grow into the Pd nano particle of large-size; The synthetic Pd nano particle of the 3rd step recycling second step as crystal seed adding further synthetic larger sized Pd nano particle in growth solution.This method can be by changing Na
2pdCl
4with the Pd of the synthetic various shapes of the ratio of crystal seed nanocrystalline (
j. Phys. Chem. C, 2007,111:5915-5925).2008, the people such as Niu were first by the palladium bichloride (PdCl of 0.1773g
2) be dissolved in and in the HCl solution of 0.2mol/L of 10mL, be diluted to 100mL and prepare tetrachloro-palladium acid (H
2pdCl
4) solution, taking softex kw as surfactant, vitamin C is reducing agent, the tetrachloro-palladium acid that reduces under 95 DEG C of conditions obtain 22nm palladium cube (
crystal Growth & Design, 2008,8,4440-4444).Within 2011, Li is with palladium acetylacetonate (Pd (acac)
2) be Pd salt precursor, utilize Hydrothermal Synthesis technology, taking toluene as solvent, in reaction system, introduce oleyl amine, taking formaldehyde as reducing agent, control reaction temperature at 100 DEG C, can prepare by changing oleyl amine consumption the different-shapes such as icosahedron, decahedron, octahedron, tetrahedron and triangular plate nanometer Pd crystalline substance (
angew. Chem. Int. Ed, 2011,50:1-6).
These methods are all the in these years successful trials in Technique of Nano Pd preparation method, but still have the problem of several aspects below:
1, in prior art, preparing the document of Technique of Nano Pd, most to adopt tetrachloro-palladium acid, chlorine palladium acid sodium or palladium etc. be Metal Palladium salt precursor; Or make tetrachloro-palladium acid, chlorine palladium acid sodium by palladium bichloride, thereby improve the dissolubility of palladium salt, but palladium content reduces relatively; Or adopt to add and carry out dissolution of metals palladium salt poisonous organic phase solvents such as toluene, the numerous and diverse and contaminated environment of experimental procedure.
2, owing to introducing many chemical reagent such as chemical reducing agent, dispersion stabilizer, covering, even using poisonous organic phase or simple alcohols as solvent, product purification processing procedure is loaded down with trivial details, the consumption of larger additive not only experimental cost is higher, also may bring certain problem of environmental pollution.
3, add such as NaBH
4deng go back original reagent be difficult to control rate of reduction, thereby in pattern control, strengthen difficulty.
4, control nano shape and divide several steps to complete, complex steps, program complexity, even requiring has refluxing unit, and process conditions are harsher, are unfavorable for industrialized production.
In a word, be also difficult at present adopt simple and easy method one-step synthesis polyhedron Technique of Nano Pd material.
Summary of the invention
For solving problems of the prior art, the object of the present invention is to provide a kind of process conditions gentleness, without complex apparatus, simple to operate, not needing high temperature and poisonous organic phase is solvent or auxiliary agent, the Simple heating preparation method of one-step synthesis polyhedron Technique of Nano Pd material.
The technical scheme that the present invention takes for realizing its object: a kind of method of utilizing ethanol reduction to prepare polyhedron Technique of Nano Pd material, comprise and utilize ethanol for reducing agent, by palladium bichloride (hereinafter referred to as PdCl
2) be reduced to Metal Palladium (hereinafter referred to as Pd) nano particle, it is characterized in that: first configure ethanol water; Then by PdCl
2powder and surfactant-macromolecule complex system is added in ethanolic solution and is configured to reaction system, and logical protection gas also adds thermal agitation, makes palladium cation generation reduction reaction obtain Pd nano particle; Centrifugation obtains black precipitate after completion of the reaction, uses ethanol, acetone washing final vacuum to be dried, and obtains polyhedron Technique of Nano Pd.
Water in described ethanol water and the volume ratio of ethanol are 3 ~ 9:1.
Contained PdCl in described mixed system
2concentration is 7.04 × 10
-4~ 2.11 × 10
-3mol/L.
Described surfactant-macromolecule complex is lauryl sodium sulfate (hereinafter referred to as SDS)-polyvinylpyrrolidone (hereinafter referred to as PVP) compound system or softex kw (hereinafter referred to as CTAB)-polyvinylpyrrolidone (hereinafter referred to as PVP) compound system; In described reaction system, the concentration range of contained lauryl sodium sulfate is 2.5 × 10
-3~ 2.5 × 10
-2mol/L, polyvinylpyrrolidone concentration is 2.5 × 10
-4mol/L, the concentration range of softex kw is 2.5 × 10
-3~ 2.5 × 10
-2mol/L; Described protection gas is nitrogen (N
2) or argon gas (Ar).The described temperature that adds thermal agitation is 65-80 DEG C, and the reaction time is 2.5-4h; Described baking temperature is 25-40 DEG C, and be 24-48h drying time.
The present invention is taking water as main body solvent, add a small amount of ethanol as cosolvent and reducing agent, be soft template with surfactant-macromolecule complex, the synthetic polyhedron pattern Technique of Nano Pd material of low temperature is the technology of a kind of convenience and comparison environmental protection, aspect practical, has great importance.
Beneficial effect of the present invention:
The present invention adopts Simple heater, in atmospheric pressure environment taking water as main body solvent, add a small amount of ethanol as cosolvent and reducing agent, at next step synthetic polyhedron Technique of Nano Pd material of 65-80 DEG C of temperature conditions, be soft template with surfactant-macromolecule complex, the synthetic polyhedron pattern Technique of Nano Pd material of low temperature is the technology of a kind of convenience and comparison environmental protection, process conditions gentleness, without complex apparatus, simple to operate, not needing high temperature and poisonous organic phase is solvent or auxiliary agent, the polyhedron Technique of Nano Pd material productive rate making is high, polyhedron pattern productive rate is 83 ~ 94%, and particle size range is between 10 ~ 35nm, distribution of sizes is concentrated, can produce in a large number, there is good application prospect.
Brief description of the drawings
Fig. 1 is polyhedron Technique of Nano Pd material transmission electron microscope figure prepared by the present invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, SDS and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, SDS and PVP concentration is respectively 7.04 × 10
-4mol/L, 1.25 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 5min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 3h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 24h, obtain polyhedron Technique of Nano Pd material;
(5) transmission electron microscope photo (TEM) is obtained by company of Jeol Ltd. JEOL-2010 type transmission electron microscope; The microscopic appearance of Technique of Nano Pd material as shown in drawings, most particles are polyhedron pattern, in figure, the illustration in the upper right corner is the high power photo of the nano particle of solid circles mark in figure, polyhedron pattern is high-visible, particle size is 18nm left and right, particle diameter distributes more concentrated, and according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 94%.
Embodiment 2:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, SDS and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, SDS and PVP concentration is respectively 7.04 × 10
-4mol/L, 2.5 × 10
-3mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 10min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 3h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 25 DEG C of vacuum drying 48h, obtain polyhedron Technique of Nano Pd material, particle size is 32nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 93%.
Embodiment 3:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, SDS and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, SDS and PVP concentration is respectively 7.04 × 10
-4mol/L, 2.5 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 10min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 3h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 24h, obtain polyhedron Technique of Nano Pd material, particle size is 25nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 91%.
Embodiment 4:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 9:1;
(2) add successively PdCl
2, SDS and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, SDS and PVP concentration is respectively 7.04 × 10
-4mol/L, 1.25 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 5min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 3.5h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 30 DEG C of vacuum drying 40h, obtain polyhedron Technique of Nano Pd material, particle size is 15nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 88%.
Embodiment 5:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 3:1;
(2) add successively PdCl
2, SDS and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, SDS and PVP concentration is respectively 7.04 × 10
-4mol/L, 1.25 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 5min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 2.5h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 35 DEG C of vacuum drying 35h, obtain polyhedron Technique of Nano Pd material, particle size is 27nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 90%.
Embodiment 6:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, CTAB and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, CTAB and PVP concentration is respectively 7.04 × 10
-4mol/L, 1.25 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 10min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 3.5h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 24h, obtain polyhedron Technique of Nano Pd material, particle size is 10nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 86%.
Embodiment 7:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, CTAB and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, CTAB and PVP concentration is respectively 7.04 × 10
-4mol/L, 2.5 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 5min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use argon shield, control 70 DEG C of reaction temperatures, reaction 3.5h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 24h, obtain polyhedron Technique of Nano Pd material, particle size is 12nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 88%.
Embodiment 8:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, CTAB and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, CTAB and PVP concentration is respectively 7.04 × 10
-4mol/L, 2.5 × 10
-3mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 10min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 70 DEG C of reaction temperatures, and reaction 3.5h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 24h, obtain polyhedron Technique of Nano Pd material, particle size is 35nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 83%.
Embodiment 9:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, CTAB and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, CTAB and PVP concentration is respectively 1.41 × 10
-3mol/L, 1.25 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 10min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 80 DEG C of reaction temperatures, and reaction 2.5h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 36h, obtain polyhedron Technique of Nano Pd material, particle size is 13nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 90%.
Embodiment 10:
(1) the water-ethanol mixed solvent system that the volume ratio of configuration water and ethanol is 5:1;
(2) add successively PdCl
2, CTAB and PVP powder in water-ethanol mixed solution system, be configured to reaction system, wherein contained PdCl
2, CTAB and PVP concentration is respectively 2.11 × 10
-3mol/L, 1.25 × 10
-2mol/L and 2.5 × 10
-4mol/L, is placed on constant temperature blender with magnetic force in 25 DEG C of stirring 10min by the solution preparing, and solution colour is light yellow;
(3) reaction solution after stirring is placed in and on magnetic stirring apparatus, stirs and heat, use N
2protection, controls 65 DEG C of reaction temperatures, and reaction 4h, obtains black suspension, stops reaction;
(4) black precipitate obtaining in centrifugation reaction solution, and with ethanol and acetone centrifuge washing, 40 DEG C of vacuum drying 48h, obtain polyhedron Technique of Nano Pd material, particle size is 15nm left and right, and particle diameter distributes more concentrated, according to TEM photo statistics, polyhedron Technique of Nano Pd pattern productive rate is 89%.
Claims (2)
1. utilize ethanol reduction to prepare a method for polyhedron Technique of Nano Pd material, it is characterized in that: utilize ethanol for reducing agent, by palladium bichloride (PdCl
2) being reduced to Metal Palladium (Pd) nano particle, its preparation process is:
(1) configuration ethanol water, the water in described ethanol water and the volume ratio of ethanol are 3 ~ 9:1;
(2) by palladium bichloride (PdCl
2) powder and surfactant-macromolecule complex system is added to and in ethanolic solution, is configured to reaction system; logical protection gas also adds thermal agitation; the described temperature that adds thermal agitation is 65-80 DEG C; reaction time is 2.5-4h; described surfactant-macromolecule complex is lauryl sodium sulfate (SDS)-polyvinylpyrrolidone (PVP) compound system or softex kw (CTAB)-polyvinylpyrrolidone (PVP) compound system, contained palladium bichloride (PdCl in described reaction system
2) concentration range is 7.04 × 10
-4~ 2.11 × 10
-3mol/L, in described reaction system, the concentration range of contained lauryl sodium sulfate (SDS) is 2.5 × 10
-3~ 2.5 × 10
-2mol/L, the concentration of polyvinylpyrrolidone (PVP) is 2.5 × 10
-4mol/L, the concentration range of softex kw (CTAB) is 2.5 × 10
-3~ 2.5 × 10
-2mol/L;
(3) centrifugation obtains black precipitate after completion of the reaction, uses ethanol, acetone to wash rear dry;
(4) vacuum drying obtains polyhedron Technique of Nano Pd; Baking temperature is 25-40 DEG C, and be 24-48h drying time.
2. the method for utilizing ethanol reduction to prepare polyhedron Technique of Nano Pd material according to claim 1, is characterized in that: in described step (2), protection gas is nitrogen (N
2) or argon gas (Ar).
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| CN103203461B (en) * | 2013-03-21 | 2015-07-22 | 燕山大学 | Method for preparing hammer-shaped palladium nanoparticle by utilizing octreotide acetate as template |
| KR101736014B1 (en) * | 2013-12-03 | 2017-05-29 | 다나카 기킨조쿠 고교 가부시키가이샤 | Method for collecting palladium |
| CN103934470B (en) * | 2014-04-04 | 2016-01-20 | 中南大学 | A kind of preparation method of Marks decahedron Pd nano particle |
| CN104722775B (en) * | 2015-03-11 | 2016-09-07 | 浙江大学 | A kind of two dimension hollow palladium nano-crystal and preparation method thereof |
| CN106744837A (en) * | 2016-12-02 | 2017-05-31 | 陕西科技大学 | A kind of method of palladium chtalyst argon hydrogen mixture redox graphene |
| CN108031858A (en) * | 2017-11-28 | 2018-05-15 | 苏州大学 | A kind of controllable octahedral preparation method of palladium nano cubic of surface topography |
| CN108057899B (en) * | 2017-12-07 | 2020-07-21 | 深圳大学 | C, N-doped AgPd nanowire and preparation method thereof |
| CN115137825B (en) * | 2022-07-03 | 2023-07-14 | 重庆医科大学 | Manganese-doped calcium phosphide-modified metal palladium nanoparticle and preparation method thereof |
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| 王艳丽.纳米钯粒子及其复合聚合物的超声原位制备与表征.《中国优秀硕士学位论文全文数据库（电子期刊）》.2008,(第7期),B014-20. * |
| 王艳丽等.超声诱导CTAB/SDS溶液中纳米Pd粒子的形貌控制及对甲醛的电催化氧化.《材料工程》.2012,(第4期), * |
| 超声诱导CTAB/SDS溶液中纳米Pd粒子的形貌控制及对甲醛的电催化氧化;王艳丽等;《材料工程》;20120420(第4期);第57页第1.2.1节 * |
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