CN107498066A - A kind of preparation method and applications of platinoid nano-material - Google Patents
A kind of preparation method and applications of platinoid nano-material Download PDFInfo
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- CN107498066A CN107498066A CN201710801814.9A CN201710801814A CN107498066A CN 107498066 A CN107498066 A CN 107498066A CN 201710801814 A CN201710801814 A CN 201710801814A CN 107498066 A CN107498066 A CN 107498066A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The present invention relates to a kind of preparation method and applications of platinoid nano-material.It is an object of the invention to provide a kind of method for using Liquid displacement methods to prepare using copper nano-wire as template platinoid nano wire, it is characterized in utilizing the activity difference between metallic copper and noble metal platinum, displacement reaction occurs with copper nano-wire and platinum acid chloride solution and obtains platinoid nano wire, with technical process is succinct, reaction condition is gentle, the reaction time is shorter, cost is low, product regular appearance, catalytic activity are high, recycles and reuses the advantages of rate is high, it is with a wide range of applications.During its application, using sodium borohydride as reducing agent, the catalytic performance of the Congo red solution of composite catalytic degradation is investigated；And investigate its recycling effect by reclaiming catalyst recycling.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, is related to and prepares monodimension nanometer material with liquid phase transformation approach, specifically
It is a kind of platinoid nano-material preparation method and applications.
Background technology
In recent years, nano metal material is due to its unique optical property, electric property and catalytic activity, in each neck
Domain is all widely used, and causes extensive concern.Wherein the nano-particle such as Au, Ag, Pt have excellent catalytic performance,
The characteristics such as good chemical stability, cause scientific circles and greatly pay close attention to.The catalytic performance of Au, Ag, Pt nano-particle and its
Size is closely related, and high dispersive, the nano-particle of small size have big specific surface area, shows more excellent catalysis and lives
Property.However, serious stability problem can be caused by the small caused bigger serface of size, such as it is easy to reunion, pattern change
Change, the breaking-up in catalytic process to surface and reduction of initial catalyst performance etc..Therefore, these nano-particles are being utilized
When a very important factor be how to stablize them so that they avoid reuniting.Furthermore, it is contemplated that Precious Metals Resources has
It is sex-limited and production cost high, usage amount is reduced in use and raising cycle efficieny is very important.Introduce cheap
Metal be a kind of effectively save Catalyst Production cost to core part and save the method for precious metal resource to prepare
The effective catalyst that catalytic activity is high, stable performance can be reused.
It is that the market price is relatively inexpensive compared to other metals, the advantages of metallic copper, there is good heat, electrical conductivity,
Chemical property is relatively stable.Copper nanometer has specific surface area is big, reactivity is high, selectivity is strong etc. as novel nano-material
Advantage.It can be used as catalyst be because nano-particles size it is small, the percentage shared by surface atom is big, the key state on surface and
Electronic state is different from inside particle, and surface atom, which is coordinated the not congruent active position for causing surface, to be increased, and this makes it possess work
For the primary condition of catalyst, and the group or valence link that are formed between nano-material surface and institute's immunoabsorbent substrate can accelerate electronics
Transfer, therefore there is catalytic performance.Meanwhile for the configuration of surface of nano-particle, as the reduction of particle diameter, surface are smooth
Degree reduces, and scraggly atomic stepses is formd, this adds increased the contact surface of chemical reaction, so as to improve catalyst
Effective rate of utilization.
1-dimention nano wire material, due to its particular geometric pattern, has such as superelevation for nano-powder material
The excellent properties such as mechanical strength, thermoelectricity capability, luminous efficiency, catalytic performance, magnetic property, absorbing property, to it in environmental improvement
The application study in field, especially it is an important field in nanoscale science and technology in dye wastewater treatment field.Made at present
Based on noble metal, its active component most noble metal in the surface of nano particle, core can be wasted catalyst
Fall.In order to save the expensive catalysis effect for obtaining metals resources and saving precious metal catalyst production cost, while improving catalyst
Rate and raising dye wastewater treatment efficiency simultaneously save treatment cost, and the metal such as precious metal and copper is used into nano fabrication technique
Composite is formed it into, production cost is reduced so as to improve the utilization of resource, is with a wide range of applications.
The content of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to provide one kind use Liquid displacement methods with
Copper nano-wire is the method that template prepares platinoid nano wire, is characterized in utilizing the poor activity between metallic copper and noble metal platinum
It is different, displacement reaction occurs with copper nano-wire and platinum acid chloride solution and obtains platinoid nano wire, has that technical process is succinct, reaction bar
Part is gentle, the reaction time is shorter, cost is low, product regular appearance, catalytic activity are high, recycles and reuses the advantages that rate is high.
A kind of preparation method of described platinoid nano-material, it is characterised in that by using copper source as raw material, sodium hydroxide
Solution is solvent, and hydrazine hydrate solution is reducing agent, and copper nano-wire is prepared in water-bath 0.8-1 hours, then with copper nano-wire
For template, using the activity difference between copper and noble metal platinum, using Liquid displacement methods, sent out by copper nano-wire and platinum acid chloride solution
Raw displacement reaction obtains platinoid nano-material.
The preparation method of described a kind of platinoid nano-material, it is characterised in that copper source is Kocide SD.
The preparation method of described a kind of platinoid nano-material, it is characterised in that be additionally added in the preparation of copper nano-wire
EDA, EDA volume and the mass ratio of Kocide SD are 10-20：1, preferably 15：1, volume unit ml, mass unit g.
The preparation method of described a kind of platinoid nano-material, it is characterised in that hydrazine hydrate solution is 35wt.% hydrazine hydrates
Solution, the volume of hydrazine hydrate solution and the mass ratio of Kocide SD are 2-3：1, preferably 2.5：1, volume unit ml, quality
Unit is g.
The preparation method of described a kind of platinoid nano-material, it is characterised in that copper nano-wire is stored in 3wt.% hydrations
In hydrazine solution.
The preparation method of described a kind of platinoid nano-material, it is characterised in that take the 0.1mol/l chlorine platinum of different volumes
Acid solution prepares the platinum acid chloride solution of 100ml difference platinum contents and copper nano-wire reacts, the volume of 0.1mol/l platinum acid chloride solutions
Mass ratio with Kocide SD is 10-50：1, preferably 20：1, volume unit ml, mass unit g.
The platinoid nano-material that the preparation method obtains as catalyst waste water from dyestuff catalytic degradation application.
In described application, using Congo red solution as waste water from dyestuff, it is specially：Using sodium borohydride as reducing agent, the Congo
Red solution is pollutant substrate（Waste water from dyestuff）, the catalytic performance of composite is investigated, is often completed after being once catalyzed to catalyst
Recycled and reused, effect is recycled to investigate it.
By using above-mentioned technology, compared with prior art, beneficial effects of the present invention are as follows：
The present invention obtains platinoid nano-material by using the technology of restriction, and its technical process is succinct, reaction condition is gentle, anti-
It is short between seasonable, cost is low, and obtain platinoid nano-material product regular appearance, and given up applied to dyestuff as catalyst
Water is degraded, and with Congo red for embodiment, in Congo red reduction reaction, its catalytic activity is high, it is high to recycle and reuse rate
Advantage.
Brief description of the drawings
Fig. 1 is the SEM figures of the platinoid nano-material of the present invention；
Fig. 2 is different chloroplatinic acid content catalytic performance figures；
Fig. 3 is different catalytic condition effect contrast figures；
Fig. 4 is recycling number design sketch.
Embodiment
The present invention is further illustrated with reference to embodiments, and the present embodiment is entered premised on technical solution of the present invention
Row is implemented, and gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.
Embodiment 1
A kind of preparation method of platinoid nano-material, comprises the following steps：
1）Hydrazine hydrate solution that mass fraction is 35% and 3% is prepared respectively, 0.1mol/l platinum acid chloride solutions are with standby；
2）Precise 120g sodium hydroxides, and be dissolved in the beaker of the deionized water containing 200ml, stir, be cooled to room temperature and obtain
To strong caustic with standby；Precise 0.1g Kocide SDs, and be dissolved in gained strong caustic,
Stirring is to being completely dissolved；
3）1~2mlEDA is pipetted with liquid-transfering gun（Ethylenediamine）In above-mentioned steps 2）In the solution of gained, gentle agitation, then add again
Enter step 1）In 0.2~0.3ml35% hydrazine hydrate solutions, 70 DEG C of water-baths obtain copper nanometer in 1 hour immediately after gentle agitation
Line；Obtained copper nano-wire is stored in 3% hydrazine hydrate solution；
4）By step 3）In copper nano-wire be placed in 50ml centrifuge tubes and cleaned three times with deionized water, then by copper nm immersion in
In centrifuge tube containing deionized water, after being centrifuged 2 minutes under the conditions of 3000 r/min by water go and rejoin deionized water from
The heart, so operation are three times；Copper nanometer is placed in without in deionized water centrifuge tube again afterwards, centrifuged under the conditions of 4000 r/min
Outwell water after 2 minutes and centrifuge again, be repeated 2 times；
5）Take 1 ml steps 1）In 0.1mol/l platinum acid chloride solutions in 100ml volumetric flasks, constant volume；Then it is poured into beaker
In, while by above-mentioned steps 4）The copper nano-wire of gained is poured into same beaker, and 10~15 points are reacted under the conditions of magnetic agitation
Clock, obtains platinoid nano-material, and the SEM of gained platinoid nano-material is schemed as shown in figure 1, from figure 1 it appears that product
Regular appearance.
Above-mentioned steps 5）During can use 1~5 ml steps 1）In 0.1mol/l platinum acid chloride solutions prepare different content
Platinum acid chloride solution, so as to prepare the platinoid nano-material of different platinum contents.
Embodiment 2
To investigate platinoid nano-material in environmental area to the performance of waste water from dyestuff catalytic degradation, using Congo red solution as ginseng
Waste water from dyestuff substrate is examined, but is not limited to Congo red solution, investigates the catalytic performance of platinoid nano-material, including following step
Suddenly：
1）0.1mol/l sodium borohydride solutions are prepared with standby；
2）Prepare the Congo red ml of solution 400 of 50 μm of ol/l, the platinoid nano-material deionized water that embodiment 1 is obtained
Poured into after cleaning centrifugation in Congo red solution, while add 5 ml steps 1）In sodium borohydride solution；
3）Congo red concentration or residual rate are embodied by determining Congo red absorbance, so as to show urging for composite
Change performance.
Using the platinoid nano-material of different platinum contents as catalyst, the step of according to embodiment 2, different platinum are investigated
The platinoid nano-material catalytic performance of content, its catalyst performance figure is as shown in Fig. 2 figure it is seen that add 2mL0.1
The platinoid nano-material that mol/l platinum acid chloride solutions obtain is optimal as catalyst, its catalytic effect.
Embodiment 3
To investigate platinoid nano-material in environmental area to the performance of waste water from dyestuff catalytic degradation, using Congo red solution as ginseng
Waste water from dyestuff substrate is examined, but is not limited to Congo red solution, is imitated by contrasting the degraded to Congo red solution at different conditions
Fruit and the catalytic performance for drawing platinoid nano-material, comprise the following steps：
1）0.1mol/l sodium borohydride solutions are prepared with standby；
2）5 empty beaker numberings 1-5 are taken, prepare the Congo red ml of solution 400 of 50 μm of ol/l respectively；In the beaker of numbering 1-3
Copper nano-wire, 5 ml steps 1 respectively）In sodium borohydride solution, embodiment 2 prepare 2 ml platinum acid chloride solutions and be prepared
Platinoid nano-material；Copper nano-wire is separately added into the beaker of numbering 4-5, embodiment 2 is prepared 2 ml chloroplatinic acids and is prepared into
The platinoid nano-material arrived, while it is rapid each to add 5 ml steps 1）In sodium borohydride solution；
3）Congo red concentration or residual rate are embodied by determining Congo red absorbance, so as to show urging for composite
Change performance.
As shown in figure 3, as can be drawn from Figure 3, the beaker catalytic effect of numbering 5 is optimal, i.e. the catalytic performance of platinoid nano wire
Most preferably.
Embodiment 4
The recycling effect of platinoid nanowire composite is investigated, experiment comprises the following steps：
1）0.1mol/l sodium borohydride solutions are prepared with standby；
2）Prepare the Congo red ml of solution 400 of 50 μm of ol/l, the platinoid that embodiment 2 is prepared into 2 ml chloroplatinic acids and is prepared
Nano-material is added in Congo red solution, while adds 5 ml steps 1）Described in sodium borohydride solution；
3）Congo red absorbance was measured by sampling by every 1 minute to embody Congo red concentration or residual rate, so as to show
The catalytic performance of composite；
4）Above-mentioned steps 3）After the completion of, by catalyst collection, centrifugation；Repeat step 2 again）, step 3）；So it is repeated 5 times；With
The recycling effect of catalysis material is investigated, as shown in figure 4, can go out from Fig. 4, the catalyst of reuse, its performance shadow
Ring less, illustrate the recyclable reuse of the catalyst, at least can be used 5 times.
The above described is only a preferred embodiment of the present invention, not make any form to technical scheme
On limitation.Any simply modification, the equivalent variations that every technical spirit according to the present invention is made to above example are with repairing
Decorations, in the range of still falling within technical scheme.
Claims (7)
1. a kind of preparation method of platinoid nano-material, it is characterised in that by using copper source as raw material, sodium hydroxide solution is molten
Agent, hydrazine hydrate solution are reducing agent, and copper nano-wire is prepared in water-bath 0.8-1 hours, then using copper nano-wire as template, profit
With the activity difference between copper and noble metal platinum, using Liquid displacement methods, it is anti-that displacement is occurred by copper nano-wire and platinum acid chloride solution
Platinoid nano-material should be obtained.
2. the preparation method of a kind of platinoid nano-material according to claim 1, it is characterised in that copper source is hydroxide
Copper.
A kind of 3. preparation method of platinoid nano-material according to claim 1, it is characterised in that the system of copper nano-wire
EDA is additionally added in standby, EDA volume and the mass ratio of Kocide SD are 10-20：1, preferably 15：1, volume unit ml, matter
Amount unit is g.
4. the preparation method of a kind of platinoid nano-material according to claim 1, it is characterised in that hydrazine hydrate solution is
35wt.% hydrazine hydrate solutions, the volume of hydrazine hydrate solution and the mass ratio of Kocide SD are 2-3：1, preferably 2.5：1, volume list
Position is ml, mass unit g.
5. the preparation method of a kind of platinoid nano-material according to claim 1, it is characterised in that copper nano-wire preserves
In 3wt.% hydrazine hydrate solutions.
6. according to a kind of preparation method of any described platinoid nano-materials of claim 1-4, it is characterised in that take difference
The 0.1mol/l platinum acid chloride solutions of volume prepare the platinum acid chloride solution of 100ml difference platinum contents and copper nano-wire reacts, 0.1mol/
The volume of l platinum acid chloride solutions and the mass ratio of Kocide SD are 10-50：1, preferably 20：1, volume unit ml, mass unit
For g.
Dropped 7. the platinoid nano-material that preparation method obtains according to claim 1 is catalyzed as catalyst in waste water from dyestuff
The application of solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108832140A (en) * | 2018-06-13 | 2018-11-16 | 青岛大学 | A kind of atomic layer deposition method prepares low platinum load copper nano-wire composite catalyst and its oxygen reduction reaction application |
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| US20090050240A1 (en) * | 2003-09-09 | 2009-02-26 | Kazuyuki Tohji | Magnetic metal power and method of producing the powder |
| CN102277622A (en) * | 2011-07-22 | 2011-12-14 | 北京化工大学 | Copper-platinum superlattice alloy nano-tube and preparation method thereof |
| CN103143717A (en) * | 2011-12-06 | 2013-06-12 | 中国科学院大连化学物理研究所 | Platinoid bimetallic nanometer material and preparation method and application thereof |
| CN106378153A (en) * | 2016-11-14 | 2017-02-08 | 河北工业大学 | Preparation method of Pt-Cu linear nano-catalyst |
| CN106424754A (en) * | 2016-10-18 | 2017-02-22 | 河北工业大学 | Preparation method of PtCu alloy nanospheres |
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|---|---|---|---|---|
| US20090050240A1 (en) * | 2003-09-09 | 2009-02-26 | Kazuyuki Tohji | Magnetic metal power and method of producing the powder |
| CN102277622A (en) * | 2011-07-22 | 2011-12-14 | 北京化工大学 | Copper-platinum superlattice alloy nano-tube and preparation method thereof |
| CN103143717A (en) * | 2011-12-06 | 2013-06-12 | 中国科学院大连化学物理研究所 | Platinoid bimetallic nanometer material and preparation method and application thereof |
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| CN106378153A (en) * | 2016-11-14 | 2017-02-08 | 河北工业大学 | Preparation method of Pt-Cu linear nano-catalyst |
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| CN108832140A (en) * | 2018-06-13 | 2018-11-16 | 青岛大学 | A kind of atomic layer deposition method prepares low platinum load copper nano-wire composite catalyst and its oxygen reduction reaction application |
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