CN107498066B - 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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- CN107498066B CN107498066B CN201710801814.9A CN201710801814A CN107498066B CN 107498066 B CN107498066 B CN 107498066B CN 201710801814 A CN201710801814 A CN 201710801814A CN 107498066 B CN107498066 B CN 107498066B
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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.The purpose of the present invention is to provide a kind of methods for using Liquid displacement methods to prepare platinoid nano wire as template using copper nano-wire, its main feature is that utilizing the activity difference between metallic copper and noble metal platinum, occur to replace to react with platinum acid chloride solution with copper nano-wire to obtain platinoid nano wire, have the advantages that technical process is succinct, reaction condition is mild, the reaction time is shorter, at low cost, product regular appearance, catalytic activity are high, it is high to recycle and reuse rate, 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 material catalytic degradation is investigated；And it is investigated by recycling catalyst recycling and reuses effect.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, it is related to preparing monodimension nanometer material with liquid phase transformation approach, specifically
It is a kind of platinoid nano-material preparation method and applications.
Background technique
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 nanoparticles such as Au, Ag, Pt have excellent catalytic properties,
The characteristics such as good chemical stability cause scientific circles and greatly pay close attention to.The catalytic performance of Au, Ag, Pt nanoparticle and its
Size is closely related, high dispersive, small size nanoparticle there is big specific surface area, show more excellent catalysis work
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 nanoparticles 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.It introduces 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, performance stabilization energy is reused.
Compared to other metals, the advantages of metallic copper, is that the market price is relatively inexpensive, has good heat, electrical conductivity,
Chemical property is relatively stable.Copper nanometer has large specific surface area, 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, percentage shared by surface atom is big, the key state on surface and
Electronic state is different from inside particle, and surface atom is coordinated the not congruent active position for leading to surface and increases, this makes it have 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 have catalytic performance.Meanwhile for the configuration of surface of nanoparticle, with the reduction of partial size, surface is smooth
Degree reduces, and forms scraggly atomic steps, this adds increased the contact surfaces of chemical reaction, 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 is especially an important field in nanoscale science and technology in dye wastewater treatment field.Made at present
Based on noble metal, active component most noble metal in the surface of nano particle, core can be wasted catalyst
Fall.In order to save expensive metal resource and save precious metal catalyst production cost, while improving the catalysis effect of catalyst
Rate and raising dye wastewater treatment efficiency simultaneously save treatment cost, and the metals such as precious metal and copper are used nano fabrication technique
Composite material is formed it into, so that improving utilizing for resource reduces production cost, is with a wide range of applications.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide it is a kind of use Liquid displacement methods with
Copper nano-wire is the method that template prepares platinoid nano wire, its main feature is that utilizing the poor activity between metallic copper and noble metal platinum
It is different, occur to replace to react with platinum acid chloride solution with copper nano-wire to obtain platinoid nano wire, reaction item succinct with technical process
Part is mild, the reaction time is shorter, at low cost, product regular appearance, catalytic activity are high, recycles and reuses the advantages that rate is high.
A kind of preparation method of the 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, copper nano-wire is prepared within water-bath 0.8-1 hours, then with copper nano-wire
For template, sent out using Liquid displacement methods by copper nano-wire and platinum acid chloride solution using the activity difference between copper and noble metal platinum
Raw displacement reaction obtains platinoid nano-material.
The preparation method of a kind of platinoid nano-material, it is characterised in that copper source is Kocide SD.
The preparation method of a kind of platinoid nano-material, it is characterised in that be additionally added in the preparation of copper nano-wire
The volume of EDA, EDA and the mass ratio of Kocide SD are 10-20:1, preferably 15:1, volume unit ml, mass unit g.
The preparation method of a kind of platinoid nano-material, it is characterised in that hydrazine hydrate solution is 35wt.% hydrazine hydrate
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 a kind of platinoid nano-material, it is characterised in that copper nano-wire is stored in 3wt.% hydration
In hydrazine solution.
The preparation method of a kind of platinoid nano-material, it is characterised in that take the 0.1mol/l chlorine platinum of different volumes
The platinum acid chloride solution that acid solution prepares 100ml difference platinum content is reacted with copper nano-wire, the volume of 0.1mol/l platinum acid chloride solution
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 the application, using Congo red solution as waste water from dyestuff, specifically: using sodium borohydride as reducing agent, the Congo
Red solution is pollutant substrate (waste water from dyestuff), the catalytic performance of composite material is investigated, to catalyst after every primary catalysis of completion
It is recycled and reused, recycles effect 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 technical process is succinct, reaction condition temperature
It is short, at low cost with the reaction time, and platinoid nano-material product regular appearance is obtained, and be applied to as catalyst
Dye wastewater degradation, with Congo red for embodiment, in Congo red reduction reaction, catalytic activity is high, recycles and reuses
The advantages that rate is high.
Detailed description of the invention
Fig. 1 is that the SEM of platinoid nano-material of the invention schemes；
Fig. 2 is different chloroplatinic acid content catalytic performance figures；
Fig. 3 is different catalytic condition effect contrast figures；
Fig. 4 is recycling number effect picture.
Specific embodiment
The present invention is further illustrated with reference to embodiments, the present embodiment based on the technical solution of the present invention into
Row is implemented, and the detailed implementation method and specific operation process are given, 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, includes the following steps:
1) hydrazine hydrate solution that mass fraction is 35% and 3%, 0.1mol/l platinum acid chloride solution are prepared respectively with spare；
2) precise 120g sodium hydroxide, and be dissolved in the beaker of the deionized water containing 200ml, it stirs, is cooled to room
Temperature obtains strong caustic with spare；Precise 0.1g Kocide SD, and it is molten to be dissolved in gained concentrated sodium hydroxide
In liquid, stirring is to being completely dissolved；
3) 1~2mlEDA(ethylenediamine is pipetted with liquid-transfering gun) in above-mentioned steps 2) in resulting solution, gentle agitation, then
Add 0.2~0.3ml35% hydrazine hydrate solution in step 1), after gentle agitation immediately 70 DEG C obtain copper within water-bath 1 hour
Nano wire；Copper nano-wire obtained is stored in 3% hydrazine hydrate solution；
4) copper nano-wire in step 3) is placed in 50ml centrifuge tube and is cleaned three times with deionized water, then copper nanometer is soaked
Water is gone after being centrifuged 2 minutes under the conditions of 3000 r/min in centrifuge tube containing deionized water and rejoins deionization by stain
Water centrifugation, so operation are three times；Copper nanometer is placed in without in deionized water centrifuge tube again later, under the conditions of 4000 r/min
Centrifugation is outwelled water and is centrifuged again after 2 minutes, is repeated 2 times；
5) take the 0.1mol/l platinum acid chloride solution in 1 ml step 1) in 100ml volumetric flask, constant volume；Then it is poured into
In beaker, while by above-mentioned steps 4) resulting copper nano-wire pours into same beaker, react 10 under the conditions of magnetic agitation~
15 minutes, obtain platinoid nano-material, the SEM figure of gained platinoid nano-material as shown in Figure 1, from figure 1 it appears that
Product regular appearance.
Above-mentioned steps 5) during 0.1mol/l platinum acid chloride solution in desirable 1~5 ml step 1) prepare different content
Platinum acid chloride solution, 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, with Congo red solution
For reference dye waste water substrate, but it is not limited to Congo red solution, investigates the catalytic performance of platinoid nano-material, including as follows
Step:
1) 0.1mol/l sodium borohydride solution is prepared with spare；
2) prepare Congo red 400 ml of solution of 50 μm of ol/l, by the platinoid nano-material that embodiment 1 obtains spend from
The sodium borohydride solution for pouring into Congo red solution after sub- water cleaning centrifugation, while being added in 5 ml step 1)；
3) Congo red concentration or residual rate are embodied by measuring Congo red absorbance, to show composite material
Catalytic 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, catalyst performance figure is as shown in Fig. 2, figure it is seen that be added 2mL0.1
For the platinoid nano-material that mol/l platinum acid chloride solution obtains as catalyst, catalytic effect is best.
Embodiment 3
To investigate platinoid nano-material in environmental area to the performance of waste water from dyestuff catalytic degradation, with Congo red solution
For reference dye waste water substrate, but it is not limited to Congo red solution, by comparing at different conditions to the drop of Congo red solution
Solution effect and obtain the catalytic performance of platinoid nano-material, include the following steps:
1) 0.1mol/l sodium borohydride solution is prepared with spare；
2) 5 empty beaker numbers 1-5 are taken, prepare Congo red 400 ml of solution of 50 μm of ol/l respectively；The burning of number 1-3
Copper nano-wire, the sodium borohydride solution in 5 ml step 1), embodiment 2 are prepared 2 ml platinum acid chloride solutions and are prepared into respectively in cup
The platinoid nano-material arrived；Copper nano-wire is separately added into the beaker of number 4-5, embodiment 2 is prepared 2 ml chloroplatinic acids and made
Standby obtained platinoid nano-material, and at the same time it is rapid that 5 ml step 1 is respectively added) in sodium borohydride solution；
3) Congo red concentration or residual rate are embodied by measuring Congo red absorbance, to show composite material
Catalytic performance.
As shown in figure 3, as can be drawn from Figure 3,5 beaker catalytic effect of number is best, i.e. the catalytic performance of platinoid nano wire
Most preferably.
Embodiment 4
The recycling effect of platinoid nanowire composite is investigated, test includes the following steps:
1) 0.1mol/l sodium borohydride solution is prepared with spare；
2) Congo red 400 ml of solution of 50 μm of ol/l is prepared, embodiment 2 is prepared into 2 ml chloroplatinic acids and is prepared
Platinoid nano-material is added in Congo red solution, while sodium borohydride solution described in 5 ml step 1) is added；
3) Congo red concentration or residual rate are embodied by Congo red absorbance being measured by sampling within every 1 minute, thus
Show the catalytic performance of composite material；
4) above-mentioned steps 3) after the completion of, by catalyst collection, centrifugation；Step 2, step 3) are repeated again；So repeat 5
It is secondary；To investigate the recycling effect of catalysis material, as shown in figure 4, can go out from Fig. 4, the catalyst of reuse, property
It can influence less, to illustrate that the catalyst is recyclable and reuse, at least can be used 5 times.
The above described is only a preferred embodiment of the present invention, not making any form to technical solution of the present invention
On limitation.According to the technical essence of the invention any simple modification to the above embodiments, equivalent variations and repair
Decorations, in the range of still falling within technical solution of the present invention.
Claims (3)
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, copper nano-wire are prepared within water-bath 0.8-1 hours, then using copper nano-wire as template, benefit
It is anti-that displacement is occurred by copper nano-wire and platinum acid chloride solution using Liquid displacement methods with the activity difference between copper and noble metal platinum
It should obtain platinoid nano-material；
Copper source is Kocide SD；
Ethylenediamine is additionally added in the preparation of the copper nano-wire, the volume of ethylenediamine and the mass ratio of Kocide SD are 10-20:1,
Volume unit is mL, mass unit g；
Hydrazine hydrate solution is 35wt.% hydrazine hydrate solution, and the volume of hydrazine hydrate solution and the mass ratio of Kocide SD are 2-3:1, body
Product unit is mL, mass unit g；
The copper nano-wire is stored in 3wt.% hydrazine hydrate solution；
0.1 mol/L platinum acid chloride solution of different volumes is taken to prepare the platinum acid chloride solution and copper nano-wire of 100 mL difference platinum contents
Reaction, the volume of 0.1 mol/L platinum acid chloride solution and the mass ratio of Kocide SD are 10-50:1.
2. a kind of preparation method of platinoid nano-material according to claim 1, it is characterised in that hydrazine hydrate solution
The mass ratio of volume and Kocide SD is 2.5:1.
3. according to claim 1 or a kind of preparation method of 2 any platinoid nano-materials, it is characterised in that take difference
The platinum acid chloride solution that 0.1 mol/L platinum acid chloride solution of volume prepares 100 mL difference platinum contents is reacted with copper nano-wire, and 0.1
The volume of mol/L platinum acid chloride solution and the mass ratio of Kocide SD are 20:1.
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