CN102847532B - Microwave method for synthesizing attapulgite and platinum nanocomposite - Google Patents
Microwave method for synthesizing attapulgite and platinum nanocomposite Download PDFInfo
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- CN102847532B CN102847532B CN201210384016.8A CN201210384016A CN102847532B CN 102847532 B CN102847532 B CN 102847532B CN 201210384016 A CN201210384016 A CN 201210384016A CN 102847532 B CN102847532 B CN 102847532B
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- recessed soil
- platinum
- composite material
- nano composite
- attapulgite
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Abstract
The invention discloses a microwave method for synthesizing an attapulgite and platinum nanocomposite. The microwave method comprises the following steps of: ultrasonically dispersing purified attapulgite into a polyvinylpyrrolidone solution; adding a Pt II or Pt IV salt solution into the polyvinylpyrrolidone solution; fully and uniformly mixing the solutions; adding a reducing agent into the mixed solutions; uniformly mixing the solutions and the reducing agent, and then carrying out reaction on the solutions and the reducing agent under microwave radiation; reducing platinum ions onto the surface of the attapulgite; and cooling, washing and drying reaction products, thus obtaining the attapulgite and platinum nanocomposite. The microwave method disclosed by the invention has the characteristics of energy conservation, environmental friendliness, rapidity and simple process; nanometre particles of platinum in the obtained attapulgite and platinum nanocomposite are uniformly distributed on a rod-shaped attapulgite structure; and the microwave method develops a new field of attapulgite development and application.
Description
Technical field
The present invention relates to a kind of preparation of attapulgite clay nano composite material, relate in particular to a kind of preparation method of recessed soil/platinum nano composite material, be i.e. a kind of preparation method of attapulgite clay supported platinum nano composite.
Background technology
Attapulgite clay (being called for short recessed soil) is a kind of native compound of nano-scale, is rich zeopan.There are little (2.0～2.3 g/cm of density
3), inner multi-pore channel, specific area (can reach 500 m greatly
2/ g), water imbibition is strong and be difficult for by characteristics such as electrolyte flocculate, thereby there is the property such as corrosion of strong adsorption capacity, good heat resistance, anti-salt, alkali, the carrier of using it for catalyst has many potential specific uses.Apply and be also in the incipient stage about the research of recessed native nano composite material at present, and for recessed native nano material itself, electric conductivity is poor.
Using recessed soil as carrier, noble metal platinum is modified on recessed soil, make recessed soil/platinum nano composite material, can effectively improve the electric conductivity of recessed soil, and give certain catalytic performance, be expected to be applied in electrochemistry and catalytic field.
Summary of the invention
The object of this invention is to provide a kind of preparation method of novel recessed soil/platinum nano composite material, described method is selected microwave heating method, under the common condition existing of recessed soil, Pt slaine and reducing agent, Fast Heating is reduced Pt and is loaded on recessed soil surface, obtains recessed soil/platinum nano composite material.
The present invention is achieved by the following technical solutions:
A method for the synthetic recessed soil/platinum nano composite material of microwave method, is characterized in that being dispersed in the polyvinylpyrrolidone aqueous solution ultrasonic the recessed soil of purifying, adds Pt
iIor Pt
iVsalting liquid, fully mixes, and adds reducing agent, after mixing, under the radiation of microwave, reacts, and platinum ion reduction back loading is on recessed soil surface, and product is cooling, washing, dryly can obtain recessed soil/platinum nano composite material.
Described method is made up of the following step:
Step 1) is by ultrasonic the recessed soil of the purifying aqueous solution that is dispersed in polyvinylpyrrolidone, and the concentration of polyvinylpyrrolidonesolution solution is 4-8 g/L, and recessed native content is 2-2.5 g/L.
Step 2) in above-mentioned solution, add Pt
iIor Pt
iVsalting liquid, fully mixes, Pt in mixed solution
iIor Pt
iVthe concentration of salt is 2-3 mmol/L.
Step 3) is by step 2) add reducing agent in the solution that obtains, after mixing, be transferred in microwave chemical reactor, heating using microwave reaction, platinum ion reduction back loading is on recessed soil surface, product is cooled to room temperature, centrifugal, washing, obtains recessed soil/platinum nano composite material after dry.
Described Pt
iIsalting liquid is PtCl
2, K
2ptCl
4or Na
2ptCl
4, Pt
iVsalting liquid is K
2ptCl
6or H
2ptCl
6.
Described reducing agent is sodium borohydride, trisodium citrate, ascorbic acid, sodium hypophosphite or sodium phosphite, preferably ascorbic acid.
Compared with the prior art, the present invention has following outstanding feature:
Recessed soil is a kind of natural nano-material, cheap, there is very high inside and outside specific area, recessed soil has good absorption property, and abundant-OH is contained on its surface, and these functional groups can be by adsorption of metal ions on its surface, under microwave, the reducing agents such as ascorbic acid are by the reduction of Pt metal ion, and the nano platinum particle obtaining loads on the surface of recessed soil, obtains recessed native supporting Pt nano particle.
In synthetic solvent, add nonionic surface active agent polyvinylpyrrolidone (PVP), this surfactant contains hydrophobic [N – C
2h
3]
nskeleton structure, and be connected with hydrophilic side group in this skeleton structure, therefore, in the time that PVP is dispersed in the aqueous solution, C=O key wherein and will be exposed to solution surface containing N group.Therefore, once there be Pt to generate, the C=O key in PVP molecule and N will be combined with Pt atom, form covalent bond, be adsorbed onto securely Pt particle surface, thereby Pt nano particle is played to good peptizaiton.
Utilize microwave method to synthesize, compare with traditional hydro-thermal method, the method has short, simple, energy-conservation and efficiency high consuming time.
Recessed soil/platinum nano composite material that the present invention obtains, the Pt that loads on recessed soil surface is bobbles shape nano particle, its particle diameter is 5 ~ 20 nm, by can significantly seeing that from enlarged drawing this structure is to be flocked together and formed by the nano platinum particle of many 2 ~ 3 nm, therefore, this structure has larger specific surface.In the recessed soil/platinum nano composite material obtaining, nano platinum particle is evenly distributed in bar-shaped recessed soil structure, has started a new field to the Application and Development of recessed soil, improves the economic value added of recessed soil.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with detailed description of the invention, but is limited by claim.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction (XRD) of recessed soil/platinum nano composite material of the present invention.
Fig. 2 is the transmission electron microscope (TEM) of recessed soil/platinum nano composite material of the present invention.
Detailed description of the invention
Embodiment 1
The method of the synthetic recessed soil/platinum nano composite material of microwave method, comprises the following steps:
1) in the distilled water of 40 mL, add the polyvinylpyrrolidone of 0.25 g, after stirring and dissolving, add again the recessed soil of 0.1 g purifying, ultrasonic dispersion;
2) in above-mentioned mixed liquor, add the K of 4.3 mL
2ptCl
4(10 mg/mL) solution stirs 1 hour;
3) last, add the ascorbic acid (80 g/L) of 5 mL to mix, solution is transferred in microwave chemical reactor, connects condensed water, setting power is 200 W, heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 DEG C of oven dry.
Transmission electron microscope observing, in recessed soil/platinum nano composite material of gained, recessed native club shaped structure surface uniform load bobbles shape Pt nanostructured, its particle diameter is 5 ~ 20 nm, this structure forms by being flocked together by the nano platinum particle of many 2 ~ 3 nm.
Embodiment 2
The method of the synthetic recessed soil/platinum nano composite material of microwave method, comprises the following steps:
1) in the distilled water of 40 mL, add the polyvinylpyrrolidone of 0.25 g, after stirring and dissolving, add again the recessed soil of 0.1 g purifying, ultrasonic dispersion;
2) in above-mentioned mixed liquor, add the H of 5.3 mL
2ptCl
66H
2o(10 mg/mL) solution stir 1 hour;
3) last, add the ascorbic acid (80 g/L) of 5 mL to mix, solution is transferred in microwave chemical reactor, connects condensed water, setting power is 200 W, heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 DEG C of oven dry.Transmission electron microscope observing, with the product comparison that embodiment 1 obtains, structure is substantially similar.
Embodiment 3
The method of the synthetic recessed soil/platinum nano composite material of microwave method, comprises the following steps:
1) in the distilled water of 40 mL, add the polyvinylpyrrolidone of 0.20 g, after stirring and dissolving, add again the recessed soil of 0.1 g purifying, ultrasonic dispersion;
2) in above-mentioned mixed liquor, add the K of 5.0 mL
2ptCl
6(10 mg/mL) solution stirs 1 hour;
3) last, add the ascorbic acid (80 g/L) of 5 mL to mix, solution is transferred in microwave chemical reactor, connects condensed water, setting power is 200 W, heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 DEG C of oven dry.Transmission electron microscope observing, with the product comparison that embodiment 1 obtains, structure is substantially similar.
Embodiment 4
The method of the synthetic recessed soil/platinum nano composite material of microwave method, comprises the following steps:
1) in the distilled water of 40 mL, add the polyvinylpyrrolidone of 0.20 g, after stirring and dissolving, add again the recessed soil of 0.1 g purifying, ultrasonic dispersion;
2) in above-mentioned mixed liquor, add the K of 2.50 mL
2ptCl
6(10 mg/mL) solution stirs 1 hour;
3) last, add the ascorbic acid (80 g/L) of 5 mL to mix, solution is transferred in microwave chemical reactor, connects condensed water, setting power is 200 W, heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 DEG C of oven dry.Transmission electron microscope observing, with the product comparison that embodiment 1 obtains, the particle diameter of bobbles shape Pt nanostructured is 5 ~ 10 nm.
Embodiment 5
The method of the synthetic recessed soil/platinum nano composite material of microwave method, comprises the following steps:
1) in the distilled water of 50 mL, add the polyvinylpyrrolidone of 0.25 g, after stirring and dissolving, add again the recessed soil of 0.1 g purifying, ultrasonic dispersion;
2) in above-mentioned mixed liquor, add the K of 5.0 mL
2ptCl
6(10 mg/mL) solution stirs 1 hour;
3) last, add the ascorbic acid (80 g/L) of 5 mL to mix, solution is transferred in microwave chemical reactor, connects condensed water, setting power is 200 W, heating using microwave reaction is after 2 minutes, take out, naturally cool to room temperature, take out sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 DEG C of oven dry.Transmission electron microscope observing, with the product comparison that embodiment 4 obtains, structure is substantially similar.
Embodiment 6
The method of the synthetic recessed soil/platinum nano composite material of microwave method, comprises the following steps:
1) in the distilled water of 50 mL, add the polyvinylpyrrolidone of 0.3 g, after stirring and dissolving, add again the recessed soil of 0.1 g purifying, ultrasonic dispersion;
2) in above-mentioned mixed liquor, add the K of 7.0 mL
2ptCl
6(10 mg/mL) solution stirs 1 hour;
3) last, add the ascorbic acid (80 g/L) of 5 mL to mix, solution is transferred in microwave chemical reactor, connects condensed water, setting power is 200 W, heating using microwave reaction is after 2 minutes, take out, naturally cool to room temperature, take out sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 DEG C of oven dry.Transmission electron microscope observing, with the product comparison that embodiment 1 obtains, structure is substantially similar.
Claims (4)
1. a method for the synthetic recessed soil/platinum nano composite material of microwave method, is characterized in that, described method comprises the following steps:
Step 1) is dispersed in the polyvinylpyrrolidone aqueous solution ultrasonic the recessed soil of purifying, and the concentration of polyvinylpyrrolidonesolution solution is 4-8 g/L, and recessed native content is 2-2.5 g/L;
Step 2) in above-mentioned solution, add Pt
iIor Pt
iVsalting liquid, fully mixes, Pt in mixed solution
iIor Pt
iVthe concentration of salt is 2-3 mmol/L;
Step 3) is in step 2) solution in add reducing agent, after mixing, be transferred in microwave chemical reactor, heating using microwave reaction, platinum ion reduction back loading is on recessed soil surface, product is cooled to room temperature, centrifugal, washing, obtains recessed soil/platinum nano composite material after dry, in described recessed soil/platinum nano composite material, the Pt that loads on recessed soil surface is bobbles shape nano particle, and particle diameter is 5 ~ 20 nm.
2. the method for synthetic recessed soil/platinum nano composite material according to claim 1 and 2, is characterized in that described Pt
iIsalt is PtCl
2, K
2ptCl
4or Na
2ptCl
4, Pt
iVsalt is K
2ptCl
6or H
2ptCl
6.
3. the method for synthetic recessed soil/platinum nano composite material according to claim 1 and 2, is characterized in that, described reducing agent is sodium borohydride, trisodium citrate, ascorbic acid, sodium hypophosphite or sodium phosphite.
4. the method for synthetic recessed soil/platinum nano composite material according to claim 3, is characterized in that, described reducing agent is ascorbic acid.
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|---|---|---|---|---|
| CN101007279A (en) * | 2007-01-20 | 2007-08-01 | 淮阴工学院 | Multivariate catalyst for hydrogenation of edible oils and its preparation method |
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|---|---|---|---|---|
| CN101007279A (en) * | 2007-01-20 | 2007-08-01 | 淮阴工学院 | Multivariate catalyst for hydrogenation of edible oils and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 凹凸棒土负载铂催化剂上对氯硝基苯的高活性高选择性液相加氢反应;王芳等;《物理化学学报》;20090617;第25卷(第8期);第1678-1682页 * |
| 王芳等.凹凸棒土负载铂催化剂上对氯硝基苯的高活性高选择性液相加氢反应.《物理化学学报》.2009,第25卷(第8期),第1678-1682页. |
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