CN102847532A - Microwave method for synthesizing attapulgite and platinum nanocomposite - Google Patents
Microwave method for synthesizing attapulgite and platinum nanocomposite Download PDFInfo
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- CN102847532A CN102847532A CN2012103840168A CN201210384016A CN102847532A CN 102847532 A CN102847532 A CN 102847532A CN 2012103840168 A CN2012103840168 A CN 2012103840168A CN 201210384016 A CN201210384016 A CN 201210384016A CN 102847532 A CN102847532 A CN 102847532A
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- recessed soil
- composite material
- platinum
- 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 the preparation method of a kind of recessed soil/platinum nano composite material, be i.e. a kind of attapulgite clay supported platinum nano composite manufacture method.
Background technology
Attapulgite clay (being called for short recessed soil) is a kind of native compound of nano-scale, is rich zeopan.Have 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 have the properties 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.The research of at present relevant recessed native nano composite material is used and also is in the incipient stage, and for recessed native nano material itself, electric conductivity is poor.
, as carrier noble metal platinum is modified on the recessed soil with recessed soil, makes recessed soil/platinum nano composite material, can effectively improve the electric conductivity of recessed soil, and give certain catalytic performance, be expected in electrochemistry and catalytic field, be applied.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of novel recessed soil/platinum nano composite material, described method is selected microwave heating method, under the common condition that exists of recessed soil, Pt slaine and reducing agent, Fast Heating is with the Pt reduction and load on recessed soil surface, obtains recessed soil/platinum nano composite material.
The present invention is achieved by the following technical solutions:
A kind of microwave method is synthesized the method for recessed soil/platinum nano composite material, it is characterized in that being dispersed in the polyvinylpyrrolidone aqueous solution the recessed soil of purifying is ultrasonic, adds Pt
IIOr Pt
IVSalting liquid fully mixes, and adds reducing agent, reacts under the radiation of microwave after mixing, and platinum ion reduction back loading is on recessed soil surface, and product cooling, washing, drying can obtain recessed soil/platinum nano composite material.
Described method is comprised of the following step:
Step 1) is with in the ultrasonic aqueous solution that is dispersed in polyvinylpyrrolidone of 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 mentioned solution, adds Pt
IIOr Pt
IVSalting liquid fully mixes, Pt in the mixed solution
IIOr Pt
IVThe concentration of salt is 2-3 mmol/L.
Step 3) is with step 2) add reducing agent in the solution that obtains, be transferred to after mixing in the microwave chemical reactor, the heating using microwave reaction, platinum ion reduction back loading is on recessed soil surface, product is cooled to room temperature, obtains recessed soil/platinum nano composite material after centrifugal, washing, the drying.
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, preferred ascorbic acid.
Compared with the prior art, the present invention has following outstanding feature:
Recessed soil is a kind of natural nano-material, cheap, has 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 with adsorption of metal ions on its surface, under microwave, the reducing agents such as ascorbic acid are with the reduction of Pt metal ion, and resulting nano platinum particle loads on the surface of recessed soil, obtains recessed native supporting Pt nano particle.
Add nonionic surface active agent polyvinylpyrrolidone (PVP) in synthetic solvent, the agent alive of this table contains hydrophobic [N – C
2H
3]
nSkeleton structure, and be connected with hydrophilic side group on this skeleton structure, therefore, when PVP is dispersed in the aqueous solution, C=O key wherein and contain the N group and will be exposed to solution surface.Therefore, in case there is Pt to generate, the C=O key in the PVP molecule and N will be combined with the Pt atom, form covalent bond, be adsorbed onto securely the Pt particle surface, thereby the Pt nano particle is played good peptizaiton.
Utilize microwave method to synthesize, compare with traditional hydro-thermal method, the method has short, simple, energy-conservation and efficient high consuming time.
The resulting recessed soil of the present invention/platinum nano composite material, the Pt that loads on recessed soil surface is bobbles shape nano particle, its particle diameter is 5 ~ 20 nm, by seeing significantly that from enlarged drawing this structure is that nano platinum particle by many 2 ~ 3 nm flocks together and forms, therefore, this structure has larger specific surface.In resulting recessed soil/platinum nano composite material, nano platinum particle is evenly distributed on the bar-shaped recessed soil structure, has started a new field for 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 the specific embodiment, but is limited by claim.
Description of drawings
Fig. 1 is the X-ray powder diffraction (XRD) of recessed soil of the present invention/platinum nano composite material.
Fig. 2 is the transmission electron microscope (TEM) of recessed soil of the present invention/platinum nano composite material.
The specific embodiment
Embodiment 1
Microwave method is synthesized the method for recessed soil/platinum nano composite material, comprises the following steps:
1) adds the polyvinylpyrrolidone of 0.25 g in the distilled water of 40 mL, add again the recessed soil of 0.1 g purifying after the stirring and dissolving, ultrasonic dispersion;
2) K of adding 4.3 mL in above-mentioned mixed liquor
2PtCl
4(10 mg/mL) solution stirred 1 hour;
3) last, ascorbic acid (80 g/L) mixing that adds 5 mL, solution is transferred in the microwave chemical reactor, connects condensed water, setting power is 200 W, the heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out the sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 ℃ of oven dry.
Transmission electron microscope observing, in the recessed soil of gained/platinum nano composite material, recessed native club shaped structure surface uniform load bobbles shape Pt nanostructured, its particle diameter is 5 ~ 20 nm, this structure is flocked together by the nano platinum particle by many 2 ~ 3 nm and forms.
Embodiment 2
Microwave method is synthesized the method for recessed soil/platinum nano composite material, comprises the following steps:
1) adds the polyvinylpyrrolidone of 0.25 g in the distilled water of 40 mL, add again the recessed soil of 0.1 g purifying after the stirring and dissolving, ultrasonic dispersion;
2) H of adding 5.3 mL in above-mentioned mixed liquor
2PtCl
66H
2O(10 mg/mL) solution stirred 1 hour;
3) last, ascorbic acid (80 g/L) mixing that adds 5 mL, solution is transferred in the microwave chemical reactor, connects condensed water, setting power is 200 W, the heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out the sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 ℃ of oven dry.Transmission electron microscope observing compares with embodiment 1 resulting product, and structure is substantially similar.
Embodiment 3
Microwave method is synthesized the method for recessed soil/platinum nano composite material, comprises the following steps:
1) adds the polyvinylpyrrolidone of 0.20 g in the distilled water of 40 mL, add again the recessed soil of 0.1 g purifying after the stirring and dissolving, ultrasonic dispersion;
2) K of adding 5.0 mL in above-mentioned mixed liquor
2PtCl
6(10 mg/mL) solution stirred 1 hour;
3) last, ascorbic acid (80 g/L) mixing that adds 5 mL, solution is transferred in the microwave chemical reactor, connects condensed water, setting power is 200 W, the heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out the sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 ℃ of oven dry.Transmission electron microscope observing compares with embodiment 1 resulting product, and structure is substantially similar.
Embodiment 4
Microwave method is synthesized the method for recessed soil/platinum nano composite material, comprises the following steps:
1) adds the polyvinylpyrrolidone of 0.20 g in the distilled water of 40 mL, add again the recessed soil of 0.1 g purifying after the stirring and dissolving, ultrasonic dispersion;
2) K of adding 2.50 mL in above-mentioned mixed liquor
2PtCl
6(10 mg/mL) solution stirred 1 hour;
3) last, ascorbic acid (80 g/L) mixing that adds 5 mL, solution is transferred in the microwave chemical reactor, connects condensed water, setting power is 200 W, the heating using microwave reaction is after 3 minutes, take out, naturally cool to room temperature, take out the sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 ℃ of oven dry.Transmission electron microscope observing compares with embodiment 1 resulting product, and the particle diameter of bobbles shape Pt nanostructured is 5 ~ 10 nm.
Embodiment 5
Microwave method is synthesized the method for recessed soil/platinum nano composite material, comprises the following steps:
1) adds the polyvinylpyrrolidone of 0.25 g in the distilled water of 50 mL, add again the recessed soil of 0.1 g purifying after the stirring and dissolving, ultrasonic dispersion;
2) K of adding 5.0 mL in above-mentioned mixed liquor
2PtCl
6(10 mg/mL) solution stirred 1 hour;
3) last, ascorbic acid (80 g/L) mixing that adds 5 mL, solution is transferred in the microwave chemical reactor, connects condensed water, setting power is 200 W, the heating using microwave reaction is after 2 minutes, take out, naturally cool to room temperature, take out the sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 ℃ of oven dry.Transmission electron microscope observing compares with embodiment 4 resulting products, and structure is substantially similar.
Embodiment 6
Microwave method is synthesized the method for recessed soil/platinum nano composite material, comprises the following steps:
1) adds the polyvinylpyrrolidone of 0.3 g in the distilled water of 50 mL, add again the recessed soil of 0.1 g purifying after the stirring and dissolving, ultrasonic dispersion;
2) K of adding 7.0 mL in above-mentioned mixed liquor
2PtCl
6(10 mg/mL) solution stirred 1 hour;
3) last, ascorbic acid (80 g/L) mixing that adds 5 mL, solution is transferred in the microwave chemical reactor, connects condensed water, setting power is 200 W, the heating using microwave reaction is after 2 minutes, take out, naturally cool to room temperature, take out the sample ultrasonic washing, washing, ethanol are washed each three times, obtain recessed soil/platinum nano composite material after 60 ℃ of oven dry.Transmission electron microscope observing compares with embodiment 1 resulting product, and structure is substantially similar.
Claims (6)
1. the method for the synthetic recessed soil of a microwave method/platinum nano composite material is characterized in that: in the ultrasonic aqueous solution that is dispersed in polyvinylpyrrolidone of recessed soil, add Pt
IIOr Pt
IVSalting liquid fully mixes, and adds reducing agent, reacts under the radiation of microwave after mixing, and platinum ion reduction back loading is on recessed soil surface, and product cooling, washing, drying can obtain recessed soil/platinum nano composite material.
2. the method for synthetic recessed soil according to claim 1/platinum nano composite material is characterized in that, described method comprises the following steps:
Step 1) is dispersed in the polyvinylpyrrolidone aqueous solution the recessed soil of purifying is ultrasonic, and the concentration of polyvinylpyrrolidonesolution solution is 4-8 g/L, and recessed native content is 2-2.5 g/L;
Step 2) in mentioned solution, adds Pt
IIOr Pt
IVSalting liquid fully mixes, Pt in the mixed solution
IIOr Pt
IVThe concentration of salt is 2-3 mmol/L;
Step 3) is in step 2) solution in add reducing agent, be transferred to after mixing in the microwave chemical reactor, the heating using microwave reaction, platinum ion reduction back loading is on recessed soil surface, product is cooled to room temperature, obtains recessed soil/platinum nano composite material after centrifugal, washing, the drying.
3. the method for synthetic recessed soil according to claim 1 and 2/platinum nano composite material 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
4. the method for synthetic recessed soil according to claim 1 and 2/platinum nano composite material is characterized in that, described reducing agent is sodium borohydride, trisodium citrate, ascorbic acid, sodium hypophosphite or sodium phosphite.
5. the method for synthetic recessed soil according to claim 4/platinum nano composite material is characterized in that, described reducing agent is ascorbic acid.
6. the method for synthetic recessed soil according to claim 1 and 2/platinum nano composite material is characterized in that, 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.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (1)
| Title |
|---|
| 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》 * |
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