CN101712487A - Method for preparing beta-type lead dioxide nanometer particles - Google Patents
Method for preparing beta-type lead dioxide nanometer particles Download PDFInfo
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- CN101712487A CN101712487A CN200910181099A CN200910181099A CN101712487A CN 101712487 A CN101712487 A CN 101712487A CN 200910181099 A CN200910181099 A CN 200910181099A CN 200910181099 A CN200910181099 A CN 200910181099A CN 101712487 A CN101712487 A CN 101712487A
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Abstract
The invention discloses beta-type lead dioxide nanometer particles and a preparation method thereof. In the method, by a hydrothermal method, lead nitrate serving as a raw material is added with proper amount of oxidant and additive at a lower temperature to prepare a large amount of beta-type lead dioxide nanometer particles. The method has the advantages that: the cost is low; the production process is greatly simplified; and the lead dioxide nanometer particles, prepared by the method, have a controllable particle size and shape, a big specific surface area, high conversion efficiency and catalytic activity and wide application prospect in fields of electrochemistry and catalysis. Therefore the method is suitable for mass industrialized production.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly, is a kind of β-type plumbic oxide nano particle and preparation method thereof.
Background technology
Plumbic oxide is broad-spectrum strong oxidizer and important electrode materials, especially in acidic medium, show excellent chemical stability, it is one of ultimate constituent of polar plate of lead acid storage battery, all having a wide range of applications aspect conversion, recycling and the environmental improvement of the energy, wherein again with the β-type plumbic oxide of tetragonal system at aspects such as electroconductibility, erosion resistances the performance than the α-type plumbic oxide of rhombic system more excellent.The plumbic oxide nano particle is because size is little, specific surface area is big, the complete and not surperficial key attitude of surface atom coordination is different with granule interior with electronic state, therefore its surperficial active sites is more, can show the not available characteristic of plumbic oxide block materials, have high transformation efficiency and catalytic activity, thereby have more wide application prospect in electrochemical field and catalytic field.
But the research of at present relevant plumbic oxide nano particle is actually rare, the nanocrystalline synthetic method of a kind of plumbic oxide was only disclosed in Chinese patent ZL02100264.9, this method mainly is earlier lead salt or plumbous oxide to be added in the entry, then to wherein adding sodium hydroxide, the pH value of regulator solution is between 9～14, again with oxygenant generation liquid phase reactions such as chlorine, thereby it is nanocrystalline to obtain β-type plumbic oxide under 60～200 ℃ of temperature.But the technology of aforesaid method is comparatively complicated, and the particle diameter of plumbic oxide nano-powder and pattern are uncontrollable, are not suitable for large-scale industrialization and use.
Summary of the invention
The object of the present invention is to provide a kind of β-type plumbic oxide nano particle and method thereof, this method is with low cost, technology is simple, and the particle diameter and the pattern of the β for preparing-type plumbic oxide nano particle can be controlled, and have higher specific surface area.
Above-mentioned purpose is achieved by the following technical solution: be raw material with the lead nitrate, with certain density aqueous sodium hydroxide solution as reaction medium, adopt hydrothermal method, under lower temperature condition, by adding proper amount of oxidant and additive, prepare β of the present invention-type plumbic oxide nano particle in a large number.Particularly, comprise the steps:
(1) 0.1～0.5 gram lead nitrate is dissolved in the sodium hydroxide solution of 30～50 milliliters of 1M, obtains mixed solution I;
(2) in mixed solution I, add 0.1～0.3 gram additive and 0.3～0.8 gram oxygenant successively, obtain mixed solution I I;
(3) mixed solution I I is packed in the encloses container, water-bath 6～24 hours (preferred 8～16 hours) is cooled to room temperature again between 80 ℃～180 ℃ (preferred 90 ℃～150 ℃), obtains mixed solution I II;
(4) with mixed solution I II centrifugal 10min under the rotating speed of 1500r/min, separate the solid obtain, use a large amount of aqueous ethanolic solution rinsings 3 times again, 50 ℃ of vacuum-drying 2 hours, the powder that obtains is β-type plumbic oxide nano particle;
Additive in the described step (2) is Sodium dodecylbenzene sulfonate, polyoxyethylene glycol, polyacrylic acid, any one in the cetyl trimethylammonium bromide.
Oxygenant in the described step (2) is any one in Sodium Persulfate, Potassium Persulphate, the ammonium persulphate.
The cost of the inventive method is inexpensive, production technique greatly obtains simplifying, the additive that adds can be adsorbed on the surface of nano particle, particulate growth and reunion have been hindered, realized the controlled of nano particle diameter and pattern, the plumbic oxide nano particle for preparing has bigger specific surface area, higher transformation efficiency and catalytic activity, thereby in electrochemical field and catalytic field, have the wide industrial purposes.
Description of drawings
Fig. 1 is the microscopic appearance picture under the Electronic Speculum (SEM) of β-type plumbic oxide nano particle of embodiment 1 scans.
Fig. 2 is the microscopic appearance picture under the Electronic Speculum (SEM) of β-type plumbic oxide nano particle of embodiment 2 scans.
Fig. 3 is the microscopic appearance picture under the Electronic Speculum (SEM) of β-type plumbic oxide nano particle of embodiment 3 scans.
Embodiment
Below further describe the present invention by embodiment, as known by the technical knowledge, the present invention also can describe by other the scheme that does not break away from the technology of the present invention feature, thus all within the scope of the present invention or the change that is equal in the scope of the invention all be included in the invention.
Embodiment 1:
The lead nitrate of getting 0.4979g is dissolved in the sodium hydroxide solution of 50 milliliters of 1M, stir and add 0.3g Sodium dodecylbenzene sulfonate and 0.5406g Sodium Persulfate down successively, in closed reactor in 80 ℃ of water-baths 6 hours, be cooled to after the room temperature above-mentioned reaction product under the rotating speed of 1500r/min centrifugal 10 minutes, separate the solid that obtains, use a large amount of aqueous ethanolic solution rinsings 3 times again, 50 ℃ of vacuum-drying 2 hours, the gained powder is the plumbic oxide nano particle.
Product to present embodiment carries out electron-microscope scanning to observe its microscopic appearance, and gained SEM picture as shown in Figure 1.
Embodiment 2:
The lead nitrate of getting 0.4979g is dissolved in the sodium hydroxide solution of 50 milliliters of 1M, stir and add 0.15g polyoxyethylene glycol and 0.5406g Potassium Persulphate down successively, in closed reactor in 130 ℃ of water-baths 18 hours, be cooled to after the room temperature above-mentioned reaction product under the rotating speed of 1500r/min centrifugal 10 minutes, separate the solid that obtains, use a large amount of aqueous ethanolic solution rinsings 3 times again, 50 ℃ of vacuum-drying 2 hours, the gained powder is the plumbic oxide nano particle.
Product to present embodiment carries out electron-microscope scanning to observe its microscopic appearance, and gained SEM picture as shown in Figure 2.
Embodiment 3:
The lead nitrate of getting 0.2650g is dissolved in the sodium hydroxide solution of 40 milliliters of 1M, stir and add 0.02g polyvinylpyrrolidone and 0.3651g ammonium persulphate down successively, in closed reactor in 180 ℃ of water-baths 24 hours, be cooled to after the room temperature above-mentioned reaction product under the rotating speed of 1500r/min centrifugal 10 minutes, separate the solid that obtains, use a large amount of aqueous ethanolic solution rinsings 3 times again, 50 ℃ of vacuum-drying 2 hours, the gained powder is the plumbic oxide nano particle.
Product to present embodiment carries out electron-microscope scanning to observe its microscopic appearance, and gained SEM picture as shown in Figure 3.
Claims (4)
1. the preparation method of β-type plumbic oxide nano particle is characterized in that, comprises the steps:
(1) 0.1～0.5 gram lead nitrate is dissolved in the sodium hydroxide solution of 30～50 milliliters of 1M, obtains mixed solution I;
(2) in mixed solution I, add 0.1～0.3 gram additive and 0.3～0.8 gram oxygenant successively, obtain mixed solution I I;
(3) mixed solution I I is packed in the encloses container, water-bath is 6～24 hours between 80 ℃～180 ℃, is cooled to room temperature again, obtains mixed solution I II;
(4) with mixed solution I II centrifugal 10min under the rotating speed of 1500r/min, separate the solid obtain, use a large amount of aqueous ethanolic solution rinsings 3 times again, 50 ℃ of vacuum-drying 2 hours, the powder that obtains is β-type plumbic oxide nano particle;
Additive in the described step (2) is Sodium dodecylbenzene sulfonate, polyoxyethylene glycol, polyacrylic acid, any one in the cetyl trimethylammonium bromide;
Oxygenant in the described step (2) is any one in Sodium Persulfate, Potassium Persulphate, the ammonium persulphate.
2. according to the preparation method of the described β of claim 1-type plumbic oxide nano particle, it is characterized in that the water-bath temperature of described step (3) is 90 ℃～150 ℃.
3. according to the preparation method of the described β of claim 1-type plumbic oxide nano particle, it is characterized in that the water-bath time of described step (3) is 8～16 hours.
4. the β for preparing according to the described method of claim 1-type plumbic oxide nano particle.
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| CN2009101810999A CN101712487B (en) | 2009-10-29 | 2009-10-29 | Method for preparing beta-type lead dioxide nanometer particles |
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| CN2009101810999A CN101712487B (en) | 2009-10-29 | 2009-10-29 | Method for preparing beta-type lead dioxide nanometer particles |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747227A (en) * | 2012-06-18 | 2012-10-24 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
| CN111097402A (en) * | 2019-12-26 | 2020-05-05 | 浙江工业大学 | Nano β -lead dioxide catalyst, and preparation method and application thereof |
| CN111889098A (en) * | 2020-08-05 | 2020-11-06 | 浙江工业大学 | Beta-lead dioxide catalyst with different morphologies as well as preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438171A (en) * | 2002-12-26 | 2003-08-27 | 东北师范大学 | Controllable preparation method of amphoteric metal oxide nano-bar |
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2009
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747227A (en) * | 2012-06-18 | 2012-10-24 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
| CN111097402A (en) * | 2019-12-26 | 2020-05-05 | 浙江工业大学 | Nano β -lead dioxide catalyst, and preparation method and application thereof |
| CN111097402B (en) * | 2019-12-26 | 2022-10-04 | 浙江工业大学 | Nano beta-lead dioxide catalyst, preparation method and application thereof |
| CN111889098A (en) * | 2020-08-05 | 2020-11-06 | 浙江工业大学 | Beta-lead dioxide catalyst with different morphologies as well as preparation method and application thereof |
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| CN101712487B (en) | 2012-07-11 |
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