A pd/sio 2 @al 2 o 3 Nanocrystalline material and its preparation method and application
A nanocrystalline material and nanocrystalline technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, fuels, etc., can solve problems such as restrictions on popularization and application, achieve good application prospects, and improve high-temperature catalysis Effect of Reaction Thermal Stability
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[0073] The present invention also provides a Pd / SiO 2 @Al 2 o 3 The preparation method of nanocrystalline material comprises the following steps:
[0074]A) After mixing polyvinylpyrrolidone, reducing agent, auxiliary agent, nano-silica, water and palladium source compound for reaction, Pd / SiO is obtained 2 Nanocrystalline;
[0075] B) Pd / SiO obtained by combining trimethylaluminum and water in the above steps 2 After deposition on the nanocrystalline surface, Al 2 o 3 Coated Pd / SiO 2 nanocrystalline materials;
[0076] C) the Al obtained by the above steps 2 o 3 Coated Pd / SiO 2 After the nanocrystalline materials were heat-treated in oxidizing and reducing atmospheres, Pd / SiO 2 @Al 2 o 3 nanocrystalline material.
[0077] The present invention is to Al in the above-mentioned preparation method 2 o 3 Coated Pd / SiO 2 The selection and requirements of nanocrystalline materials, as well as the corresponding optimization principles, are similar to those of the afo...
Embodiment 1
[0126] Cubic Pd{100} / SiO 2 Synthesis of Nanocrystals
[0127] Take 105mg of polyvinylpyrrolidone (Mw=55000), 60mg of ascorbic acid, 75mg of KBr, and 141mg of KCl and dissolve them in 7ml of ultrapure water in a single-necked flask with a capacity of 25ml, keep the temperature in an oil bath at 80°C for 10min, and then add 1ml of SiO 2 Suspension (150mg / ml) was kept at constant temperature for 5 minutes, and 3ml of 65mmol / L Na was added again 2 PdCl 4 The aqueous solution reacted for 3h. Finally, centrifuge washing and vacuum drying at room temperature for 24 hours, and then the three-dimensional Pd{100} / SiO with PVP protective agent on the surface was obtained. 2 Nanocrystalline.
[0128] The cubic Pd{100} prepared in Example 1 of the present invention was characterized.
[0129] see figure 1 , figure 1 TEM image of cubic Pd nanocrystals prepared in Example 1 of the present invention.
[0130] Depend on figure 1 It can be seen that the present invention prepares cubic...
Embodiment 2
[0136] Octahedral Pd{111} / SiO 2 Synthesis of Nanocrystals
[0137] Take 105mg of polyvinylpyrrolidone (Mw=55000), 180mg of citric acid, and 3ml of ethanol and dissolve them in 4ml of ultrapure water in a single-necked flask with a capacity of 25ml, keep the temperature in an oil bath at 80°C for 10min, and then add 1ml of SiO 2 The suspension (150mg / ml) was kept at a constant temperature for 5min, and 3ml of 65mmol / L Na was added again 2 PdCl 4 The aqueous solution reacted for 3h. Finally, centrifuge washing and vacuum drying at room temperature for 24 hours, and then the octahedral Pd{111} / SiO with PVP protective agent on the surface was obtained. 2 Nanocrystalline.
[0138] The octahedral Pd{100} prepared in Example 2 of the present invention was characterized.
[0139] see Figure 4 , Figure 4 TEM image of the octahedral Pd nanocrystals prepared in Example 2 of the present invention.
[0140] Depend on Figure 4 It can be seen that the present invention prepares o...
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