Nanoparticle film of fullerene derivative/palladium and its preparation method and application
A technology of fullerene derivatives and nanoparticles, applied in the nano field, can solve the problems of low catalytic activity, low reaction conversion rate, low product selectivity, etc., achieve uniform particle size distribution, good promotion effect, and improve catalytic activity. low effect
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Embodiment 1
[0028] Example 1 Synthesis of Fullerene Derivatives
[0029] Add 5.55g (5mL, 42mmol) phenylallyl aldehyde and 22.5mL acetic anhydride into the three-necked flask, add 1.5mL concentrated nitric acid and 5.0mL acetic acid to the dropping funnel, magnetically stir, cool the three-necked flask with an ice-salt bath When the temperature drops to 0-5°C, slowly add concentrated nitric acid-acetic acid mixture dropwise under magnetic stirring. The temperature is controlled below 5°C and the addition is completed within 30 minutes. Then warm to room temperature, stand for 48h, add dropwise 20% dilute hydrochloric acid solution until needle-like yellow crystals are precipitated, and recrystallize with 95% ethanol to obtain 3.4g of light yellow crystals, namely 3-(2-nitrophenyl) ) Allyl aldehyde, the yield is 46.0%, and the melting point is 126-128°C.
[0030]
[0031] Take 720mg C 60 Dissolve in freshly steamed 800mL toluene, magnetically stir for 1.5h under the protection of argon to make ...
Embodiment 2A
[0036] Example 2A Preparation of Fullerene Derivative Nanoparticles by Solvent Method
[0037] The fullerene derivative of Example 1 was dissolved in toluene to prepare a toluene solution of 1g / L fullerene derivative, and then the toluene solution and propanol were mixed in a volume ratio of 1:10, and then stirred at room temperature 2h to obtain a nano-suspension of fullerene derivatives. The nano suspension was centrifuged at a rotation speed of 5000 r / min, and the centrifugation time was 10 min; then the separated solid was washed with an ethanol aqueous solution to obtain fullerene derivative nanoparticles, and dried at room temperature.
[0038] Through SEM and TEM electron microscopy analysis, it can be found that the prepared fullerene derivative nanoparticles are basically spherical. In addition, a laser particle size analyzer was used to determine the D of fullerene derivative nanoparticles 90 The diameter is 68nm.
Embodiment 2B
[0039] Example 2B Preparation of Fullerene Derivative Nanoparticles by Solvent Method
[0040] The fullerene derivative of Example 1 was dissolved in chloroform to prepare a toluene solution of 10g / L fullerene derivative, and then the chloroform solution was mixed with isopropanol in a volume ratio of 1:5 Then, it was stirred at room temperature for 6 hours to obtain a nano-suspension of the fullerene derivative. The nano suspension was centrifuged at a rotation speed of 5000 r / min, and the centrifugation time was 15 min; then, the separated solid was washed with an aqueous ethanol solution to obtain fullerene derivative nanoparticles, and dried at room temperature.
[0041] Through SEM and TEM electron microscope analysis, it can be found that the prepared fullerene derivative nanoparticles are basically spherical. In addition, a laser particle size analyzer was used to determine the D of fullerene derivative nanoparticles 90 The diameter is 62nm.
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