Method for preparing polymer nanospheres and nanorods by virtue of ultrasonic-assisted soap-free click polymerization reaction
A click polymerization and ultrasonic technology, applied in the direction of nanotechnology, can solve the problems of large demand for surfactants, cumbersome processes, high energy consumption, etc., and achieve the effects of avoiding the use of surfactants, broad social prospects, and huge economic benefits
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Embodiment 1
[0080] Embodiment 1: the preparation of polymer nanosphere
[0081] Take 9.5 mg (75.0 μmol) of 3,5-diethynpyridine and 19.1 mg (50.0 μmol) of B 2 Dissolve in 2.4mL of dry acetonitrile, fill with argon gas protection, and then put the argon-protected reaction bottle into an ultrasonic water bath. The temperature of the ultrasonic water bath is controlled within the range of 11°C to 14°C.
[0082] 10.3 mg (11.0 μmol) of catalyst Cu (PPh 3 ) 3 Br was dissolved in 100 μL of chloroform and injected into the reaction system. During the entire polymerization process, the ultrasonic frequency and action time were cycled at 45kHz (5s)-80kHz (5s)-100kHz (20s), and the reaction was stopped after 3 hours.
[0083] The obtained yellow emulsion was centrifuged at high speed (16500rpm), the supernatant was discarded, the precipitate was washed three times with chloroform, dried, and the polymer nanospheres were collected ( image 3 ). The apparent average particle diameter is about 553n...
Embodiment 2
[0084] Embodiment 2: the preparation of polymer nanosphere
[0085] Take 95.3mg (0.75mmol) of 3,5-diethynpyridine and 191mg (0.50mmol) of B 2 Dissolve in 24mL of dry acetonitrile, fill with argon for protection, and then put the reaction bottle into an ultrasonic water bath.
[0086] During the whole polymerization process, the ultrasonic frequency and action time are cycled at 45kHz (5s)-80kHz (5s)-100kHz (20s). The temperature of the water bath was controlled within the range of 11°C to 14°C. 103.0 mg (0.11 mmol) of catalyst Cu (PPh 3 ) 3 Br was dissolved in 1 mL of chloroform and injected into the reaction system, and the reaction was stopped after 3 hours of reaction. The obtained yellow emulsion was centrifuged at high speed (16500 rpm), the precipitate was washed three times with chloroform, dried, and polymer nanospheres were collected.
Embodiment 3
[0087] Embodiment 3: the preparation of polymer nanosphere
[0088] Take 9.5 mg (75.0 μmol) of 3,5-diethynpyridine and 17.6 mg (37.5 μmol) of B 3 Dissolve in 2.4mL of dry acetonitrile solvent, fill with argon for protection, and then put the reaction bottle into an ultrasonic water bath. Ultrasonic frequency is 45kHz. The temperature of the ultrasonic water bath is controlled within the range of 11°C to 14°C. 10.3 mg (11.0 μmol) of catalyst Cu (PPh 3 ) 3 Br was dissolved in 100 μL of chloroform, and then injected into the system, and the reaction was stopped after 3 hours.
[0089] The obtained yellow emulsion was centrifuged at high speed (16500rpm), the supernatant was discarded, the precipitate was washed three times with chloroform, dried, and the polymer nanospheres were collected ( Figure 4 ). The apparent average particle diameter is about 494nm, and the particle size dispersion index PDI is 0.298.
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