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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

Inactive Publication Date: 2014-05-14
NORTHWEST A & F UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 1) In the traditional emulsion polymerization method, the demand for surfactant is large, the process is cumbersome, the energy consumption is high, and the efficiency is low;

Method used

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  • Method for preparing polymer nanospheres and nanorods by virtue of ultrasonic-assisted soap-free click polymerization reaction
  • Method for preparing polymer nanospheres and nanorods by virtue of ultrasonic-assisted soap-free click polymerization reaction
  • Method for preparing polymer nanospheres and nanorods by virtue of ultrasonic-assisted soap-free click polymerization reaction

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a new method for preparing shape-controllable high polymer nanospheres and nanorods by virtue of an ultrasonic-assisted soap-free click polymerization reaction. The method comprises the following steps: dissolving a certain amount of acetenyl pyridine and polyazido crosslinking agent in a proper solvent; with Cu(PPh3)3Br as a catalyst, performing click polymerization by controlling the ultrasonic frequency and reaction temperature to obtain polymer nanospheres or nanorods with clickable functional group on the surface. According to the method disclosed by the invention, the polymer nanospheres and nanorods are prepared by virtue of ultrasonic-assisted click polymerization, a surfactant is not required in the polymerization process, and the process is environment-friendly; the shape of the prepared polymer nanoparticles can be selectively controlled by changing the solvent system and the ultrasonic assist mode; meanwhile, with clickable azido and alkynyl on the surfaces of nanoparticles, further functionalization is facilitated, and the method has broad application prospect in the fields of new material preparation, drug delivery, fluorescence imaging and the like.

Description

technical field [0001] The invention belongs to the technical field of synthesis of polymer nanospheres and nanorods, and in particular relates to a new method for preparing polymer nanospheres and nanorods through ultrasonic-assisted soap-free click polymerization. Background technique [0002] The synthesis of nanospheres and nanorods with controllable morphology has attracted the attention of many researchers. On the one hand, it is due to the characteristics of nanostructures in electricity, light, and magnetism; Potential applications in needles, optoelectronic materials. So far, the most commonly used method for synthesizing polymer nanoparticles is still emulsion polymerization, which has the following problems to be solved urgently: [0003] 1) Traditional emulsion polymerization requires a large amount of surfactants, and surfactants are not only expensive, but also require high energy consumption and time-consuming post-processing, and it is especially important t...

Claims

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Application Information

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IPC IPC(8): C08G73/06B82Y40/00
Inventor 裴玉新侯勇裴志超操守鹏王林王贝贝
Owner NORTHWEST A & F UNIV
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