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Temperature-sensitive polymer/gold nanoparticle hybrid microspheres and preparation method thereof

A technology of gold nanoparticles and hybrid microspheres, applied in the field of polymer/gold nanoparticle hybrid smart microspheres and their preparation, can solve the problems of easy detachment, non-adjustment and loss of gold nanoparticles, and achieve high catalytic reaction Activity, broad application prospects, convenient adjustment effect

Inactive Publication Date: 2012-06-13
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the binding strength of the existing hybrid polymer microspheres to the gold nanoparticles is not high, the gold nanoparticles are easy to fall off and run off, and the catalytic activity decreases rapidly and cannot be adjusted.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1). The preparation of the chain transfer agent (MCEDB): under the protection of nitrogen, the magnesium bar of (1.10g, 0.046mol), the dry THF of 40mL and the iodine of catalytic amount are added in the 100mL three-neck round-bottomed flask, cold water Under a nitrogen bath environment, a THF solution of bromobenzene (THF 20 mL, bromobenzene 7.85 g, 0.05 mol) was added dropwise to the reaction mixture, 2-3 drops per second, and the dropwise addition was completed after 15 minutes. The reaction temperature was controlled at 40° C. until the magnesium strips completely disappeared, and the reaction solution turned off-white at this time. Then add CS dropwise 2 (3.81g, 0.05mol, the solution turned red gradually, after the dropwise addition was completed, at 40°C, the reaction was continued for 4h. Then methyl 2-chloropropionate (5.51g, 0.045mol) was added dropwise to the reaction solution, and the reaction Stir and reflux at 90°C for 60h. Cool down to 5°C and add 100mL o...

Embodiment 2

[0023] (1). With embodiment 1;

[0024](2). N-isopropylacrylamide (NIPAM) (5g, 0.045mol), 2-(methoxycarbonyl)-ethyl dithiophenyl ester (MCEDB) (84.9mg, 0.35mmol), even Azobisisobutyronitrile (AIBN) (5.81 mg, 0.035 mmol) was added to the sealed tube and dissolved with 16 mL of 1,4-dioxane. Freeze in liquid nitrogen, vacuumize, fill with nitrogen to dissolve, repeat 3 times, and finally seal the tube. Electromagnetic stirring, react at 70°C for 24 hours, cool with ice water and open to the atmosphere to terminate the reaction, concentrate the polymer solution to about 5 mL, precipitate in a large amount of anhydrous ether (500 mL), remove the monomer and solvent, and wash the precipitate with anhydrous ether for 3 times, vacuum dried for two days to constant weight;

[0025] (3). With embodiment 1;

[0026] (4). With embodiment 1.

Embodiment 3

[0028] (1). With embodiment 1;

[0029] (2). N-isopropylacrylamide (NIPAM) (10g, 0.089mol), 2-(methoxycarbonyl)-ethyl dithiophenyl ester (MCEDB) (84.9mg, 0.35mmol), even Azobisisobutyronitrile (AIBN) (5.81 mg, 0.035 mmol) was added to the sealed tube and dissolved with 16 mL of 1,4-dioxane. Freeze in liquid nitrogen, vacuumize, fill with nitrogen to dissolve, repeat 3 times, and finally seal the tube. Electromagnetic stirring, react at 70°C for 10 h, cool with ice water and open to the atmosphere to terminate the reaction, concentrate the polymer solution to about 5 mL, precipitate in a large amount of anhydrous ether (500 mL), remove monomer and solvent, and wash the precipitate with anhydrous ether for 3 times, vacuum dried for two days to constant weight;

[0030] (3). With embodiment 1;

[0031] (4). With embodiment 1.

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Abstract

The invention relates to temperature-sensitive polymer / gold nanoparticle hybrid microspheres and a preparation method thereof. The temperature-sensitive polymer / gold nanoparticle hybrid microspheres consist of more than 99.9 weight percent of polymer and less than 0.1 weight percent of gold nanoparticles. The preparation method comprises the following steps of: a) preparing a 2-(methoxycarbonyl)-ethyldithiophenyl ester chain transfer agent; b) synthesizing an N-isopropylacrylamide macromolecular chain transfer agent by using 2-(methoxycarbonyl)-ethyldithiophenyl ester obtained in step a) and azodiisobutyronitrile; c) further polymerizing 4-vinylpyridine by using the macromolecular chain transfer agent obtained in step b) and the azodiisobutyronitrile to obtain a block copolymer; d) preparing polymer microsphere suspension by using the block copolymer obtained in step (c); and e) adding chloroauric acid into the microsphere suspension, and reducing by using excessive sodium borohydride to obtain the temperature-sensitive hybrid polymer microspheres. The temperature-sensitive polymer / gold nanoparticle hybrid microspheres overcome the disadvantages that the gold nanoparticles are not firmly combined and are easy to fall off and the catalytic activity is not adjustable, and can be used for the fields of controllable catalysis and the like.

Description

technical field [0001] The invention belongs to the field of polymer science and technology, in particular to a polymer / gold nanoparticle hybrid intelligent microsphere and a preparation method thereof. Background technique [0002] Gold nanoparticles have unique stability related to size, small size effect, quantum effect, surface effect and biological affinity. As a good classical nanomaterial, it is a research hotspot in optics, electronics, catalysis and biomedicine. Ideal gold nanomaterials or composite materials require gold nanoparticles with limited size and shape, modified organic and / or biomolecules on the surface, special composite structures (such as core-shell structure) and the ability to be in 2-D or 3D. Ordered arrangements in -D space or devices, which often have different properties than individual particles and macroscopic entities. Therefore, it is a research trend in this field to synthesize gold nanoparticle carriers with special structures and develo...

Claims

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Application Information

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IPC IPC(8): C08L53/00C08K3/08C08F293/00C08F2/38B01J31/26
Inventor 陈熙陈莉史丛丛赵义平陈明星王泽亚
Owner TIANJIN POLYTECHNIC UNIV
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