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Polymer/precious metal nanoparticle hybrid hollow intelligent microsphere and preparation method thereof

A technology of nanoparticles and hollow microspheres, which is applied in the field of polymer/precious metal nanoparticle hybrid smart hollow microspheres and its preparation, can solve the problems of not having a hollow structure and a single hollow sphere structure, and achieve broad application prospects Effect

Inactive Publication Date: 2010-06-02
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hybrid hollow spheres prepared by self-assembly technology are basically limited to two-block copolymers. The hollow spheres have a relatively simple structure and simple functions, because this technology requires that the block copolymer must have a suitable hydrophilic-lipophilic value, otherwise no hollow structure can be obtained by assembly (LiYT, Macromolecules.; 2007, 40, 8524)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Add 0.136g of initiator BMP, 0.075g of catalyst CuCl, 0.13g of complexing agent PMDETA and 15g of monomer tBA into the 25mL sealed tube. Vacuum and fill nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React for 8h in an oil bath at 90°C to stop the reaction. Dissolve the polymer with methylene chloride and pass through neutral Al 2 O 3 The chromatography column removes impurities such as catalysts. Precipitate in methanol and vacuum dry to obtain white solid PtBA;

[0023] 2. Add 2.75g initiator PtBA, 0.031g catalyst CuCl, and 0.067g complexing agent Me into the 25mL sealed tube. 6 TREN, a mixed solvent of methyl ethyl ketone / isopropanol with a volume ratio of 6:4 and the second monomer NIPAM. Vacuum and fill nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React for 48h in a 40°C water bath to stop the reaction. Dissolve the polymer with methylene chloride and pass through neutral Al 2 O 3 The chromatogra...

Embodiment 2

[0029] 1. Using the poly-tert-butyl acrylate homopolymer described in Example 1, add 2.75g initiator PtBA, 0.031g catalyst CuCl, and 0.067g complexing agent Me into a 25mL sealed tube. 6 TREN, 5mL DMF / H 2 O mixed solvent and 3g of the second monomer DMAEMA. Vacuum and fill nitrogen in an ice-water bath, repeat 3 times, and seal the tube under vacuum. React for 5h in a water bath at 40°C to stop the reaction. Dissolve the polymer with methylene chloride and pass through neutral Al 2 O 3 The chromatography column removes impurities such as catalysts. Repeated precipitation in methanol / water, vacuum drying to obtain pale yellow solid PtBA-b-PDMAEMA;

[0030] 2. Add 20 mL of dichloromethane, 1.5 g of PtBA-b-PDMAEMA and 1 mL of trifluoroacetic acid to a 50 mL conical flask, and stir at 20°C for 10 hours. After removing the solvent by rotary evaporation, dialysis with water, freeze-drying to obtain the hydrolyzate P(AA-co-tBA)-b-PDMAEMA.

[0031] 3. Dissolve 0.50g of the block-random ...

Embodiment 3

[0034] 1. Using the poly-tert-butyl acrylate homopolymer described in Example 1, a certain amount of 2.75g initiator PtBA, 0.031g catalyst CuCl, and 0.067g complexing agent Me were added into a 25mL sealed tube. 6 TREN, 3 mL of toluene solvent and 5 g of the second monomer 4-vinylpyridine. Vacuum and fill nitrogen in an ice water bath, repeat 3 times, and seal the tube under vacuum. The reaction was stopped for 72 hours in a 40°C water bath. Dissolve the polymer with methylene chloride and pass through neutral Al 2 O 3 The chromatography column removes impurities such as catalysts. Repeated precipitation in methanol / water, vacuum drying to obtain pale yellow solid PtBA-b-P4VP;

[0035] 2. Add 10 mL of dichloromethane, 0.5 g of PtBA-b-P4VP and 0.6 mL of trifluoroacetic acid to a 50 mL conical flask, and stir at 20°C for 3 hours. After removing the solvent by rotary evaporation, dialysis with water, freeze-drying to obtain the hydrolysis product P(AA-co-tBA)-b-P4VP.

[0036] 3. Di...

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Abstract

The invention relates to a polymer / precious metal nanoparticle hybrid hollow intelligent microsphere and a preparation method thereof. The polymer / precious metal nanoparticle hybrid hollow microsphere comprises the following components in percentage by weight: 0.001 to 0.01 percent of precious metal nanoparticles and 99.99 to 99.999 percent of polymer. The experimental results of p-nitrophenol catalytic reduction tests show that the polymer / precious metal nanoparticle hybrid hollow intelligent microsphere prepared by the method has high catalytic activity at room temperature and is adjustable in catalytic activity. The hybrid hollow intelligent microsphere having novel structural characteristics and adjustable performance is hopeful to have important application in efficient selective catalysis, biomedicine and other wide fields.

Description

Technical field [0001] The invention belongs to the field of polymer science and technology, and particularly relates to a polymer / noble metal nanoparticle hybrid smart hollow microsphere and a preparation method thereof. Background technique [0002] Noble metal nanoparticles have unique stability related to size, small size effect, quantum effect, surface effect and biological affinity. As a good classic nanomaterial, it is a research hotspot in optics, electronics, catalysis and biomedicine. Ideal noble metal nanomaterials or composite materials require noble metal nanoparticles to have a limited size and shape, have modified organic and / or biomolecules on the surface, have a special composite structure (such as a core-shell structure), and be able to perform in 2-D or 3 -D space or orderly arrangement within the device, which usually has properties different from individual particles and macroscopic entities. Therefore, it is a research trend in this field to synthesize pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02B01J35/08B01J37/02B01J23/38
Inventor 陈熙
Owner TIANJIN POLYTECHNIC UNIV
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