Preparation methods of cyclodextrin-based star-block polymer and cyclodextrin-based star-block polymer/gold nano-rod composite material

A technology of block polymer and cyclodextrin, which is applied in the field of preparation of cyclodextrin-based star-shaped block polymer and cyclodextrin-based star-shaped block polymer/gold nanorod composite material. The effect of controllable shape, clear structure and simple synthesis route

Active Publication Date: 2013-07-31
ANKANGDEMEI ZHONGSHAN NANO TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large number of studies have shown that the preparation of specific morphology and monodisperse gold nanoparticles is still a challenging task

Method used

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  • Preparation methods of cyclodextrin-based star-block polymer and cyclodextrin-based star-block polymer/gold nano-rod composite material
  • Preparation methods of cyclodextrin-based star-block polymer and cyclodextrin-based star-block polymer/gold nano-rod composite material
  • Preparation methods of cyclodextrin-based star-block polymer and cyclodextrin-based star-block polymer/gold nano-rod composite material

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preparation example Construction

[0028] A preparation method of cyclodextrin-based star block polymer, comprising the following steps:

[0029] 1) Combine β-cyclodextrin, P 2 S 5 , p-methoxybenzoic acid three in K 2 CO 3 Reflux reaction in the organic solvent DMF for 16-18h in the presence and anaerobic conditions, purify the obtained product to obtain dithioester, and obtain RAFT polymer chain transfer agent (CD-CTA);

[0030] 2) Mix the RAFT polymer chain transfer agent prepared in the previous step, methyl methacrylate, and functional monomers, and carry out living free radical polymerization in the solvent DMF in the presence of free radical initiators and under anaerobic conditions, and ice-water bath Cooling stops the polymerization, and the resulting product is purified and separated;

[0031] 3) The product obtained in the above steps is used as a macromolecular chain transfer agent. In the presence of a free radical initiator and under oxygen-free conditions, the hydrophilic monomer and the macro...

Embodiment 1

[0040] Example 1: Synthesis of RAFT polymeric chain transfer agent (CD-CTA):

[0041] Into a 250 ml three-necked bottle, add metered 10mmol β-CD (ie β-cyclodextrin), 70mL DMF, 30mmol P 2 S 5 , 1.5g K 2 CO 3 And 30mmol of p-methoxybenzoic acid, passed through Ar and stirred for 15 minutes, then refluxed for 16 hours, and finally a reddish-brown suspension was obtained. Wash with deionized water (3*50mL), extract with ethyl acetate (2*30mL), spin dry and pass through a silica gel column. The mobile phase used is a mixture of petroleum ether:ethyl acetate (volume ratio)=20:1 , collect the orange-red fraction, and recrystallize from ethyl acetate to obtain the orange-red solid product CD-CTA, with a yield of 30%. FI-IR: 1069.5cm -1 (S=C-S-), 1390~1560 cm -1 (-C 6 h 4 -); H-NMR: 7.01~7.53 (-C 6 h 4 -); 2.75~3.60 (β-CD). like figure 1 Infrared spectrum of the RAFT polymeric chain transfer agent (CD-CTA) synthesized in this example.

Embodiment 2

[0042] Embodiment 2: the synthesis of star block copolymer

[0043] CD-[P(A-co-B)] n Synthesis: A is methyl methacrylate, B is hydroxyethyl acrylate

[0044] According to the molar ratio of Monomer(A+B):CD-CTA:AIBN=1000:5:1 (A:B=6:1, molar ratio), DMF (10~15ml) was used as solvent, argon gas was passed for 15min, and then Vacuum degassing, vacuum fusion sealing after 3 cycles. React under magnetic stirring at 80°C for 12 hours, then cool in an ice-water bath to stop polymerization, use methanol as a precipitant, dissolve with DMF after suction filtration, dissolve-precipitate twice, and then dialyze for 72 hours with a dialysis bag with a molecular weight cut-off of 7000Da. After vacuum drying, light yellow solid CD-[P(A-co-B)] was obtained n .

[0045] CD-[P(A-co-B-b-C)] n Synthesis of: the C monomer described below is N-hydroxypropyl acrylamide;

[0046] CD-[P(A-co-B)] synthesized above n It is a macromolecular chain transfer agent (Macro-CTA) with a molar ratio of Mo...

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Abstract

The invention discloses a preparation method of a cyclodextrin-based star-block polymer. The method comprises the steps that: (1) beta-cyclodextrin, P2S5, and p-methoxybenzoic acid are subjected to a sufficient reflux reaction under an alkaline and anaerobic condition in an organic solvent; the obtained product is purified, such that a RAFT polymerization chain-transfer agent is obtained; (2) the prepared RAFT polymerization chain-transfer agent, methyl methacrylate, and a functional monomer are mixed; the mixture is subjected to a polymerization reaction under the existence of a free radical initiator and an anaerobic condition in a solvent; polymerization is stopped, and the obtained product is purified and separated; and (3) the obtained product is adopted as a macromolecular chain-transfer agent; a hydrophilic monomer and the macromolecular chain-transfer agent are subjected to a polymerization reaction in a solvent under the existence of a free radical initiator and an anaerobic condition; polymerization is stopped by ice-water bath cooling; the obtained product is purified and separated; and the product is reduced by using a reducing agent. The synthesis route provided by the invention is simple. The star-block polymer has a clear structure. The particle size and morphology of the nano-gold are controllable.

Description

technical field [0001] The invention relates to a preparation method of a cyclodextrin-based star-shaped block polymer and a cyclodextrin-based star-shaped block polymer / gold nanorod composite material. Background technique [0002] Due to the small size effect, quantum effect, surface effect and macroscopic quantum tunneling effect of nanomaterials, it shows unique properties in physics and chemistry that are completely different from traditional macroscopic materials, and has become a research hotspot in various fields such as materials science. . A large number of studies have shown that the preparation of specific morphology and monodisperse gold nanoparticles is still a challenging task. The current methods for preparing such gold nanoparticles mainly include: 1) preparation of gold nanoparticles within a limited size and shape; 2) modification of the surface of nanoparticles by organic and / or biomolecules; 3) formation of composite nanostructures, such as Spherical c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/58C08F220/14C08F220/28C08F2/38C08F8/04C08L53/00C08K3/08C08B37/16
Inventor 刘意杨帆孙福强潘育方魏木培
Owner ANKANGDEMEI ZHONGSHAN NANO TECH CO LTD
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