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Alkoxy ethers temperature-sensitive polymer nanometer microsphere and preparation method thereof

A technology of nano-microspheres and alkoxy ethers, which is applied in the field of alkoxy-ether thermosensitive polymer nano-microspheres and their preparation, and achieves the effects of rapid phase change process, small hysteresis and excellent temperature-sensitive performance.

Inactive Publication Date: 2015-08-26
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The work of preparing temperature-sensitive and controllable nanospheres by cross-linking alkoxyether thermosensitive polymers through dynamic bonds in aqueous solution has not been reported.

Method used

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  • Alkoxy ethers temperature-sensitive polymer nanometer microsphere and preparation method thereof
  • Alkoxy ethers temperature-sensitive polymer nanometer microsphere and preparation method thereof
  • Alkoxy ethers temperature-sensitive polymer nanometer microsphere and preparation method thereof

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Experimental program
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Embodiment 1

[0030] Embodiment one: the synthesis of monomer

[0031] (a) The first-generation alkoxyether dendron (G1-CH 2 OH), 1.5 equivalents of p-alkynylbenzoic acid, 0.2 equivalents of N,N-diisopropylethylamine (DIEA) were dissolved in DCM, 1.2 equivalents of EDC·HCl was added in an ice-salt bath under nitrogen protection, and stirring was continued at room temperature until the reaction was complete; after washing with saturated brine, the aqueous phase was extracted with DCM, anhydrous MgSO 4 The organic phase was dried and spin-dried in DCM, and the crude product was purified by column chromatography with DCM to obtain a monomer containing a dendron unit.

[0032] (b) Polymer Poly(Pa-G1-R- co -Pa-CHO) synthesis

[0033] Dissolve the phenylacetylene monomer containing dendrons and p-aldehyde phenylacetylene in a certain proportion in a small amount of THF, and add 1 / 50 equivalent of [Rd(nbd)Cl] under nitrogen protection 2 , Triethylamine (TEA) 1 drop. The reaction was carried ...

Embodiment 2

[0036] The temperature-sensitive behavior of the nano-microspheres was characterized by ultraviolet spectroscopy. as attached figure 2 As shown, the nanospheres at room temperature (25 o C) The light transmittance is higher, 70%, indicating that the solubility and dispersion of the nanospheres in water are better. As the temperature rises slowly to about the phase transition temperature (31.5°C), the light transmittance of the aqueous nanosphere solution drops rapidly. When the temperature rises above the phase transition temperature (35°C), the transmittance is lower than 10%. It shows that the nano-microsphere has excellent temperature-sensitive behavior.

Embodiment 3

[0038] The size of the nanospheres in aqueous solution was characterized by dynamic light scattering. As shown in Table 1, at room temperature (20°C), the size radius of the nanospheres can reach more than 1100nm, and its polydispersity index is 0.491; when the temperature rises above the phase transition temperature (40°C), its size radius is less than 1000nm, its polydispersity index is 4.56, which shows that the size of the smart nanosphere changes with the change of temperature, and it is more stable at room temperature, and its radius distribution is more uniform.

[0039] Table 1. Dynamic light scattering diagram of smart nanospheres.

[0040] Radius (nm) polydispersity index 20℃ 1166.28 0.491 40℃ 803.56 4.56

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Abstract

The invention discloses an alkoxy ethers temperature-sensitive polymer nanometer microsphere and a preparation method thereof. The method includes the steps of first catalyzing two monomers for copolymerization through rhodium metal to obtain a temperature-sensitive polymer; dissolving the polymer in an acidic aqueous solution, and adding a corresponding cross-linking agent to obtain the intelligent nanometer microsphere. The nanometer microsphere has good dispersibility in an aqueous solution and shows good temperature-sensitive behavior. The size of the nanometer microsphere can be reversibly regulated through external temperature stimuli. The alkoxy ethers temperature-sensitive polymer nanometer microsphere and the preparation method thereof provide a theoretical basis for the construction of the nanometer microsphere through a dynamic keys crosslinked temperature-sensitive polymer, have an important academic value in the preparation of novel intelligent nanometer materials and are instructive for the expansion of the application of the stimulus responsive temperature-sensitive polymer in the fields of materials science, drug sustained release and envelope.

Description

technical field [0001] The invention relates to an intelligent nano-microsphere and a preparation method thereof, in particular to an alkoxy ether-based temperature-sensitive polymer nano-microsphere and a preparation method thereof. Background technique [0002] Designing and synthesizing nano-microspheres with different sizes and making them intelligent has important research value in the preparation of new functional materials. Among the various nanosphere preparation methods that have been reported, the construction of various nanomaterials from polymers has attracted widespread attention. As a kind of non-covalent bond, dynamic bond has become an important research direction because of its advantages such as reversibility and easy regulation. Thermosensitive polymers, as an important class of smart polymers, have attracted widespread attention due to their easy manipulation, non-pollution and wide range of applications. This type of polymer usually has a minimum criti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F238/00C08J3/24C07C69/76C07C67/08A61K47/32
Inventor 张阿方武方刘芸丽许安球陶雄刘坤
Owner SHANGHAI UNIV
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