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Method for preparing environmentally responsive monodisperse cyclodextrin polymer hollow microspheres

A cyclodextrin polymer, environment-responsive technology, which is applied in the field of preparation of monodisperse cyclodextrin polymer hollow microspheres, achieves the effects of increasing permeability and simple post-processing process

Inactive Publication Date: 2013-03-13
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to avoid the deficiencies of the prior art, the present invention proposes a preparation method of monodisperse cyclodextrin polymer hollow microspheres with environmental responsiveness, which solves the existing "self-removable template" technology to prepare hollow microspheres. question

Method used

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  • Method for preparing environmentally responsive monodisperse cyclodextrin polymer hollow microspheres
  • Method for preparing environmentally responsive monodisperse cyclodextrin polymer hollow microspheres
  • Method for preparing environmentally responsive monodisperse cyclodextrin polymer hollow microspheres

Examples

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Embodiment 1

[0035] Example 1: Prepare 50 mL of N-isopropylacrylamide aqueous solution with a concentration of 10 g / L, add 30 mg of methacrylic acid to it, pour the mixed solution into a 100 mL round bottom flask, and place it in an oil bath at 60°C for magnetic stirring At the same time, nitrogen gas was introduced, and after 20 minutes, 2 mL of potassium persulfate aqueous solution with a concentration of 4 mg / mL was added to the solution with a syringe. 2mL aqueous solution of sodium dialkylbenzene sulfonate, and then add 2mL aqueous solution of monovinylcyclodextrin with a concentration of 0.08g / mL and 2mL aqueous solution of cross-linking agent N,N-methylenebisacrylamide (concentration: 10mg / mL), polymerized at 60°C, N 2 Under atmosphere for 10h. After the reaction, stir and cool to room temperature, adjust the pH value of the solution to 9.4 with 1:1 diluted ammonia water under the monitoring of the pH meter, stir at room temperature for 4 hours, and then put the sample into a dial...

Embodiment 2

[0036] Example 2: Prepare 50 mL of N-isopropylacrylamide aqueous solution with a concentration of 20 g / L, add 100 mg of ethacrylic acid to it, pour the mixed solution into a 100 mL round bottom flask, and place it in an oil bath at 80°C for magnetic stirring At the same time, nitrogen gas was introduced, and after 20 minutes, 2 mL of azobisisobutylamidine hydrochloride (V-50) aqueous solution with a concentration of 5 mg / mL was added to the solution with a syringe. Add 2 mL of sodium lauryl sulfate aqueous solution with a concentration of 12 mg / mL to the syringe first, and then add 2 mL of polyvinyl cyclodextrin aqueous solution with a concentration of 0.15 g / mL and cross-linking agent ethylene glycol dimethacrylic acid Ester 25 μL, polymerized at 80 °C, N 2 Under the atmosphere for 8h. After the reaction, stir and cool to room temperature, adjust the pH value of the solution to 10.0 with 1:1 diluted ammonia water under the monitoring of the pH meter, stir at room temperature...

Embodiment 3

[0037] Example 3: Prepare 50 mL of N-isopropylacrylamide aqueous solution with a concentration of 15 g / L, add 60 mg of maleic anhydride to it, pour the mixed solution into a 100 mL round bottom flask, and place it in an oil bath at 70°C for magnetic stirring At the same time, nitrogen gas was introduced, and after 20 minutes, 2 mL of azobisisobutylamidine hydrochloride (V-50) aqueous solution with a concentration of 4.5 mg / mL was added to the solution with a syringe, and after 3 to 5 minutes, the solution appeared light blue. First add 2 mL of sodium dodecylbenzenesulfonate aqueous solution with a concentration of 10 mg / mL into it with a syringe, and then add 2 mL of polyvinyl cyclodextrin aqueous solution with a concentration of 0.15 g / mL and cross-linking agent ethylene glycol di Methacrylate 15 μL, polymerized at 70 °C, N 2 Under atmosphere for 12h. After the reaction, stir and cool to room temperature, adjust the pH value of the solution to 9.8 with 1:1 diluted ammonia wa...

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Abstract

The invention relates to a method for preparing environmentally responsive monodisperse cyclodextrin polymer hollow microspheres. In the process of preparing multi-cavity poly (N-isopropylacrylamide-cyclodextrin) hollow microspheres, the hollow microspheres are endowed with environmental responsiveness, and in the process of preparing crosslinking cores, acid monomers are added to be copolymerized with NIPAM monomers so as to obtain acidic cores; and after cyclodextrin monomers and a crosslinking agent are added into the acidic cores so as to obtain core / shell-structured microspheres, the core / shell-structured microspheres are treated by using alkali liquor, and an ionization effect generated by acid-base neutralization accelerates the collapse of cores and the swelling of crosslinking shell layers, so that the permeability of the shell layers subjected to swelling is enhanced, therefore, a situation that PNIPAM (core) chains in the shell layers quickly escape so as to obtain microspheres is facilitated, and PNIPAM and acid ingredients in the microspheres also endow the hollow microspheres with pH and temperature responsiveness. The method disclosed by the invention solves the problems existing in hollow microsphere preparation implanted by using the existing 'self-removable' technique.

Description

technical field [0001] The invention belongs to the field of functional polymer materials and relates to a method for preparing monodisperse cyclodextrin polymer hollow microspheres with environmental responsiveness. Background technique [0002] In recent years, new environment-responsive polymer hollow microspheres have potential application value in the fields of drug loading and controlled release, and the loading of active macromolecules such as proteins, enzymes, and DNA, and have become a subject of much concern in the field of materials. [0003] Poly(N-isopropylacrylamide) (PNIPAM) is the most studied environment-responsive polymer. It will undergo a microphase transition at about 32 °C due to the destruction of the hydrogen bond between its own amide group and water. Rapidly changing from hydrophilic to hydrophobic, this temperature is called its lowest critical solution temperature (LCST). [0004] Cyclodextrin (Cyclodextrin, referred to as CD) is formed by the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/10C08F220/54C08F220/06C08F220/04C08F222/06C08J9/26
Inventor 田威张卫红刘婷婷
Owner NORTHWESTERN POLYTECHNICAL UNIV
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