Method for preparing modified cyclodextrin based porous microspheres

A cyclodextrin and microsphere technology, applied in the field of polymer microsphere synthesis, can solve the problems of difficult removal of oil and other impurities in the separation process, cumbersome post-processing, complex system, etc., and achieves low production cost, versatility, separation Handling simple effects

Active Publication Date: 2018-11-27
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has defects such as complex system, cumbersome post-processing, difficult to remove impurities such as emulsifier and oil, and complicated separation process.

Method used

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  • Method for preparing modified cyclodextrin based porous microspheres
  • Method for preparing modified cyclodextrin based porous microspheres
  • Method for preparing modified cyclodextrin based porous microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Take 10g of β-cyclodextrin in a three-necked flask, add 40mL of 0.04mol / L NaOH solution, and basify with magnetic stirring in a water bath at 60°C for 0.5h; then add 24g of sodium chloroacetate, and continue to stir magnetically in a water bath at 60°C After 1 hour, use 6mol / L hydrochloric acid to adjust the pH of the solution to 7, then pour at least 5 times the volume of absolute ethanol into the solution and stir quickly until a large amount of white precipitate is produced, and then keep the solution in cold storage for 12 hours. The solution was subjected to suction filtration, and the solid obtained by suction filtration was washed with absolute ethanol and then vacuum-dried to obtain carboxymethyl-β-cyclodextrin.

[0022] (2) Take 5g of carboxymethyl-β-cyclodextrin in a beaker, add 29.12g of NaOH solution with a mass fraction of 35%, stir magnetically at 60°C until carboxymethyl-β-cyclodextrin is dissolved, and then add 6g Add polyethylene glycol 600, then ad...

Embodiment 2

[0029](1) Take 11g of β-cyclodextrin in a three-neck flask, add 45mL of 5mol / L NaOH solution, and alkalinize it with magnetic stirring in a water bath at 60°C for 0.5h; then add 31g of sodium chloroacetate, and continue stirring for 1h under a water bath at 60°C Use 6mol / L hydrochloric acid to adjust the pH of the solution to 7, then pour at least 5 times the volume of absolute ethanol into the solution and stir it quickly until a large amount of white precipitate is produced, then put the solution in a refrigerator for 12 hours, and refrigerate the processed solution Suction filtration is carried out, and the solid obtained by suction filtration is washed with absolute ethanol and then vacuum-dried to obtain carboxymethyl-β-cyclodextrin.

[0030] (2) Take 10g of carboxymethyl-β-cyclodextrin in a beaker, add 60.3g of NaOH solution with a mass fraction of 35%, stir magnetically at 60°C until carboxymethyl-β-cyclodextrin is dissolved, and then add 12g Polyethylene glycol 600, th...

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Abstract

The invention discloses a method for preparing modified cyclodextrin based porous microspheres. According to the method, water serves as a reaction medium, an initiator is not needed, an oil phase, anemulsifier and other mixed solvents are also not needed, polyethylene glycol 600 serves as a stabilizer in the reaction system and also serves as a soft segment polymer for participating in the reaction, and the stabilizer does not need to be removed during later separating treatment. Compared with the conventional dispersion copolymerization method, the microsphere preparation method provided bythe invention is less in needed raw materials and assistants, simple in preparation and separation and low in production cost. In addition, according to the microsphere preparation method provided bythe invention, carboxymethyl-beta-cyclodextrin serves as a reactive monomer, and lots of ionizable groups exist in the system, so that enough surface charge can be provided under alkaline conditions.The dispersion can be assisted by utilizing the electrostatic repulsion mechanism, the stability is provided, and the microsphere product is endowed with more functionality (such as pH sensitivity).

Description

Technical field: [0001] The invention relates to the field of synthesis of polymer microspheres, in particular to a preparation method of modified cyclodextrin-based porous microspheres. Background technique: [0002] Polymer microspheres are widely used in adsorption, separation, catalysis, and carrier applications in many fields such as environmental science, medicinal chemistry, and material chemistry because of their uniformity, regularity of structure, large specific surface area, and easy functionalization. . Among them, polymer microspheres prepared from natural polymers have attracted much attention in drug controlled release systems and adsorption carriers because of their good biocompatibility, biodegradability, no toxic and side effects, and low price. . [0003] β-cyclodextrin is an oligosaccharide composed of 7 glucose units with a cavity structure of "hydrophilic on the outside and hydrophobic on the inside". The special cavity structure makes it suitable for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08J3/12C08G81/00C08G65/28C08B37/16A61K47/69
CPCA61K47/6951C08B37/0012C08G65/2606C08G81/00C08J3/12C08J9/28C08J2201/0484C08J2387/00
Inventor 刘泽华徐力刘瑜张佳音赵志强张永林
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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