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Preparation method of water-soluble polymer cyclodextrin

A technology of water-soluble polymer and cyclodextrin, which is applied in the field of preparation of water-soluble polymer cyclodextrin, can solve the problems of reduced solubility, storage resistance and insolubilization of cyclodextrin polymer, and achieves easy to grasp, The effect of prolonging the reaction time of gelation and high practical value

Active Publication Date: 2021-11-16
CHENGDU TECHCAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the preparation of cyclodextrin polymers is mainly divided into linear polymers and dendritic polymers. The most convenient preparation method is to prepare polymers with epichlorohydrin as a crosslinking agent in an alkaline environment. As the degree increases, the molecular weight gradually increases. After reaching the crosslinking limit, an insoluble cyclodextrin polymer is formed. In actual operation, the reaction end point is often difficult to control accurately.
At the same time, because it also contains active tail groups, the cross-linking degree of the water-soluble cyclodextrin synthesized in this way will further increase after being placed for a long time. Therefore, the cyclodextrin polymer obtained by this method is not durable to storage , the solubility is greatly reduced or cannot be dissolved at all after being placed for a long time

Method used

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  • Preparation method of water-soluble polymer cyclodextrin
  • Preparation method of water-soluble polymer cyclodextrin
  • Preparation method of water-soluble polymer cyclodextrin

Examples

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Embodiment 1

[0028] The present embodiment provides a kind of preparation method of water-soluble polymer cyclodextrin, comprising the following steps:

[0029] 1) Dissolve 5g of cyclodextrin into 10ml of 30wt% NaOH aqueous solution, and continue stirring for 12 hours to dissolve into a transparent solution, and the hydroxyl group is fully activated;

[0030] 2) Heating the cyclodextrin solution obtained in step (1) and maintaining it at 40° C., adding epichlorohydrin and glycerin, the total amount of the two added is 10 times the molar amount of cyclodextrin, and epichlorohydrin and propane The molar ratio of triols is 1:5, stir and continue to react for 280min;

[0031] 3) Add 1 volume of acetone to the reaction system to terminate the reaction, stir at 240rpm for 5 minutes and then let it stand, remove the acetone in the upper layer after the system is layered; add hydrochloric acid drop by drop, adjust the pH value of the reaction system to 12; heat to React at 50°C for 12 hours, pour...

Embodiment 2

[0035] The present embodiment provides a kind of preparation method of water-soluble polymer cyclodextrin, comprising the following steps:

[0036] 1) Dissolve 5g of cyclodextrin into 10ml of NaOH aqueous solution with a concentration of 15wt%, and continue to stir for 8 hours to dissolve it into a transparent solution, and the hydroxyl group is fully activated;

[0037] 2) Heating the cyclodextrin solution obtained in step (1) and maintaining it at 50° C., adding epichlorohydrin and glycerin, the total amount of the two added is 15 times the molar amount of cyclodextrin, and epichlorohydrin and propane The molar ratio of triols is 1:2, stir and continue to react for 200min;

[0038] 3) Add 1 volume of acetone to the reaction system to terminate the reaction, stir at 200rpm for 5 minutes and then let it stand, remove the acetone in the upper layer after the system is layered; add hydrochloric acid drop by drop, adjust the pH value of the reaction system to 12; heat to React a...

Embodiment 3

[0040] The present embodiment provides a kind of preparation method of water-soluble polymer cyclodextrin, comprising the following steps:

[0041] 1) Dissolve 5g of cyclodextrin into 10ml of 25wt% NaOH aqueous solution, and continue to stir for 10 hours to dissolve into a transparent solution, and the hydroxyl group is fully activated;

[0042] 2) Heating the cyclodextrin solution obtained in step (1) and maintaining it at 70° C., adding epichlorohydrin and glycerin, the total amount of the two added is 25 times the molar amount of cyclodextrin, and epichlorohydrin and propane The molar ratio of triols is 1:12, stir and continue to react for 10 minutes;

[0043] 3) Add 1 volume of acetone to the reaction system to terminate the reaction, stir at 200rpm for 5 minutes and then let it stand, remove the acetone in the upper layer after the system is layered; add hydrochloric acid drop by drop, adjust the pH value of the reaction system to 12; heat to React at 50°C for 12 hours, ...

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Abstract

The invention provides a preparation method of water-soluble polymer cyclodextrin. The preparation method is simple in steps, and the prepared polymer is high in molecular weight and still has good water solubility after being placed for a long time, meanwhile, a cyclodextrin cavity is reserved, and the structure is in a lamellar dendritic shape. The method comprises the following step: polymerizing cyclodextrin, epoxy chloropropane and glycerol under an alkaline condition to obtain the water-soluble polymer cyclodextrin. The cyclodextrin polymer disclosed by the invention has relatively high thermal stability, can still keep good water solubility after being placed for a long time, structurally retains a hydrophobic cavity of cyclodextrin, also has high molecular weight, and has a relatively high practical value in the field of supramolecular solution rheological property regulation.

Description

technical field [0001] The invention relates to the technical field of cyclodextrin preparation, in particular to a method for preparing water-soluble polymer cyclodextrin. Background technique [0002] Cyclodextrin is a product from starch hydrolysis. Because of its special circular cavity structure with hydrophilic outside and hydrophobic inside, it can form host-guest inclusion complexes with various target molecules. Cyclodextrin has good affinity, and it is usually prepared into various cyclodextrin polymers according to needs. [0003] Cyclodextrin polymer not only has polymer effect, but also retains the inclusion ability of the parent cyclodextrin cavity, and has better inclusion performance when the guest molecule is larger. At present, the preparation of cyclodextrin polymers is mainly divided into linear polymers and dendritic polymers. The most convenient preparation method is to prepare polymers with epichlorohydrin as a crosslinking agent in an alkaline enviro...

Claims

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Application Information

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IPC IPC(8): C08B37/16
CPCC08B37/0012C08B37/0015
Inventor 李玺叶仲斌罗平亚舒政
Owner CHENGDU TECHCAL UNIV
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