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Triple-response type starch based microgel and preparation method thereof

A triple-response, microgel technology, applied in the field of starch deep processing, can solve the problems of poor biodegradability, toxicity, and poor biocompatibility, and achieve mild reaction conditions, simple and controllable preparation process, good biocompatibility and biocompatibility. The effect of degradability

Active Publication Date: 2015-10-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most microgels are prepared from synthetic macromolecules, such as PMA, PVCL, PDEA, and PAA, etc. However, such macromolecules have the disadvantages of poor biodegradability, poor biocompatibility, and certain toxicity.
However, there are no reports on multiple sensitive microgels based on natural macromolecules

Method used

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Examples

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preparation example Construction

[0026] In a more typical embodiment, the preparation method comprises:

[0027] (1) Preparation of amorphous granular starch

[0028] The starch lactoalcohol solution was treated with microwave field to obtain amorphous granular starch.

[0029] (2)C 6 Synthesis of Site-directed Oxidized Starch

[0030] Using TEMPO / NaClO / NaBr system for amorphous granular starch C 6 Site-directed oxidation of the primary alcohol hydroxyl group to obtain C 6 Site-directed oxidation of starch.

[0031] (3) Preparation of oil phase emulsion

[0032] The composition and preparation method of the oil phase emulsion can adopt any suitable type and method known in the industry.

[0033] For example, Tween-80 and Span-80 can be mixed in a volume ratio of 1-2:8-9 to prepare a mixed surfactant, and then the mixed surfactant can be mixed with an organic solvent such as n-hexane in a volume ratio of 2 -5: Mix 995-998, stir at a speed of 400-500 rpm in a protective atmosphere, such as nitrogen gas, ...

Embodiment 1

[0043] (1) get 20g wax paper cornstarch, be dispersed in 100mL mass fraction and be 50% ethanol solution, obtain starch lactoalcohol solution, utilize microwave field to starch lactoalcohol solution is processed, microwave power 1000W, processing time 20 minutes, obtain non- Crystalline granular starch: Add 30% of the above-mentioned amorphous granular starch milk 100mL to a three-neck flask equipped with a stirrer, dropping funnel, and thermometer, add 0.02g TEMPO and 0.4g NaBr, control the temperature in an ice-water bath, and drop Add 60 mL of 20% NaClO solution into a liquid funnel, and dropwise add 0.1 mol / L NaOH solution to keep the pH of the reaction medium at 10. After reacting for 2-4 hours, the reaction solution was slowly added to ethanol to precipitate, filtered, washed, and vacuum-dried at 40°C. get C 6 Oxidized starch with a degree of oxidation of 80%. Dissolve 1g of oxidized starch, 95mmol monomer NIPAM and 3mmol crosslinking agent BIS prepared above into 100mL ...

Embodiment 2

[0045] Take 25g wax paper cornstarch and disperse it in 100mL ethanol solution with a mass fraction of 50% to obtain a starch lactoalcohol solution. Use a microwave field to process the starch lactoalcohol solution. The microwave power is 1200W and the treatment time is 30 minutes to obtain an amorphous granular state. Starch: add 30% of the above-mentioned amorphous granular starch milk 100mL to a three-neck flask equipped with a stirrer, dropping funnel, and thermometer, add 0.05g TEMPO and 0.5g NaBr, control the temperature in an ice-water bath, and add it through the dropping funnel 75 mL of 20% NaClO solution was added dropwise with 0.1 mol / L NaOH solution to keep the pH of the reaction medium at 10. After reacting for 4 hours, the reaction solution was slowly added to ethanol to precipitate, filtered, washed, and dried under vacuum at 40°C. Prepared to get C 6 Oxidized starch with a degree of oxidation of 95%. Dissolve 1g of oxidized starch, 95mmol monomer NIPAM and 3m...

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Abstract

The invention discloses a triple-response type starch based microgel and a preparation method thereof. According to the preparation method, pH sensitive C6-site fixed-point oxidized starch and temperature sensitive NIPAM (N-isopropylacrylamide) are used as raw materials, and an inverse emulsion polymerization method is adopted to prepare C6-site fixed-point oxidized starch and PNIPAM semi-interpenetrating polymer network microgel, namely the triple-response type starch based microgel. The triple-response type starch based microgel disclosed by the invention is in the form of spherical particles, the particle size is 15-25 microns, and the triple-response type starch based microgel has triple sensitivity of pH, temperature and ionic strength and good biocompatibility and biodegradability, can be widely used in the fields of nutrient protection, drug controlled release, protein separation and purification and the like, and meanwhile is simple and controllable in preparation process, mild in reaction condition and suitable for large-scale production.

Description

technical field [0001] The invention relates to a starch-based microgel, in particular to a triple-response starch-based microgel and a preparation method thereof, belonging to the technical field of starch deep processing. Background technique [0002] Smart microgels refer to microgels that respond to stimuli in response to changes in external conditions (such as temperature, pH, light, ionic strength, electric or magnetic fields, etc.). According to different sources of raw materials, microgels can be divided into synthetic microgels and natural microgels. Most microgels are prepared from synthetic macromolecules, such as PMA, PVCL, PDEA, and PAA, etc. However, such macromolecules have disadvantages such as poor biodegradability, poor biocompatibility, and certain toxicity. Natural macromolecules have attracted more and more attention because of their biodegradable, biocompatible, non-toxic and other advantages. [0003] At the same time, the research on poly-N-isopropy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/54C08F222/38C08F2/30C08L33/24C08L3/10C08B31/18
Inventor 金征宇田耀旗章宝陶晗魏本喜胡秀婷吴春森徐学明杨哪
Owner JIANGNAN UNIV
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