Preparation method of modified starch nanocrystal

A technology of starch nanocrystals and modified starch, applied in the field of modified starch development, can solve the problems of short carbon chain, low reaction efficiency and degree of substitution, etc., and achieve the effect of expanding the scope of application

Inactive Publication Date: 2013-10-02
JIANGNAN UNIV
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

Octenyl succinic anhydride modified starch is generally accepted because of its better emulsifying properties, but due to its short carbon chain, in order to obtain better emulsifying properties, its degree of substitution must be appropriately increased; if the carbon chain is too long, Low reaction efficiency and substitution degree during starch denaturation due to steric hindrance

Method used

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Examples

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preparation example Construction

[0028] A method for preparing modified starch nanocrystals, using waxy rice starch as a raw material, using dilute sulfuric acid to hydrolyze raw starch granules to prepare starch nanocrystals, and using dodecenyl succinic anhydride as a modifier, lipase method The surface of the starch nanocrystal is hydrophobically modified to prepare the dodecenyl succinic acid modified starch nanocrystal. The process is:

[0029] (1) Starch pretreatment conditions:

[0030] Prepare 2-4M sulfuric acid solution, add 10%-20% starch, stir evenly, and then place it in an ultrasonic cell pulverizer for treatment. The ultrasonic treatment power is 400-600W, below 25°C, each action time is 30s, and the interval is 30s. The processing time is 50-60 minutes;

[0031] (2) Restricted degradation conditions of starch:

[0032] Place the ultrasonically treated starch milk in a constant temperature water bath at 30-40°C and stir at a speed of 100-200rpm for 72-96 hours, centrifuge the obtained nanocry...

Embodiment 1

[0040] Prepare a 3M sulfuric acid solution, add 10% waxy rice starch, and then act for 40 minutes under the condition of ultrasonic power of 500W and 25°C. The starch slurry was placed at 40° C. and stirred at a speed of 100 rpm for 72 hours, centrifuged to remove the supernatant, and the precipitate was washed with deionized water until it was neutral, and then freeze-dried.

[0041] Dodecenyl succinic anhydride was dissolved in absolute ethanol (30% V / V) and 10% wt of starch nanocrystals were added, then ultrasonically dispersed for 1 h, and 2‰ lipase and After molecular sieve, the mixture was stirred and reacted at 100 rpm for 36 h under the condition of 45° C. water bath. Molecular sieves and enzymes were removed by filtration, washed three times with 80% ethanol, and then vacuum-dried at 40° C. to obtain dodecenyl succinic anhydride modified starch nanocrystals. The degree of substitution was 0.089 as measured by back titration.

Embodiment 2

[0043] Prepare a 4M sulfuric acid solution, add 15% waxy rice starch, and act on it for 60 minutes under the condition of ultrasonic power 400W and 25°C. The starch slurry was placed at 50° C. and stirred at a speed of 100 rpm for 96 hours, centrifuged to remove the supernatant, and the precipitate was washed with deionized water until it was neutral, and then freeze-dried.

[0044] Dodecenyl succinic anhydride was dissolved in absolute ethanol (40% V / V) and then 15% wt of starch nanocrystals were added and ultrasonically dispersed for 1 h, and 5‰ lipase and After molecular sieve, the mixture was stirred and reacted at 100 rpm for 48 hours under the condition of 40° C. water bath. Molecular sieves and enzymes were removed by filtration, washed three times with 90% ethanol, and then vacuum-dried at 40° C. to obtain dodecenyl succinic anhydride modified starch nanocrystals. The degree of substitution was 0.148 as measured by back titration.

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Abstract

The invention provides a preparation method of modified starch nanocrystal, belonging to the technical field of the development of modified starch. The principle of the preparation method provided by the inversion is based on the situation that the difference of the acid tolerance is caused by the hemi-crystal capability of a starch structure, an amorphous region of starch particles is restrictively hydrolyzed by dilute acid, and the acid-resistant starch microcrystal particles can be formed, wherein the sizes of the acid-resistant starch microcrystal particles are 10-100nm. The particles are ultramicro, so that the particles are easily absorbed onto an oil-water interface, and have a certain surface activity, and the surface activity of the particles can be greatly improved after the particles are modified on surfaces in an esterification way by the DDSA (dodecenly succinic anhydride) through an enzymic method. 0.5% of the modified nanocrystal is added, so that a water and weak-polarity methylbenzene (1:1) oil-water system can form stable O/W type emulsion, the emulsifying capacity reaches 76%, and the median diameter of the emulsion D50=55 microns; after the emulsion is placed for four months under room temperature (0.2% of sodium azide bacteriostat is added), the particle size distribution of the emulsion can not be obviously changed. The modified starch nanocrystal prepared by the preparation method provided by the invention is high in emulsifying capacity, and high in emulsifying stability, thereby being wide in industrial application prospect.

Description

technical field [0001] A preparation method of modified starch nanocrystals relates to ultrasonic pretreatment technology and starch enzymatic esterification technology, and belongs to the field of modified starch development. Background technique [0002] As a new type of emulsifier, nanoparticles have attracted more and more attention. Nano-CaCO 3 Powder, Nano SiO 2 Emulsions stabilized by inorganic nanoparticles such as particles, kaolin, and montmorillonite have been widely used in the fields of chemistry, materials science, and polymer science. But because the inorganic nature of these particles limits their application range, organic nanoparticles have attracted attention in recent years. Starch is an important basic raw material in food, medicine, chemical industry, textile and other industries, and its particle size ranges from 5 to 100 μm due to different sources. Particles with a particle size in this range cannot be stably adsorbed to the oil-water interface du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/00C08B31/04
Inventor 金征宇田耀旗魏本喜章宝赵建伟徐学明谢正军周星
Owner JIANGNAN UNIV
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