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Preparation method of starch nanocrystal ester

A starch nanocrystal and starch nanotechnology, applied in the direction of fermentation, can solve problems such as poor oil phase compatibility, and achieve the effect of expanding the scope of application

Active Publication Date: 2015-01-28
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Starch nanocrystals are composed of dextrin with a specific degree of polymerization, and the surface contains more hydroxyl groups, which leads to its strong hydrophilicity and poor compatibility with the oil phase.

Method used

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Examples

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Effect test

preparation example Construction

[0029] A kind of preparation method of starch nanocrystalline ester, technique is:

[0030] (1) Starch pretreatment

[0031] The waxy cornstarch is placed in a Soxhlet extractor, extracted at 50-60°C for 6-12h, and the extracted starch granules are air-dried in an oven at 45°C for 24h to obtain waxy cornstarch powder.

[0032] (2) Restricted degradation of starch:

[0033] Prepare 2-4M sulfuric acid solution, add 10%-20% of the above-mentioned waxy cornstarch, place in a constant temperature water bath at 30-40°C and stir at a speed of 100-200rpm for 48-72h, centrifuge the obtained nanocrystals, wash with water until the supernatant The liquid is neutral, and it is dispersed in water and freeze-dried to obtain nanocrystalline powder. Starch nanocrystals are composed of dextrins with two distribution ranges of degree of polymerization DP=10-18 and DP=21-33.

[0034] (3) Lipase catalyzes the transesterification reaction between methyl oleate and starch nanocrystals:

[0035]...

Embodiment 1

[0041] Weigh 10 g of waxy corn starch, Soxhlet extraction at 50°C for 12 hours, and then oven-dry at 45°C. Prepare a 3M sulfuric acid solution, add 10% of the above-mentioned waxy cornstarch, place the starch slurry at 40°C and stir at a speed of 100rpm for 72h, centrifuge to remove the supernatant, wash the precipitate with deionized water to neutrality, and freeze-dry.

[0042] Dissolve methyl oleate in absolute ethanol (45% V / V), add 20% wt starch nanocrystals, and then ultrasonically disperse for 1 h, add 2‰ lipase and stir at 100 rpm for 36 h at 45°C and a vacuum of 0.01 MPa . The enzyme was removed by filtration, washed three times with 80% ethanol, and then vacuum-dried at 40° C. to obtain oleic acid starch nanocrystalline ester. The degree of substitution was 0.043 as measured by back titration.

[0043] Water and liquid paraffin are mixed at a volume ratio of 1:1, a certain mass fraction of starch oleate nanocrystalline ester is added, and Ultra Turrax T20 (IKA) is u...

Embodiment 2

[0046] Weigh 10 g of waxy corn starch, Soxhlet extraction at 60°C for 8 hours, and then oven-dry at 45°C. Prepare a 3M sulfuric acid solution, add 10% of the above-mentioned waxy cornstarch, place the starch slurry at 50°C and stir at a speed of 100rpm for 48h, centrifuge to remove the supernatant, wash the precipitate with deionized water until neutral, and freeze-dry.

[0047] Dissolve dodecenyl succinic anhydride in absolute ethanol (55% V / V), add 30%wt starch nanocrystals, and then ultrasonically disperse for 1h, add 5‰lipase, and stir at 100rpm at 40°C and a vacuum of 0.01MPa. 48h. The enzyme was 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 0.094 as measured by back titration.

[0048] Mix water and liquid paraffin at a volume ratio of 1:1, add a certain mass fraction of oleic acid starch nanocrystalline ester, use Ultra Turrax ...

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Abstract

The invention provides a preparation method of starch nanocrystal ester, belonging to the technical field of starch deep processing. According to the principle of the method, based on the strong adsorption capacities of nanoscale particles on the oil-water interfaces, acid is adopted to hydrolyze starch restrictively to micronize the starch to obtain starch nanocrystals with certain surface activities and dimensions of 50-100nm. After the micronized starch nanocrystals are subjected to surface modification through enzymatic ester exchange by adopting methyl oleate, the surface hydroxyl groups of the micronized starch nanocrystals are connected with hydrophobic carbon chains by ester bonds, thus further improving the surface activities of the micronized starch nanocrystals. By adding 1% of the surface esterified nanocrystals, water and liquid paraffin (1:1) systems can form stable emulsion, the emulsifying capacity reaches 65% and the median diameter D50 of the emulsion is 70mu m. The particle size distribution of the emulsion is free from obvious change after the emulsion is put under room temperature for three months. The oleic acid esterified nanocrystals prepared by the preparation method have strong emulsifying capacities and high emulsifying stability and have extensive industrial application prospects.

Description

technical field [0001] The invention discloses a preparation method of starch nano-crystal ester, which relates to starch limited degradation technology and enzyme method catalyzed transesterification reaction technology, and belongs to the field of modified starch development. Background technique [0002] Due to its wide source, low cost, biodegradable, good biocompatibility and non-toxic characteristics, organic nanoparticles have been paid more and more attention by people, and they have been widely studied as material fillers. The study found that nanoparticles can also be adsorbed to the oil-water interface to show a certain surface activity, and it will have broad application prospects as a new type of emulsifier. [0003] Starch is an important basic raw material in food, medicine, chemical industry, textile and other industries, and its particle size is between 5 and 100 μm. During the emulsion formation process, the original starch granules have poor emulsificatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P19/04
Inventor 金征宇田耀旗魏本喜陈煌莉胡秀婷徐学明谢正军赵建伟
Owner JIANGNAN UNIV
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