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Surface cross-linking esterification compound modification method of starch nanocrystal

A starch nanocrystal and compound modification technology, which is applied in the field of starch nanocrystal surface cross-linking and esterification compound modification, can solve the problems of difficulty, harsh reaction conditions, complex reaction route, etc., achieve low cost and inhibit agglomeration , The effect of simple process

Inactive Publication Date: 2012-08-15
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It should be pointed out that most of these starch nanocrystal modification methods are carried out in toxic organic solvents such as toluene and tetrahydrofuran. The reaction conditions are harsh, the reaction route is complicated, and the industrial implementation is costly and difficult.

Method used

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  • Surface cross-linking esterification compound modification method of starch nanocrystal
  • Surface cross-linking esterification compound modification method of starch nanocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Waxy cornstarch is dispersed in 3.16mol / L sulfuric acid aqueous solution, the quality of waxy cornstarch is 10% (w / v) of the volume of sulfuric acid solution, is stirred at 40 ℃ for 6 days, and the stirring speed is 200rpm, then centrifugal washing until the pH is 6-8, and dry to obtain starch nanocrystals.

[0030] Mix the prepared starch nanocrystals and water in a mass ratio of 1 / 200, ultrasonically oscillate in a water bath at 30°C and stir at a speed of 200 rpm for 60 minutes to obtain a starch nanocrystal aqueous phase suspension; use 2mol / L hydrogen Sodium oxide solution adjusts suspension pH to be 12.0, adds the sodium sulfate of starch nanocrystal quality 0.5 times and the phosphorus oxychloride of starch nanocrystal quality 20%, reacts 2 hours at 20 ℃; Then adjust pH with the hydrochloric acid solution of 2mol / L to 8.0, slowly drop acetic anhydride accounting for 10% of the mass of starch nanocrystals, and at the same time use 0.5mol / L sodium hydroxide solutio...

Embodiment 2

[0032]Same as Example 1, the difference is that the pH of the suspension is adjusted to 10.0 with 0.05mol / L sodium hydroxide solution, sodium trimetaphosphate with 15% starch nanocrystal mass is added, and reacted at 50°C for 3 hours; then use 0.05mol / L hydrochloric acid solution to adjust the pH to 7, add 10mL mass fraction of 0.1% sulfuric acid solution as a catalyst, slowly drop into the mixture of acetic acid and acetic anhydride (volume ratio is 1:1) accounting for 100% of the starch nanocrystal mass, add acetic acid and acetic anhydride Mixture volume 5% mass concentration is 0.1% sulfuric acid aqueous solution, react at 50 ℃ for 4 hours, adjust the suspension pH to 7 with 0.05mol / L sodium hydroxide solution, wash and dry at 30 ℃, obtain dispersible in N, N-dimethylformamide, methanol, ethanol, acetone, tetrahydrofuran, butanol, dichloroethane, chloroform, dichloromethane, bromoethane, benzene, toluene, carbon tetrachloride surface cross-linked esterification composite mo...

Embodiment 3

[0034] Same as Example 1, the difference is that the pH of the suspension is adjusted to 11.0 with 1mol / L sodium hydroxide solution, and sodium chloride with 1 times the mass of starch nanocrystals and phosphorus oxychloride with 30% of the mass of starch nanocrystals are added, at 30°C React for 5 hours; then adjust the pH to 8.5 with 1mol / L hydrochloric acid solution, slowly drop in acetic anhydride accounting for 50% of the mass of starch nanocrystals, and keep the pH of the system between 8.5-9.0 with 1mol / L sodium hydroxide solution and react at 35°C for 4 hours, adjust the pH to 6 with 0.1mol / L hydrochloric acid solution, wash and dry at 40°C to obtain dispersible N,N-dimethylformamide, methanol, ethanol, acetone, tetrahydrofuran, Butanol, dichloroethane, chloroform, dichloromethane surface cross-linked esterification composite modified starch nanocrystals.

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Abstract

The invention relates to a surface cross-linking esterification compound modification method of a starch nanocrystal and belongs to the technical field of a solid material modification method. The technical scheme comprises the following steps of: dispersing the starch nanocrystal into a water-phase medium by ultrasonic waves and adding an auxiliary reagent and a reaction reagent (comprising a cross-linking agent and an esterification agent); heating the system (wherein the temperature is lower than a gelatinization temperature of starch); enabling the cross-linking agent and a protracted hydroxyl on the surface of the nanocrystal to have a reaction; connecting the hydroxyls which are close on the surfaces of crystal particles to enable the esterification agent and the protracted hydroxyl of the nanocrystal to have a reaction; leading a hydrophobic group into the surface of the starch nanocrystal; and finally, carrying out centrifugal washing and drying treatment to obtain the surface cross-linking esterification compound modified starch nanocrystal. The surface cross-linking esterification compound modification method of the starch nanocrystal has the characteristics of simplicity in operation and low cost; and the prepared surface cross-linking esterification compound modified starch nanocrystal has a very good application prospect on the field of a macromolecular nano compound material.

Description

technical field [0001] The invention relates to a method for performing crosslinking and esterification compound modification on the surface of starch nanocrystals, which relates to the reaction of crosslinking agents and esterification agents with hydroxyl groups on the surface of starch nanocrystals, and belongs to the technical field of solid material modification methods. Background technique [0002] Starch is a natural polymer composed of amylose and amylopectin, with a semi-crystalline structure. After mild hydrolysis of starch granules by acid or enzyme, the amorphous part is removed, so as to obtain nanoscale particles with higher crystallinity, that is, starch nanocrystals. [0003] As a functionally modified starch, starch nanocrystals not only have the advantages of being renewable, degradable, low density, and low energy consumption for production, but also have a dense structure, high rigidity, low moisture permeability, and a small flake shape. Ideal reinforc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/00C08B31/04
Inventor 周江任丽丽蒋蔓董晓刚佟金陈东辉马云海孙霁宇陈玉香常志勇
Owner JILIN UNIV
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