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Method for preparing acetate starch with mechanical activation solid phase reaction

A technology of acetate starch and solid phase reaction, which is applied in the field of mechanically activated solid phase reaction to prepare acetate starch, which can solve the problems of high dispersion loss rate, low product substitution degree, and high heating rate, so as to improve the reaction activity and simplify the operation process , the effect of reducing production costs

Inactive Publication Date: 2013-04-24
YULIN NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the reaction time of this method is short, in the preparation process, as the temperature rises, the water loss rate of the starch surface layer is higher than the water loss rate of the starch inner layer.
At the same time, the microwave reaction temperature measuring device can only measure the temperature of the surface layer of the reactive starch, resulting in a higher heating rate of the inner layer than that of the surface layer. The inside of the reactive starch is gelatinized due to excessive temperature, and the product has a low degree of substitution and is difficult to control. It can only exist in the experiment. chamber small scale preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Measure 20mL of acetic anhydride and mix with 50g of starch, then add 1.25g of solid sodium hydroxide, stir evenly, seal and place for 24 hours;

[0022] Put the mixture obtained in the previous step into a self-made stirring ball mill, add 300mL of zirconia as a ball milling medium, the diameter of the ball milling medium is 6mm, stir and react at 50°C for 50 minutes, and the speed of the stirring blade is 300 rpm;

[0023] The product is separated from the ball medium, washed with 70% ethanol by volume until the pH value is 6.0-7.0, vacuum-filtered, dried at 50°C, and crushed to 120 mesh.

[0024] The degree of substitution of the obtained acetate starch was 0.18.

Embodiment 2

[0026] Measure 25mL of acetic anhydride and mix with 50g of starch, then add 1.5g of solid sodium hydroxide, stir evenly, seal and place for 24 hours;

[0027] Put the mixture obtained in the previous step into a self-made stirring ball mill, add 500mL of zirconia as a ball milling medium, the diameter of the ball milling medium is 6mm, stir and react at 60°C for 50 minutes, and the speed of the stirring blade is 380 rpm;

[0028] The product is separated from the ball medium, washed with 80% ethanol by volume until the pH value is 6.0-7.0, vacuum-filtered, dried at 50°C, and crushed to 120 mesh.

[0029] The degree of substitution of the obtained acetate starch was 0.26.

Embodiment 3

[0031] Measure 30mL of acetic anhydride and mix with 50g of starch, then add 2.0g of solid sodium hydroxide, stir evenly, seal and place for 36 hours;

[0032] Put the mixture obtained in the previous step into a self-made stirring ball mill, add 500mL of zirconia as a ball milling medium, the diameter of the ball milling medium is 6mm, stir and react at 50°C for 60 minutes, and the speed of the stirring blade is 500 rpm;

[0033] The product is separated from the ball medium, washed with 80% ethanol by volume until the pH value is 6.0-7.0, vacuum-filtered, dried at 50°C, and crushed to 120 mesh.

[0034] The degree of substitution of the obtained acetate starch was 0.23.

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Abstract

The invention discloses a method for preparing acetate starch with mechanical activation solid phase reaction, comprising the following steps: a, mixing acetic anhydride equivalent to 40-80% of starch mass with starch, then adding solid sodium hydroxide equivalent to 1.0-4.0% of starch mass, stirring uniformly and then sealing for placing for 12-36h; b, loading a mixture obtained in the step a in a self-made ball-stirring mill, adding a ball milling medium with a ball material volume ratio of (6-12): 1, wherein the diameter of the ball milling medium is 4-8mm, stirring reaction lasts 40-80 min at the temperature of 40-80 DEG C, and the rotating speed of strirrer is 200-500 rpm; and c, separating the product with the ball milling medium, washing with ethanol with the volume fraction of 60-90% till the pH value is 6.0-7.0, vacuumizing and filtering, drying at the temperature of 30-60 DEG C, and then crashing till 100-120 meshed. According to the method, the acetate starch with high substitution value can be prepared, and the technology is simple and environmentally-friendly.

Description

technical field [0001] The invention relates to a method for preparing acetate starch by mechanically activating solid phase reaction. Background technique [0002] Acetate starch is an important type of modified starch, also known as acetylated starch. It is a starch derivative obtained by reacting the hydroxyl group in the starch macromolecule with acetic acid directly or indirectly with acetic acid derivatives under certain conditions. So far, there has been a Hundred years of history. According to the average number of ester groups introduced in each glucose group of starch molecules, acetylated starch can be divided into high, medium and low degrees of substitution. Acetate starch with a degree of substitution of 2 to 3 is a high degree of substitution, acetate starch with a degree of substitution of 0.3 to 1 is a starch with a degree of substitution of medium; and low-esterified starch is a derivative with a degree of substitution of 0.01 to 0.2. Acetate starch with ...

Claims

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Application Information

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IPC IPC(8): C08B31/04C08B30/02
Inventor 陈渊朱其虎杨家添梁露锋朱万仁玉琼广韦庆敏甘振登何军陈江枫梁著棋曾成伟黄晓英
Owner YULIN NORMAL UNIVERSITY
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