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Method for preparing methyl starch

A technology of methyl starch and starch, which is applied in the field of chemical modification of natural polysaccharide polymers, can solve the problems that the efficiency of starch is difficult to be greatly improved, and achieves remarkable thickening and emulsifying effects, good cold water solubility, low cost effect

Inactive Publication Date: 2012-05-30
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In Chinese patent application CN 101168568, ethanol is used as a solvent, cetyltrimethylammonium bromide and tetrabutylammonium bromide are used as catalysts, and dimethyl carbonate is used to methylate starch to obtain methoxy Methylated starch with a base content of up to 3%, but failed to take reasonable measures to activate and pretreat starch macromolecules, making it difficult to increase the efficiency of starch in a heterogeneous reaction system by a large margin. improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add 9 parts of absolute dry tapioca starch, 2 parts of activator urea, 3 parts of sodium chloride and 20 parts of 95% ethanol into the reactor, react at 58°C; add 1 part of cetyltrimethylammonium bromide 1, 1 part of tetrabutylammonium bromide and 3 parts of ammonium chloride are mixed catalysts, then add 57 parts of dimethyl carbonate, and react at 58 ° C for 2 hours;

[0024] (2) Warm up to 69°C, add 4 parts of 50% potassium carbonate aqueous solution dropwise, react for 8 hours, wash, extract, dry and pulverize the product to obtain methyl starch after cooling.

[0025] The parts are parts by mass.

[0026] The 1H NMR spectra of starch at δ5.05, 4.6, 3.6, 3.42, and 3.35 are the absorptions of H-1, H-4, H-3, H-2, H-5, and H-6 on starch glucose residues, respectively peak. Compared with starch, in the 1H NMR spectrum of the product of this example, there is a sharp absorption peak at δ3.15, which is the characteristic absorption of methoxy. It shows that the pro...

Embodiment 2

[0029] (1) Add 9 parts of absolute dry potato starch, 4 parts of urea and 19 parts of 95% ethanol into the reactor to start the reaction; then add 5 parts of tetrabutylammonium bromide, 58 parts of dimethyl carbonate, Down reaction 1.5 hours;

[0030] (2) Warm up to 68°C, add 5 parts of 51% potassium carbonate aqueous solution dropwise, react for 7 hours, wash, extract, dry and pulverize the product to obtain methyl starch after cooling.

[0031] The parts are parts by mass.

[0032] The 1H NMR spectrum of the product in this example is the same as in Example 1, except that the absorption peak at δ3.15 is weaker and the peak area is smaller. It shows that the product is indeed methyl starch.

[0033] The determination of methoxyl content adopts Zeisel methoxyl determination method. After determination, the methoxyl content of the methyl starch prepared in this embodiment is 3.3%.

Embodiment 3

[0035] (1) 10 parts of dry corn starch, 4 parts of urea and 17 parts of 95% ethanol are added to the reactor to start the reaction; 5 parts of cetyltrimethylammonium bromide and 60 parts of dimethyl carbonate are added, React at 53°C for 1 hour;

[0036] (2) Warming up to 74°C, adding 4 parts of 52% potassium carbonate aqueous solution dropwise, reacting for 8 hours, washing, extracting, drying and pulverizing the product after cooling to obtain methyl starch.

[0037] The parts are parts by mass.

[0038] The 1H NMR spectrum of the product in this example is the same as in Example 1, except that the absorption peak at δ3.15 is weaker and the peak area is smaller. It shows that the product is indeed methyl starch.

[0039] The determination of methoxyl content adopts Zeisel methoxyl determination method. After determination, the methoxyl content of the methyl starch prepared in this embodiment is 3.8%.

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Abstract

The invention relates to a method for preparing methyl starch. The method comprises the following steps of: (1) mixing 8-10 parts of absolute dried starch, 3-5 parts of activating agent and 17-20 parts of ethanol aqueous solution and reacting; adding 57-60 parts of dimethyl carbonate and 4-6 parts of catalyst, mixing and activating for 1-2 hours at 53-58 DEG C; (2) heating to 65-75 DEG C, dripping 2-7 parts of potassium carbonate aqueous solution and reacting for 6-8 hours; and after the product is cooled, washing, drying and pulverizing to obtain the methyl starch. The method of the invention has the advantages of simple process, mild reaction condition, low cost and no emission of toxic and harmful gas and wastes; and by reasonably optimizing a reaction system and adopting a certain starch activating technology, reacting section by section, adding efficient catalyst, and the like, the starch and the dimethyl carbonate fully react for preparing the methyl starch with high methoxyl content, and a series of problems in the prior art are solved.

Description

technical field [0001] The invention relates to a chemical modification method of natural polysaccharide polymers, in particular to a preparation method of methyl starch. Background technique [0002] The hydrogen atoms on the hydroxyl groups of starch molecules are replaced by methyl groups, which is methyl starch. Methyl starch is an important variety of natural starch modified products, and it is also a functional fine polymer material with a wide range of uses. It can be widely used in food, medicine, textile, building materials, metallurgy and many other industrial fields; at the same time, methylation technology is also a very important means to determine the composition of sugar residues and the connection position of polysaccharides. In recent years, with the improvement of people's awareness of environmental protection, environmentally friendly and biodegradable methyl starch has been paid more and more attention by people, but the traditional methyl starch prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/10
Inventor 陈玉放侯成敏李建
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI