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A kind of preparation method of high degree of substitution carboxymethyl starch

A technology for carboxymethyl starch and starch, which is applied in the field of preparation of high degree of substitution carboxymethyl starch, can solve the problems of poor solubility, easy gelatinization, large amount of waste water, etc., so as to improve the dispersibility of the system and increase the degree of etherification , Reduce the effect of gelatinization and agglomeration

Active Publication Date: 2019-04-16
SHANGHAI ARGUS NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The degree of substitution of CMS prepared by dry method and semi-dry method is not high, and the distribution of substituents is uneven, and the solubility of the product is poor
The wet process uses water as the medium. Because CMS is easy to gelatinize in cold water, the product is difficult to purify, and the amount of waste water is large, so the wet process has little industrial significance and is rarely used now.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0011] In a preferred embodiment, a method for preparing carboxymethyl starch with a high degree of substitution of the present invention includes the following steps: 1) dispersing the starch in a mixed solvent of alcohol / water, adding 30-40% NaOH in a total molar amount Alkaline the starch at 30-40°C for 1-3 hours; 2) add etherification agent, osmotic dispersant, optional viscosity diluent and the remaining 60-70 mole% NaOH, and etherify at 45-60°C React for 4-6 hours; finally 3) neutralize with hydrochloric acid, wash with 90% ethanol, filter, and dry to obtain CMS with a high degree of substitution.

[0012] In a preferred embodiment, the starch used in the method of the present invention can be any type of starch, for example including corn starch, tapioca starch, potato starch or mixtures thereof.

[0013] In a preferred embodiment, the alcohol used in the method of the present invention is a water-miscible alcohol, such as methanol, ethanol, isopropanol, n-butanol, isob...

Embodiment 1

[0038] Disperse 45.6g of cornstarch (water content 9%) in a mixed solvent of 160g of ethanol and 40g of water, stir, add 9g of NaOH (purity 99%), and react at 35-36°C for 90min. Add 34g monochloroacetic acid (purity 99%), react at 45°C for 60min, heat up to 50°C, react for 60min, add 17g NaOH, 0.6g isooctyl alcohol polyoxyethylene ether (10EO) sulfate, 1.5g urea, heat up to 60 ℃, continue to react for 180min. Cool down to 30-35°C, add hydrochloric acid to neutralize to about pH 7, filter, wash the filter cake 2-3 times with 90% ethanol, and dry at about 50°C to obtain a light yellow powder CMS product. It was determined that the degree of substitution of the CMS was 1.22.

Embodiment 2

[0040]Disperse 45.6g tapioca starch (water content 9%) in a mixed solvent of 170g diethylene glycol and 30g water, stir, add 10g NaOH (purity 99%), and react at 38-40°C for 60min. Add 38.7g monochloroacetic acid (purity 99%), react at 45°C for 60min, heat up to 52°C, react for 90min, add 23g NaOH, 0.8g lauryl polyoxyethylene ether (15EO) sulfate, 2g urea, heat up to 55°C , continue to react for 90min. Cool down to 30-35°C, add hydrochloric acid to neutralize to about pH 7, filter, wash the filter cake 2-3 times with 90% ethanol, and dry at about 50°C to obtain a light yellow powder CMS product. It was determined that the degree of substitution of the CMS was 1.36.

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Abstract

The invention discloses a method for preparing high-substitution carboxymethyl starch. The method comprises the following steps: 1) dispersing starch in mixed solvent of alcohol / water, adding alkali metal hydroxide with a total molar weight of 30-40% to cause the starch to undergo alkalization reaction for 0.5-4 h at 25-45 DEG C; 2) adding an etherifying agent, a permeating dispersant, optional viscosity diluent and remaining 60-70% of alkali metal hydroxide to a reaction mixture in the step 1), so as to undergo the etherification reaction for 4-6 h at 40-65 DEG C; and 3) performing neutralization to obtain the high-substitution carboxymethyl starch. The prepared carboxymethyl starch (CMS) is high in substitution, the reaction process is easy to control, no gelatinization occurs, and the etherifying agent utilization rate is high.

Description

technical field [0001] The invention relates to a method for preparing starch carboxymethyl starch, in particular to a method for preparing carboxymethyl starch with a high degree of substitution used in the textile industry. Background technique [0002] Carboxymethyl starch (CMS), a cold-water soluble starch derivative, is one of the main varieties of modified starch. It is widely used in papermaking, petrochemical, textile, pharmaceutical, daily chemical, food and other fields, and its preparation and application has always been a research hotspot. The structural unit of starch is glucose. There are three hydroxyl groups that can be substituted on the glucose unit structure, and the average number of substituted groups is called the degree of substitution (DS). Theoretically, the degree of substitution of carboxymethyl starch is 0‐3. Generally speaking, DS less than 0.4 is called low substitution, DS between 0.4 and 1.0 is called medium substitution, and DS greater tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/12
CPCC08B31/12
Inventor 李正雄郑国国
Owner SHANGHAI ARGUS NEW MATERIAL CO LTD
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