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Preparation method of carboxymethyl starch by semi-dry method

A technology of carboxymethyl starch and semi-dry method, which is applied in the field of preparation of carboxymethyl starch, can solve the problems of uneven mixing of dry raw materials, easy corrosion of equipment, large solvent consumption, etc. Freeze-thaw stability and antifreeze performance, the effect of moderate product substitution

Active Publication Date: 2017-05-31
无锡秋可生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems in the prior art that the solvent method has large pollution, large solvent consumption, easy corrosion of equipment, etc., uneven mixing with dry raw materials, easy agglomeration and uneven reaction in the starch alkalization process, the applicant provides a Method for preparing carboxymethyl starch by semi-dry method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) With rice starch as raw material and absolute ethanol solution as the wet medium, 4 parts of NaOH and 5 parts of water are mixed in parts by mass, and 40 parts of absolute ethanol are added to fully stir and NaOH is completely dissolved. It is 160r / min, and then this solution is mixed with 15 parts of starch, so that the starch is fully wetted, and a slurry-like mixture is obtained;

[0023] (2) Put the aforementioned slurry-like mixture into a box-type reactor, carry out an alkalization reaction at 35°C for 55 minutes, after the alkalization is completed, cool to room temperature, and fully mix with 6 parts of powdered sodium chloroacetate in a pulverizer ;

[0024] (3) Put the mixture from the pulverizer into the box reactor, carry out the etherification reaction at 67° C. for 2.5 hours, and cool to room temperature after the reaction;

[0025] (4) the reaction product after cooling is washed 1h with 200 parts of mass fraction of methanol aqueous solution of 80%,...

Embodiment 2

[0029] (1) With cornstarch as raw material and absolute ethanol solution as the wet medium, 5 parts of NaOH and 6 parts of water are mixed in parts by mass, and 45 parts of absolute ethanol is added to fully stir and NaOH is completely dissolved, and the stirring speed It is 150r / min, and then this solution is mixed with 15 parts of starch, so that the starch is fully wetted, and a slurry-like mixture is obtained;

[0030] (2) Put the aforementioned slurry-like mixture into a box-type reactor, carry out an alkalization reaction at 40°C for 70 minutes, after the alkalization is completed, cool to room temperature, and fully mix with 5 parts of powdered sodium chloroacetate in a pulverizer ;

[0031] (3) Put the mixture from the pulverizer into the box reactor, carry out the etherification reaction at 73° C. for 2 hours, and cool to room temperature after the reaction;

[0032] (4) The cooled reaction product is washed with 210 parts of mass fraction of 85% aqueous methanol sol...

Embodiment 3

[0036] (1) With rice starch as raw material and absolute ethanol solution as the wet medium, 6 parts of NaOH and 7 parts of water are mixed in parts by mass, and 50 parts of absolute ethanol is added to fully stir and NaOH is completely dissolved. It is 180r / min, and then this solution is mixed with 16 parts of starch, so that the starch is fully wetted, and a slurry-like mixture is obtained;

[0037] (2) Put the aforementioned slurry-like mixture into a box reactor, carry out alkalization reaction at 30°C for 50 minutes, after the alkalization is completed, cool to room temperature, and fully mix with 5.5 parts of powdered sodium chloroacetate in a pulverizer ;

[0038] (3) Put the mixture from the pulverizer into the box reactor, carry out the etherification reaction at 68° C. for 3 hours, and cool to room temperature after the reaction;

[0039] (4) The cooled reaction product was washed with 220 parts by mass fraction of 75% aqueous methanol solution for 1.5 h, and added ...

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Abstract

The invention relates to a preparation method of carboxymethyl starch by a semi-dry method. The preparation method comprises the following steps: by using starch as a raw material and using an absolute ethyl alcohol solution as a wetting medium, adding NaOH and absolute ethyl alcohol to alkalify the starch; mixing with a certain amount of sodium chloroacetate; generating etherification reaction at certain temperature, cooling, cleaning by methyl alcohol, sucking and filtering, washing, and drying to constant weight; completely volatizing the remained methyl alcohol, and screening, so as to obtain the carboxymethyl starch. The preparation method has the advantages that the alkalification and etherification reaction under the organic solvent wetting condition is performed, and the sodium chloroacetate is used for replacing chloroacetic acid and is used as an etherification agent, so as to overcome the defects of consumption of a large amount of organic solvent and low utilization rate of reaction equipment in a solvent method, and also overcome the defects of nonuniform material mixing, nonuniform reaction and the like in a dry method; the toxicity and corrosion of the chloroacetic acid are avoided; the DS (degree of substitution) of the carboxymethyl starch prepared by the semi-dry method can reach 0.58.

Description

technical field [0001] The invention relates to the field of deep processing of agricultural products, in particular to a preparation method of carboxymethyl starch. Background technique [0002] The research on carboxymethyl starch began in 1924, and the development of carboxymethyl starch in my country began in the mid-1980s. Carboxymethyl starch (CMS for short) is an important class of etherified starch derivatives. It is a polymer electrolyte soluble in cold water produced by the etherification reaction of starch with sodium chloroacetate under alkaline conditions. It has been widely used Used in food, textile, medicine, paper making, agriculture and petrochemical industry, etc. In recent years, new hotspots have emerged in domestic research on the application of carboxymethyl. Such as preservatives and stabilizers for food texture properties; pharmaceutical excipients and disintegrants; washing anti-dirt redeposition agents, environmental protection flocculants for se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/12
CPCC08B31/12
Inventor 于秋生
Owner 无锡秋可生物科技有限公司
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