Preparation method of carboxymethyl inulin

A technology of carboxymethyl inulin and inulin, which is applied in the field of preparation of carboxymethyl inulin, can solve the problems that the synthesis process cannot expand production, and achieve the effects of good appearance, reduced reaction time, and mild reaction conditions

Inactive Publication Date: 2021-09-24
赵三虎
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, some studies have used microwave, ultrasonic and other methods for the carboxymethylation of inulin. Although the reaction time has been shortened and the degree of substitution of the product has been improved, the microwave and ultrasonic synthesis processes cannot expand production.

Method used

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  • Preparation method of carboxymethyl inulin

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[0024] The invention provides a kind of preparation method of carboxymethyl inulin, comprising the following steps:

[0025] (1) mix inulin, sodium hydroxide, pyridinium salt and solvent, carry out alkalization reaction, obtain alkalized inulin;

[0026] (2) Mix the alkalized inulin, sodium hydroxide, organic chloride and solvent to carry out etherification reaction to obtain the carboxymethyl inulin.

[0027] In the present invention, the pyridinium salt in the step (1) is preferably N-butylpyridine tetrafluoroborate.

[0028] In the present invention, the solvent in the step (1) is preferably ethanol or isopropanol.

[0029] In the present invention, the volume fraction of the ethanol is preferably 93-97%, more preferably 94-96%.

[0030] In the present invention, the mass ratio of inulin to pyridinium salt in the step (1) is preferably 4-5: 0.05-0.1, more preferably 4.2-4.8: 0.06-0.09, more preferably 4.4-4.6: 0.07- 0.08.

[0031] In the present invention, the dosage ra...

Embodiment 1

[0051] Mix 4.5g of inulin, 1g of sodium hydroxide and 20mL of isopropanol, add 0.1g of N-butylpyridine tetrafluoroborate dropwise at a rate of 55 drops / min, and control the stirring speed to 25rpm after the addition , alkalized at room temperature for 15 minutes to obtain alkalized inulin;

[0052] Keep stirring after obtaining alkalized inulin, continue to add 0.76g of sodium hydroxide; then weigh 2.3g of chloroacetic acid and dissolve it in 10mL of isopropanol, and mix the mixture of chloroacetic acid and isopropanol at a rate of 60 drops / min. Add the mixture dropwise into the reaction system. After etherification reaction at room temperature for 2 hours, suction filter at 0.01 MPa, wash the suction filtered product thoroughly with 95% ethanol, and dry at 40°C for 6 hours after washing to obtain carboxymethyl base inulin.

[0053] The degree of substitution of the carboxymethyl inulin prepared in this example is 0.71.

[0054] The infrared spectrum of the carboxymethyl inu...

Embodiment 2

[0056] Take 45g of inulin, 12g of sodium hydroxide and 250mL of 95% ethanol and mix them, and add 0.8g of N-butylpyridine tetrafluoroborate dropwise at a rate of 60 drops / min. Alkalizing reaction at room temperature for 20 minutes to obtain alkalized inulin;

[0057] Keep stirring after obtaining the alkalized inulin, continue to add 8g of sodium hydroxide; then weigh 30g of chloroacetic acid and dissolve it in 120mL of isopropanol, and drop the mixture of chloroacetic acid and isopropanol at a rate of 60 drops / minute Add it into the reaction system, after etherification reaction at room temperature for 2.3h, then suction-filter at 0.01MPa, fully wash the suction-filtered product with 95% ethanol, and dry at 38°C for 6.3h after washing to obtain carboxymethyl base inulin.

[0058] The degree of substitution of the carboxymethyl inulin prepared in this example is 0.71.

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Abstract

The invention belongs to the technical field of chemical engineering. The invention provides a preparation method of carboxymethyl inulin. According to the invention, inulin, pyridinium salt and a solvent are mixed, gelatinization of the inulin is avoided in the alkalization reaction, and the whole reaction process can be carried out at room temperature; due to the solubilizing effect of the pyridinium salt on reactants, molecules of the reactants are in effective contact, alkalization and etherification reactions are promoted, the reaction time is shortened, and the substitution degree of the carboxymethyl inulin is increased; and meanwhile, sodium hydroxide is added in batches, so that degradation of inulin under a strong alkali condition and reaction of organic chloride and alkali are avoided. Therefore, the preparation method provided by the invention is mild in reaction condition and high in reaction speed, and the prepared carboxymethyl inulin is excellent in appearance.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of carboxymethyl inulin. Background technique [0002] Inulin, also known as inulin, is a polylinear fructose formed by connecting D-fructofuranose through β(1-2) glycosidic bonds, and often contains a glucose group at the end. Inulin is a soluble dietary fiber that exists naturally in nature. Inulin can be found in almost all plants. The main source of inulin is the extracts of crops such as asparagus, Jerusalem artichoke, and chicory. In recent years, research on inulin and its derivatives at home and abroad is on the rise, and green chemicals based on inulin have made some progress. Carboxymethyl inulin is formed by replacing the primary or secondary alcohol groups on the inulin molecule with carboxymethyl groups, adding new functions on the basis of maintaining the biodegradable, renewable and non-toxic properties of inulin . Carboxymethyl in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/18
CPCC08B37/0054
Inventor 赵三虎王志军赵志翀贾晓丽
Owner 赵三虎
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