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Method for preparing carboxymethyl inulin under promotion of ionic liquid

A technology of carboxymethyl inulin and ionic liquid, applied in the chemical industry, can solve the problems such as unsatisfactory degree of substitution and yield of carboxymethyl inulin, inability to expand production by synthesis process, influence of carboxymethylation of inulin, and the like. Excellent appearance, promotion of alkalization and etherification reactions, and high degree of substitution

Inactive Publication Date: 2014-12-24
XINZHOU TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, gelatinization of inulin is its main drawback, due to gelatinization, carboxymethylation of inulin is affected
Chinese patent CN1914230A provides a method for preparing carboxylic acid alkyl inulin, adding inulin to the aqueous solution of halogenated carboxylate to form a slurry, controlling the reaction temperature between 20-70°C, and the reaction time is 60-120min , to obtain carboxymethyl inulin, but the degree of substitution and the yield of carboxymethyl inulin produced by this method are not ideal enough
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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  • Method for preparing carboxymethyl inulin under promotion of ionic liquid
  • Method for preparing carboxymethyl inulin under promotion of ionic liquid
  • Method for preparing carboxymethyl inulin under promotion of ionic liquid

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Embodiment 1

[0019] In this embodiment, a method for preparing carboxymethyl inulin under the promotion of ionic liquid is obtained by taking 56 g of inulin, 29 g of chloroacetic acid, 22 g of sodium hydroxide, and 1 g of N-butylpyridine tetrafluoroborate, and preparing it according to the following steps:

[0020] 1) Put 56g of inulin, 1g of N-butylpyridine tetrafluoroborate and 11g of sodium hydroxide into the round-bottomed flask filled with 284ml of ethanol according to the above parts by weight;

[0021] 2) After stirring at a room temperature of 20°C for 10 minutes, add the remaining 11 g of sodium hydroxide to prepare alkalized inulin for later use;

[0022] 3) Dissolve 29 g of chloroacetic acid in an appropriate amount of ethanol, add the obtained chloroacetic acid alcohol solution dropwise to the alkalized inulin prepared in step 2), and then react at room temperature for 1.5 h;

[0023] 4) The reactant prepared in step 3) was left to stand for 5 minutes, and suction filtered acc...

Embodiment 2

[0026] In this embodiment, a method for preparing carboxymethyl inulin under the promotion of ionic liquid is obtained by taking 112 g of inulin, 58 g of chloroacetic acid, 44 g of sodium hydroxide, and 2 g of N-butylpyridine tetrafluoroborate, and preparing it according to the following steps:

[0027] 1) Put 112g of inulin, 2g of N-butylpyridine tetrafluoroborate and 22g of sodium hydroxide into the round-bottomed flask filled with 856ml of isopropanol according to the above parts by weight;

[0028] 2) After stirring at a room temperature of 30°C for 15 minutes, add the remaining 22 g of sodium hydroxide to prepare alkalized inulin for later use;

[0029] 3) The chloroacetic acid of the above ratio is dissolved in an appropriate amount of isopropanol, and the obtained chloroacetic acid alcohol solution is added dropwise to the alkalized inulin prepared in step 2), and then at room temperature at 30 Reaction at ℃ for 2h;

[0030] 4) The reactant prepared in step 3) was left...

Embodiment 3

[0033] The preparation method of a kind of ionic liquid carboxymethyl inulin in this embodiment, take inulin 84g, chloroacetic acid 43.5g, sodium hydroxide 16.5g, N-butylpyridine tetrafluoroborate 1.5g, make according to the following steps :

[0034] 1) Put 84g of inulin, 1.5g of N-butylpyridine tetrafluoroborate and 8.25g of sodium hydroxide into the round-bottomed flask filled with 535ml of isopropanol according to the above parts by weight;

[0035] 2) After stirring at a room temperature of 25°C for 13 minutes, add the remaining 8.25 g of sodium hydroxide to prepare alkalized inulin for later use;

[0036] 3) The chloroacetic acid of the above ratio is dissolved in an appropriate amount of isopropanol, and the obtained chloroacetic acid alcohol solution is added dropwise to the alkalized inulin prepared in step 2), and then at room temperature at 25 Reaction at ℃ for 2h;

[0037] 4) The reactant prepared in step 3) was left to stand for 8 minutes, and suction filtered a...

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Abstract

The invention relates to a method for preparing carboxymethyl inulin under promotion of ionic liquid and belongs to the technical field of chemical engineering. The carboxymethyl inulin is prepared from the following raw materials: inulin, chloroacetic acid, sodium hydroxide and the ionic liquid. The method comprises the following steps: putting the inulin, the ionic liquid and 1 / 2 of sodium hydroxide in an ethanol or isopropanol reaction vessel containing the inulin; after stirring at the room temperature, adding the surplus sodium hydroxide to prepare alkaline inulin; dissolving the chloroacetic acid in moderate ethanol or isopropanol, and dropwise adding the obtained chloroacetic acid alcohol solution in the alkaline inulin for reaction at the room temperature; standing the reactant, carrying out suction filtration to obtain a filter cake; after washing the filter cake with 95% ethanol, drying to obtain a pale yellow product, namely the carboxymethyl inulin. The method effectively avoids gelatinization of the inulin, and the whole reaction process can be carried out well at the room temperature. The method effectively promotes alkalization and etherification reaction and significantly shortens reaction time, and the obtained carboxymethyl inulin is high in degree of substitution and good in appearance.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing carboxymethyl inulin promoted by ionic liquid. Background technique [0002] Inulin, also known as inulin, is a poly straight-chain fructose formed by connecting D-fructofuranose through β(l-2) glycosidic bonds, and often contains a glucose group at the end (for the structure see figure 1 ). Inulin is a soluble dietary fiber naturally occurring in nature. Inulin can be found in almost all plants. It was approved as a new resource food by the Ministry of Health in 2009. The main sources of inulin are extracts from 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. [0003] Carboxymethyl inulin is formed by replacing the primary or secondary alcohol groups on the inulin molecul...

Claims

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Application Information

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IPC IPC(8): C08B37/18
Inventor 赵三虎赵志翀
Owner XINZHOU TEACHERS UNIV
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