A kind of preparation method of carboxymethyl chitin

A technology of carboxymethyl chitin and chitin, which is applied in the field of preparation of carboxymethyl chitin, can solve the problems of decreasing molecular weight, low purity, affecting the effectiveness of products, etc., and achieves concentrated molecular weight distribution, high product substitution, and product Purity-enhancing effect

Active Publication Date: 2021-06-25
BLOOMAGE BIOTECHNOLOGY CORP LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] At present, the preparation methods of carboxymethyl chitin include homogeneous reaction and heterogeneous reaction. The homogeneous reaction is to completely dissolve the raw materials in the reaction solvent to achieve the purpose of full reaction, but the homogeneous reaction is more complex than the heterogeneous reaction. The molecular weight of the product is severely reduced, which seriously affects the effectiveness of the product in later applications; the heterogeneous reaction is to react the raw materials in a solid-liquid heterogeneous system. Wide distribution
[0005] In addition, at present, carboxymethyl chitin is mostly extracted from the reaction solution by means of forward alcohol precipitation, that is, alcohol is added to the solution to precipitate carboxymethyl chitin. Patent CN1261170C discloses a preparation method of carboxymethyl chitin , add chitin to isopropanol or ethanol, basify with sodium hydroxide or potassium hydroxide, add chloroacetic acid dropwise to react, wash the reacted solid, dissolve in water, adjust pH to neutral, filter , adding ethanol to precipitate the solution under stirring, and drying the solid to obtain purified carboxymethyl chitin, wherein the purification method used is forward alcohol precipitation. Although this alcohol precipitation method can play a certain role in purification, the molecular weight distribution of the final product Inhomogeneous, and the impurities are not easy to remove, the purity is low
As a biomedical material, the purity and molecular weight of the product will affect the safety and effectiveness of the product, so the current purification method limits the application of carboxymethyl chitin in the biomedical field

Method used

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  • A kind of preparation method of carboxymethyl chitin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]1. Primary carboxymethylation reaction: Mix 10g of 60mesh chitin, 250g of 50% sodium hydroxide aqueous solution, and 40mg of sodium lauryl sulfate in a 500ml three-necked flask, under nitrogen protection and dark conditions, at 20°C Stir in a water bath for 20 hours, remove excess sodium hydroxide solution by suction filtration, add 170ml of isopropanol to the residue and stir evenly, dissolve 30g of chloroacetic acid in 30ml of isopropanol, add dropwise chloroacetic acid isopropanol solution at 15°C for 2.5 h, the temperature was raised to 20°C to react for 46 hours after the dropwise completion.

[0042] 2. Secondary carboxymethylation reaction: Filtration, the primary reaction crude product was repeatedly washed with 500ml of 75% ethanol aqueous solution and then dried. Mix 5g of crude product, 45g of 50% sodium hydroxide and 18mg of sodium lauryl sulfate in 250ml In a three-neck flask, under the condition of nitrogen protection and light protection, stir in a water b...

Embodiment 2

[0047] 1. Primary carboxymethylation reaction: Mix 10g of 60mesh chitin, 100g of 40% aqueous sodium hydroxide solution, and 40mg of sodium lauryl sulfate in a 500ml three-necked flask, under nitrogen protection and dark conditions, at 20°C Stir in a water bath for 20 hours, remove excess sodium hydroxide solution by suction filtration, add 125ml of isopropanol to the residue and stir evenly, dissolve 75g of chloroacetic acid in 75ml of isopropanol, add chloroacetic acid isopropanol solution dropwise at 10°C for 6 hours , After dropping, the temperature was raised to 15°C for 24h.

[0048] 2. Secondary carboxymethylation reaction: Filtration, the primary reaction crude product was repeatedly washed with 500ml of 70% ethanol aqueous solution and then dried. Mix 5g of crude product, 25g of 40% sodium hydroxide and 15mg of sodium lauryl sulfate in 250ml In a three-neck flask, under the condition of nitrogen protection and light protection, stir in a water bath at 20°C for 20h, add...

Embodiment 3

[0053] 1. Primary carboxymethylation reaction: Mix 10g of 60mesh chitin, 500g of 55% sodium hydroxide aqueous solution, and 200mg of sodium lauryl sulfate in a 2000ml three-necked flask, under nitrogen protection and dark conditions, at 20°C Stir in a water bath for 20 hours, remove excess sodium hydroxide solution by suction filtration, add 680ml of isopropanol to the residue and stir evenly, dissolve 120g of chloroacetic acid in 120ml of isopropanol, add dropwise chloroacetic acid isopropanol solution at 15°C for 1 hour , After dropping, the temperature was raised to 20°C for 48h.

[0054] 2. Secondary carboxymethylation reaction: Filtration, the primary reaction crude product was repeatedly washed with 500ml of 80% ethanol aqueous solution and then dried. Mix 5g of crude product, 100g of 55% sodium hydroxide and 100mg of sodium lauryl sulfate in 1000ml In a three-necked flask, under the condition of nitrogen protection and light protection, stir in a water bath at 20°C for ...

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Abstract

The invention discloses a method for preparing carboxymethyl chitin. The method adopts a secondary carboxymethylation reaction to prepare a crude product on the basis of a heterogeneous reaction, and then dissolves the crude product in a mixed solution of physiological saline and water. Remove the insoluble matter after the soluble matter is completely dissolved, continue to drop absolute ethanol into the solution, stop the dropwise addition when a white precipitate begins to appear in the solution, then drop the solution into the remaining absolute ethanol, collect the precipitate, After washing and drying, the finished product of carboxymethyl chitin is obtained. The present invention adopts the secondary carboxymethylation reaction, the reaction is more thorough, the product has a higher degree of substitution and higher uniformity; the crude product is purified by the combination of forward alcohol precipitation and reverse alcohol precipitation, which can not only improve the molecular weight Screening can also improve the purity of the product. The resulting product has a larger molecular weight, a more concentrated molecular weight distribution, and a higher purity. It has better safety, effectiveness, and biocompatibility, and has a wider range of applications in the field of biomedical materials. .

Description

technical field [0001] The invention relates to a preparation method of carboxymethyl chitin, in particular to a preparation method of carboxymethyl chitin with concentrated molecular weight distribution and high purity, and belongs to the technical field of carboxymethyl chitin preparation. [0002] technical background [0003] Chitin (C8H13O5N)n, also known as chitin, chitin, English name Chitin. It was discovered by French scholar Braconno in 1811 and extracted from crustacean shells by Ogier in 1823. There are many related application researches on biomedical materials, which have the advantages of good biocompatibility, no biotoxicity, low price, easy modification, and good mechanical strength. The chitin derivative carboxymethyl chitin has good water solubility, and while retaining the good characteristics of chitin, it can be used in a wider range of fields. [0004] At present, the preparation methods of carboxymethyl chitin include homogeneous reaction and heterog...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
CPCC08B37/0003C08B37/003
Inventor 田悦李超刘建建李敏韩月梅郭学平
Owner BLOOMAGE BIOTECHNOLOGY CORP LTD
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