A kind of water-soluble antibacterial monocarboxyl chitosan and its preparation method and application

A single carboxyl group, chitosan technology, applied in textile and papermaking, fiber processing, animal fiber and other directions, to achieve the effect of simple process, high yield and mild reaction conditions

Active Publication Date: 2017-08-08
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

C6 position oxidized chitosan (monocarboxyl chitosan) that the present invention relates to prepares and the method for amide-modified real silk fabric has not seen any report yet

Method used

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  • A kind of water-soluble antibacterial monocarboxyl chitosan and its preparation method and application
  • A kind of water-soluble antibacterial monocarboxyl chitosan and its preparation method and application
  • A kind of water-soluble antibacterial monocarboxyl chitosan and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: monocarboxy chitosan preparation

[0038] Weigh 4.0g of chitosan with a viscosity-average molecular weight of 800,000 and a deacetylation degree of 85% and place it in a 2% (v / v) dilute acetic acid solution at a bath ratio of 1:25 (w / v), stir at 60°C Dissolve in 1 hour, cool to 40°C and add 15mL of mixed acid (V 浓硝酸 :V 浓磷酸 =1:1), then add sodium nitrite with a mass volume ratio of 0.007g / mL to the mixed acid in a light-proof airtight container, and slightly shake it at 40°C for 2 hours, and immediately add 230mL of absolute ethanol after the reaction Terminate the oxidation reaction, the oxidation product is precipitated with acetone, vacuum filtered until the pH of the filtrate is about 6, washed with absolute ethanol, vacuum dried and refined to obtain a light yellow monocarboxyl group with a molecular weight of 180,000 and a carboxyl degree of 29.72%. Chitosan A, stored at 4°C for later use. After testing, the degree of deacetylation of the monocarbo...

Embodiment 2

[0040] Weigh 4.0g of chitosan with a viscosity-average molecular weight of 800,000 and a deacetylation degree of 85% and place it in a 4% (v / v) dilute acetic acid solution at a bath ratio of 1:25 (w / v), stir at 60°C Dissolve in 1 hour, cool to 25°C and add 15mL of mixed acid (V 浓硝酸 :V 浓磷酸 =2:1), then add sodium nitrite with a mass volume ratio of 0.014g / mL to the mixed acid in a light-proof airtight container, and slightly shake it at 25°C for 3 hours, and immediately add 230mL of absolute ethanol after the reaction The oxidation reaction was terminated, the oxidation product was precipitated with acetone, filtered under reduced pressure until the pH of the filtrate was about 6, washed with absolute ethanol, dried in vacuum and refined to obtain a yellow single carboxyl shell with a molecular weight of 110,000 and a carboxyl degree of 40.36%. Glycan B, stored at 4°C for later use. After testing, the degree of deacetylation of the monocarboxychitosan B obtained in this exampl...

Embodiment 3

[0042] Weigh 4.0g of chitosan with a viscosity-average molecular weight of 800,000 and a deacetylation degree of 85% and place it in a 4% (v / v) dilute acetic acid solution at a bath ratio of 1:25 (w / v), stir at 60°C Dissolve in 1h, cool to 25°C and add 21mL of mixed acid (V 浓硝酸 :V 浓磷酸 =2:1), then add sodium nitrite with a mass volume ratio of 0.014g / mL to the mixed acid in a light-proof airtight container, and slightly shake it at 25°C for 8 hours, and immediately add 242mL of absolute ethanol after the reaction Terminate the oxidation reaction, the oxidation product is precipitated with acetone, vacuum filtered until the filtrate pH is about 6, washed with absolute ethanol, vacuum dried and refined to obtain a dark yellow single carboxyl shell with a molecular weight of 60,000 and a carboxyl degree of 53.57%. Glycan C, stored at 4°C for later use. After testing, the degree of deacetylation of the monocarboxychitosan C obtained in this example is 85.3%, the solubility in wat...

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Abstract

The invention discloses a water-soluble antibacterial monocarboxylic chitosan as well as a preparation method and application thereof. The preparation method of the monocarboxylic chitosan is characterized by comprising the following steps: dissolving macromolecular chitosan in a diluted acetic acid solution, and then selectively oxidizing part or all of hydroxyl groups at the C6 site of the chitosan into carboxyl groups by utilizing a concentrated nitric acid-concentrated phosphoric acid-sodium nitrite system, thereby obtaining the monocarboxylic chitosan. The water-soluble antibacterial monocarboxylic chitosan disclosed by the invention can be used for carrying out amide modification on real silk fabrics so as to obtain monocarboxylic chitosan amide modified real silk fabrics. The method disclosed by the invention is simple in operation, high in reaction speed and easy to control, the prepared monocarboxylic chitosan amide modified real silk fabrics have lasting and efficient antibacterial activity and good wearability and are environment-friendly, and the negative effects on good real silk characteristics and human health caused by using chemical crosslinking agents in conventional chitosan modification are overcome.

Description

technical field [0001] The present invention relates to a kind of water-soluble antibacterial monocarboxyl chitosan and its preparation method and its application in amide modified silk fabrics, especially relates to the method of preparing durable antibacterial silk fabrics by adopting amide modification technology and utilizing monocarboxy chitosan , which belongs to antibacterial chitosan and its modification technology applied to silk fabrics. Background technique [0002] Natural silk is non-toxic, non-irritating, skin-friendly, has excellent biocompatibility, degradability, flexibility, stretch resistance, breathability, moisture absorption, and elegant luster, soft and smooth, gorgeous appearance, It is comfortable to take and is known as the "Queen of Fiber". It has shown great application prospects in the fields of medical hygiene, textile and clothing, drug carriers, tissue engineering, food additives, cosmetics, etc. [Li Guohong, Liu Hong, et al.Surface modificati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08D06M15/03D06M13/02D06M11/13D06M13/345D06M101/10
Inventor 许云辉钟娇杜兆芳汪雨夏翱鲍康赟
Owner ANHUI AGRICULTURAL UNIVERSITY
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