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Chitosan/5-hydroxymethylfurfural composition preparation method

A technology of hydroxymethyl furfural and chitosan is applied in the field of preparation of chitosan/5-hydroxymethyl furfural composition, and can solve the problem of difficulty in popularization and use, low yield, chitosan/genipin-like hydrogels The problem of high price of glue, to achieve the effect of fast response, low cost, and promotion of resource utilization

Active Publication Date: 2015-08-05
GUANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it is reported that genipin cross-linking agents have low cytotoxicity, the only shortcoming is that genipin is almost all obtained by biological extraction, and the yield is very low, so chitosan / genipin water The price of gel is generally high and it is difficult to popularize and use

Method used

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  • Chitosan/5-hydroxymethylfurfural composition preparation method
  • Chitosan/5-hydroxymethylfurfural composition preparation method
  • Chitosan/5-hydroxymethylfurfural composition preparation method

Examples

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Effect test

Embodiment 1

[0030] (1) Preparation of chitosan solution: Weigh 1.5 g of dry chitosan powder (deacetylation degree is 93.5%, weight average molecular weight is 1.254×10 6 Da) Disperse in 70 ml of deionized water, then add 30 ml of 5% acetic acid solution, stir until the chitosan is completely dissolved, and the concentration of chitosan is calculated to be 15 mg / ml (15% w / v).

[0031] (2) Preparation of 5-hydroxymethylfurfural solution: Weigh 10.0 g of fructose and put it into a 0.15 L stainless steel autoclave, add 100 ml of deionized water, vacuumize at room temperature to remove the air in the autoclave, and then fill it with CO 2 When the pressure in the kettle reached 5.0 MPa, the temperature was rapidly raised to 160°C, and the reaction was stopped after reacting for 100 min at a stirring speed of 250 r / min, and 2 ml of the reaction solution was taken from the sampling tube to analyze the product by high performance liquid chromatography. It is known that the degradation product is ...

Embodiment 2

[0036] (1) Preparation of chitosan solution: Weigh 2.5 g of dry chitosan powder (deacetylation degree is 95.8%, weight average molecular weight is 1.852×10 5 ), add 50 ml of 2% acetic acid solution, stir until the chitosan is completely dissolved, and the calculated chitosan concentration is 50 mg / ml.

[0037] (2) Preparation of 5-hydroxymethylfurfural solution: Weigh 0.5 g of 5-hydroxymethylfurfural (purity: 99.9%), add 100 ml of absolute ethanol, stir well, and calculate that 5-hydroxymethylfurfural The concentration is 5 mg / ml.

[0038] (3) Condensation reaction of chitosan and 5-hydroxymethylfurfural: Measure 50 ml of the chitosan solution described in step (1), 50 ml of the 5-hydroxymethylfurfural solution described in step (2) and 30 ml of absolute ethanol, mixed the above solutions together, adjusted the pH of the system to 8.0 with 2% NaOH aqueous solution, stirred at 85 °C (250 r / min) for 1.5 h, and obtained flocculent chitosan / 5 - Hydroxymethylfurfural Schiff base....

Embodiment 3

[0042] (1) Preparation of chitosan solution: Weigh 5.0 g of dry O-carboxymethyl chitosan powder (deacetylation degree is 100%, weight average molecular weight is 4.0×10 6 Da) Disperse in 80 ml of deionized water, then add 20 ml of 25% hydrochloric acid solution, stir until chitosan is completely dissolved, and the concentration of chitosan is calculated to be 50 mg / ml (50% w / v).

[0043] (2) Preparation of 5-hydroxymethylfurfural solution: Weigh 8.0 g of sucrose and put it into a 0.15 L stainless steel autoclave, add 100 ml of ethyl acetate, vacuumize at room temperature to remove the air in the autoclave, and then fill it with CO 2 When the pressure in the kettle reached 5.0 MPa, the temperature was rapidly raised to 160°C, and the reaction was stopped after reacting for 100 min at a stirring speed of 250 r / min, and 2 ml of the reaction solution was taken from the sampling tube to analyze the product by high performance liquid chromatography. It is known that the degradation...

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Abstract

The invention relates to a chitosan / 5-hydroxymethylfurfural composition preparation method. The method includes dissolving a chitosan substance by an acid aqueous solution to obtain a solution A, mixing the solution A with a solution containing 5-hydroxymethylfurfural to obtain a pre-reaction solution, adding alkali liquor into the pre-reaction solution to regulate a pH (potential of hydrogen) value of the pre-reaction solution, subjecting the pre-reaction solution to condensation reaction at a stirring speed of 100-500r / min at the temperature of 4-85 DEG C to obtain a gelatinous or flocculent chitosan / 5-hydroxymethylfurfural composition, and subjecting the chitosan / 5-hydroxymethylfurfural composition obtained after the reaction to dialysis treatment by deionized water prior to freeze drying so as to obtain a dry chitosan / 5-hydroxymethylfurfural composition. By the aid of the chitosan / 5-hydroxymethylfurfural composition prepared according to the chitosan / 5-hydroxymethylfurfural composition preparation method, more -NH2 radical groups can be retained, so that more excellent unique antibacterial performance, biological adhesion performance and the like can be retained.

Description

technical field [0001] The invention belongs to the field of natural polymer material processing, and in particular relates to a preparation method of a chitosan / 5-hydroxymethylfurfural composition. Background technique [0002] Chitosan (Chitosan, referred to as CS) is the product of deacetylation of chitin under the action of hot, concentrated hydroxide (usually sodium hydroxide). It is the only alkaline polysaccharide in nature. Sugars dissolve in acidic media and thus can be processed into many different physical forms such as solutions, films, and gels. [0003] It is generally believed that -NH on the molecular chain of chitosan 2 It endows chitosan with many unique properties, such as coordination ability with metal ions, bioadhesion, biodegradability, biocompatibility, antibacterial and antitumor properties. These unique properties make chitosan widely used in the fields of medicine, cosmetics, spices, agriculture and food industry. [0004] C-NH on chitosan molec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08C08J9/28C08J3/075C08L5/08
Inventor 黎演明李秉正潘丽霞
Owner GUANGXI ACAD OF SCI
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