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Thermo-sensitive chitosan derivative-hydroxypentyl chitosan and preparation method thereof

A technology of chitosan derivatives and hydroxyamyl shells, applied in the field of thermosensitive chitosan derivatives - hydroxyamyl chitosan and its preparation, to achieve the effect of simple preparation method and good water solubility

Inactive Publication Date: 2012-10-03
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, there is no research on the preparation, properties and application of hydroxyamyl chitosan at home and abroad.

Method used

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  • Thermo-sensitive chitosan derivative-hydroxypentyl chitosan and preparation method thereof
  • Thermo-sensitive chitosan derivative-hydroxypentyl chitosan and preparation method thereof
  • Thermo-sensitive chitosan derivative-hydroxypentyl chitosan and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: the preparation of hydroxypentyl chitosan

[0029] The first step, the preparation of chitosan:

[0030] Take 100 grams of fresh shrimp shells, soak in 800 ml of 5% (W / V) hydrochloric acid to remove calcium, then soak in 800 ml of 10% (W / V) sodium hydroxide to remove impurities, and wash with deionized water PH to 7-8, drying and grinding to obtain powdered chitin, then add 800 ml of 50% (W / V) sodium hydroxide solution to deacetylation reaction at 90°C for 24 hours, wash the PH with deionized water value to 7, then dehydrated with 95% alcohol, and finally vacuum-dried to obtain chitosan with a deacetylation degree of 85%.

[0031] The second step, the purification of chitosan:

[0032] Add the chitosan prepared in the first step to 1000 ml of sodium hydroxide solution with a concentration of 2% (W / V), control the temperature at about 75°C, stir for 2 hours, filter with suction, and then add 800 ml of 2% ( W / V) sodium hydroxide solution, the same process...

Embodiment 2

[0038] Embodiment 2: the preparation of hydroxypentyl chitosan

[0039] The first step, the preparation of chitosan is with embodiment 1;

[0040] Second step, the purification of chitosan is with embodiment 1;

[0041] The 3rd step, the alkalization of chitosan is with embodiment 1;

[0042] The fourth step, the hydroxypentylation of chitosan:

[0043] Filter and extrude excess lye in 10 grams of alkalized chitosan with 100-mesh silk cloth, transfer to a three-necked bottle, add 80 ml of isopropanol and stir for 2 hours to completely disperse chitosan, then separate liquids Slowly add 200 ml of 1,2-epoxypentane dropwise into the funnel, stir in the container at a speed of 300 rpm at room temperature, react for 5 days, after the reaction is complete, precipitate with 9 times the volume of acetone, and wash with 75% ethanol pH value to 7-8, dehydration, and vacuum drying at 50°C to obtain white powdery hydroxypentyl chitosan.

Embodiment 3

[0044] Embodiment 3: the preparation of hydroxypentyl chitosan

[0045] The first step, the preparation of chitosan is with embodiment 1;

[0046] Second step, the purification of chitosan is with embodiment 1;

[0047] The third step, alkalization of chitosan:

[0048] Add 10 grams of purified chitosan into 100 milliliters of 50% (W / V) potassium hydroxide solution, and place it at room temperature for 24 hours.

[0049] The 4th step, the hydroxypentylation of chitosan is the same as example 2.

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Abstract

The invention relates to the technical field of biological materials, and particularly relates to thermo-sensitive chitosan derivative-hydroxypentyl chitosan and a preparation method of the hydroxypentyl chitosan. The invention provides the preparation method of the thermo-sensitive chitosan derivative-hydroxypentyl chitosan. The method comprises the steps of firstly carrying out alkali activation on purified chitosan, then taking 1,2-pentane oxide as an etherifying agent, taking isopropanol as a dispersed phase, carrying out mild reaction for 3-6 days at room temperature, participating with acetone and washing until a neutral state reaches after reaction, carriying out vacuum drying in at 50 DEG C to obtain the hydroxypentyl chitosan. The hydroxypentyl chitosan disclosed by the invention has water-solubility and thermosensitivity; the lowest critical solution temperature (LCST) is 17 DEG C (2%W / V), and the hydroxypentyl chitosan can be fast cured into a stable gel state from a liquid state at physiological temperature of 37 DEG C.

Description

technical field [0001] The invention relates to the technical field of biological materials, in particular to a thermosensitive chitosan derivative-hydroxypentyl chitosan and a preparation method thereof. Background technique [0002] Chitosan [Chitosan, (1,4)-2-amino-2-deoxy-β-D-glucan] is a high molecular weight polysaccharide obtained by partial deacetylation of chitin. It is estimated that nearly 10 billion tons of chitin are biosynthesized every year in the biological world. It is a natural organic compound second only to cellulose on the earth, and it is mainly synthesized by animals. [0003] In the middle and late 20th century, the international community attached great importance to the development and utilization of this resource, and its application has involved many departments and fields such as food, medicine, chemical industry, environmental protection and agriculture. However, due to the -O-H┈O-type and -N-H┈O-type hydrogen bonds in the chitosan molecule, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 侯春林刘文魏长征
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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