Preparation method of temperature sensitivity chitosan derivate-hydroxybutyl chitosan
A technology of chitosan derivatives and hydroxybutyl chitosan, which is applied in the preparation of hydroxybutyl chitosan and the preparation of temperature-sensitive chitosan derivatives-hydroxybutyl chitosan, can solve mechanical problems Poor performance, slow response speed, and limited application of hydrogels, etc., to achieve good water solubility
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Embodiment 1
[0023] A kind of preparation method of thermosensitive chitosan derivative-hydroxybutyl chitosan is:
[0024] The first step. the preparation of chitosan:
[0025] Preparation of chitosan solution: take 100 grams of fresh shrimp shells, remove the head, feet and tail, wash with water, soak in 5% hydrochloric acid with 800 ml concentration to remove calcium, and soak with 800 ml concentration of 10% sodium hydroxide to remove the chitosan solution. Miscellaneous protein, washed with water for injection to pH 7-8, dried, and ground to obtain powdered chitin, and then deacetylated in 800 ml of 50% sodium hydroxide solution at a temperature of 80°C-100°C for 18- For 24 hours, wash the pH value with water for injection to 7-8, dehydrate with 95% alcohol, and finally vacuum-dry to obtain chitosan with a deacetylation degree of 85-95%;
[0026] The second step. the purification of chitosan, remove residual protein and pigment in chitosan:
[0027] Add the chitosan prepared in the f...
Embodiment 2
[0034] The preparation of embodiment 2 hydroxybutyl chitosan of the present invention
[0035] The preparation of the first step chitosan is with embodiment 1;
[0036] The purification of second step chitosan is with embodiment 1;
[0037] The alkalization of the third step chitosan is with embodiment 1;
[0038] Step 4. Hydroxybutylation of Chitosan
[0039]Filter and extrude the excess lye in 10 grams of alkalized chitosan with 100-mesh silk cloth, transfer it to a three-necked bottle, add 80 ml of isopropanol and stir for 2 hours to completely disperse the chitosan, then separate the liquids Slowly add 100 ml of 1,2-epoxybutane dropwise into the funnel, and react at room temperature for 5 days. After the reaction is complete, 9 times the volume of acetone is precipitated, washed to a pH value of 7-8, and vacuum-dried at 50°C to obtain a white powder.
Embodiment 3
[0040] The preparation of embodiment 3 hydroxybutyl chitosan of the present invention
[0041] The preparation of the first step chitosan is with embodiment 1;
[0042] The purification of second step chitosan is with embodiment 1;
[0043] The alkalization of the third step chitosan is with embodiment 1;
[0044] Step 4. Hydroxybutylation of Chitosan
[0045] Filter and extrude excess lye in 10 grams of alkalized chitosan with 100 mesh silk cloth, transfer to a three-necked bottle, add 80 milliliters of isopropanol and stir for 1-2 hours to disperse chitosan completely, then Slowly add 200 ml of 1,2-epoxybutane dropwise into the separatory funnel, and react at room temperature for 4 days. After the reaction is complete, 9 times the volume of acetone precipitates, washes the pH value to 7-8, and vacuum-dries at 50°C to obtain a white powder .
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