Method for preparing chitosan immobilized cyclodextrin derivative from chitin
A technology of cyclodextrin and its derivatives, which is applied in the field of polymer material preparation, can solve problems such as yield reduction, water solubility of chitosan 6-OH immobilized cyclodextrin, limitation of application effect, and limited application.
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Embodiment 1
[0066] Weigh 1 part of chitin, under nitrogen protection, add 40 parts of DMAc and 3 parts of LiCl at the same time, stir at 40°C for 30 minutes to fully swell the chitin. Afterwards, the temperature of the reaction system was lowered to 0°C under the reaction conditions, 15 parts of NaOH was added, and then 5 parts of p-toluenesulfonyl chloride was dissolved in 40 parts of chloroform, and slowly added into the chitin solution within 20 minutes using a dropping funnel. React for 10 hours. After the reaction, add ethanol to precipitate, filter with suction, wash off unreacted p-toluenesulfonyl chloride with chloroform, and dry under vacuum at 60°C to obtain chitin derivative a.
[0067] Weigh 1 part of chitin derivative a and dissolve it in 20 parts of DMAc, stir at 30°C to dissolve it. After adding 2 parts of sodium azide, the reaction was stirred at 60° C. for 10 hours. After the reaction, use ethanol to precipitate, wash the precipitate with water, and finally wash with DMA...
Embodiment 2
[0073] Chitin-loaded cyclodextrin derivative e was prepared by the click chemical reaction of chitin derivative b and β-cyclodextrin derivative d prepared in Example 1:
[0074] Weigh 1 part of chitin derivative b, disperse and swell in 12 parts of DMAc, and weigh another 0.03 part of CuSO 4 ·5H 2 O was dispersed in 6 parts of organic solvent, adding 0.03 part of sodium ascorbate and 0.08 part of water to promote dissolution, and mixed the solution; weighed 3.5 parts of β-cyclodextrin derivative d, added the above solution, and stirred at 40°C for reaction After 6 hours, stop the reaction, add precipitant acetonitrile, wash 4 times with DMF, vacuum dry the filter cake at 60°C to obtain chitin-immobilized cyclodextrin derivative e.
[0075] Soak 1 part of the obtained chitin-supported cyclodextrin derivative e in 20 parts of an aqueous solution of NaOH with a mass concentration of 20%, stir and react by heating at 80°C for 20 hours, filter, wash twice with DMF, and place in V...
Embodiment 3
[0077]Weigh 1 part of chitin, add 40 parts of hexafluoroisopropanol at the same time, stir at 40°C for 30 minutes to fully swell the chitin. Then cool down the reaction system to -10°C under the reaction conditions, add 30 parts of triethylamine, then dissolve 4 parts of p-toluenesulfonyl chloride in 40 parts of chloroform, and slowly add chitin in 15 minutes with a dropping funnel The solution was reacted for 10 hours. After the reaction was completed, tetrahydrofuran was added, filtered with suction, unreacted p-toluenesulfonyl chloride was washed away with chloroform, and the chitin derivative a was obtained by vacuum drying at 60°C.
[0078] Weigh 1 part of chitin derivative a and dissolve it in 25 parts of hexafluoroisopropanol, stir at 30°C to dissolve it. After adding 2.8 parts of sodium azide, the reaction was stirred at 60° C. for 12 hours. After the reaction is finished, use acetone to precipitate, wash the precipitate with water, and finally wash with hexafluoroiso...
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