A kind of long-chain soluble chitosan and preparation method thereof
A technology of chitosan and chitosan solution, applied in the field of medicine, can solve the problems of inability to directly dissolve in water, limited application and the like
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Embodiment 1
[0023] Embodiment 1: the invention provides a kind of preparation method of long-chain easily soluble chitosan, comprises the following steps:
[0024] 1) Put 50 mmol of dibromoethane and 10 mmol of N,N-dimethylethylamine into 30 mL of acetonitrile, purify with nitrogen, stir at 50°C for 16 hours, and then reflux for 1 hour. The solvent was evaporated to dryness and washed with ether. A white paste was obtained, which was dried at 35°C for 48 hours to obtain the terminal bromide quaternary ammonium salt a.
[0025] 2) Disperse 1 g of chitosan in 30 mL of DMSO, and stir for 1 hour at 85 ° C with nitrogen gas to obtain a chitosan solution; add 5 mmol of the synthesized terminal brominated quaternary ammonium salt a to dissolve in 10 mL of DMSO, and slowly drop into the above Chitosan solution was maintained at 85°C and stirred for 8 hours to obtain a crude product. The crude product was filtered in acetone at 25°C, precipitated and washed with acetone at 40°C. Dry at 40°C for...
Embodiment 2
[0026] Embodiment 2: the present invention provides a kind of preparation method of long-chain easily soluble chitosan, comprises the following steps:
[0027] 1) Put 50 mmol of dibromopropane and 10 mmol of N,N-dimethyloctylamine into 30 mL of acetonitrile, purify with nitrogen, stir at 50°C for 16 hours, and then reflux for 1 hour. The solvent was evaporated to dryness and washed with ether. Obtain a white paste, dry, and dry at 35°C for 48 hours to obtain terminal bromide quaternary ammonium salt b.
[0028] 2) Disperse 1 g of chitosan in 40 mL of DMSO, and stir at 85° C. for 1 hour by blowing nitrogen gas. Add 5 mmol of the synthesized terminal bromide quaternary ammonium salt b to be dissolved in 10 mL of DMSO, slowly drop into the above-mentioned chitosan solution, maintain 85° C. and stir for 8 hours to obtain a crude product. The crude product was filtered in acetone at 25°C, precipitated and washed with acetone at 40°C. Dry at 40°C for 24 hours. Finally, Soxhlet e...
Embodiment 3
[0029] Embodiment 3: the present invention provides a kind of preparation method of long-chain easily soluble chitosan, comprises the following steps:
[0030] 1) Put 50 mmol of dibromobutane and 10 mmol of N,N-dimethyldodecylamine into 30 mL of acetonitrile, purify with nitrogen, stir at 50°C for 16 hours, and then reflux for 1 hour. The solvent was evaporated to dryness and washed with ether. Obtain white paste, dry, and dry at 35 ℃ for 48 hours to obtain terminal bromide quaternary ammonium salt c.
[0031] 2) Disperse 1 g of chitosan in 50 mL of DMSO, and stir at 85° C. for 1 hour by blowing nitrogen gas. Add 5 mmol of the synthesized terminal bromide quaternary ammonium salt c to be dissolved in 10 mL of DMSO, slowly drop into the above chitosan solution, keep stirring at 85° C. for 8 hours to obtain a crude product. The crude product was filtered in acetone at 25°C, precipitated and washed with acetone at 40°C. Dry at 40°C for 24 hours. Finally, Soxhlet extraction wa...
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